6890 Standard Operating Procedures G1530-90380

Standard Operating Procedures
The HP 6890 Series Gas Chromatograph
Hewlett-Packard Company 1995 All Rights Reserved. Reproduction, adaptation, or translation without permission is prohibited except as allowed under copyright laws. HP part number G1530-90380 First Edition: November 1995 Printed in USA
Warranty The information contained in this document is subject to change without notice. Hewlett-Packard makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Hewlett-Packard shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material Safety Information This manual contains safety information that should be followed by the user to ensure safe operation. WARNING A warning calls attention to a condition or possible situation that could cause injury to the user. CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the user s work. The HP 6890 Series Gas Chromatograph Operating Manual supplied with the Hewlett-Packard 6890 gas chromatograph (HP GC) contains WARNING and CAUTION messages that inform the user about potential hazards that accompany working on and/or operating the instrument. Refer to them for complete safety information.
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Table of Contents
Overview...................................................................................................................................... Using This Handbook.................................................................................................................. 1 2
BASIC MAINTENANCE
Column Adapter/Makeup Gas Fitting, Installation.................................................................... Column Installation..................................................................................................................... 3 9
Liner/Insert, Installation ............................................................................................................. 17 Inlet Septum, Installation............................................................................................................ 23
FID CHECKOUTS
FID (Flame Ionization Detector) Checkout Using a Packed or Purged Packed ..................... 27 Column Inlet FID (Flame Ionization Detector) Checkout Using a Split-Only or Split/Splitless ................... 41 (in Split Mode) Capillary Column Inlet FID (Flame Ionization Detector) Checkout Using a Cool On-Column Capillary .................... 55 Column Inlet
TCD CHECKOUTS
TCD (Thermal Conductivity Detector) Checkout Using a Packed or Purged Packed ........... 67 Column Inlet TCD (Thermal Conductivity Detector) Checkout Using a Split-Only or Split/Splitless ......... 79 (in Split Mode) Capillary Column Inlet TCD (Thermal Conductivity Detector) Checkout Using a Cool On-Column Capillary .......... 91 Column Inlet
ECD CHECKOUTS
ECD (Electron Capture Detector) Checkout Using a Packed or Purged Packed .................. 103 Column Inlet ECD (Electron Capture Detector) Checkout Using a Split-Only or Split/Splitless ................ 115 (in Split Mode) Capillary Column Inlet ECD (Electron Capture Detector) Checkout Using a Cool On-Column Capillary ................. 127 Column Inlet
Table of Contents
NPD CHECKOUTS
NPD (Nitrogen Phosphorus Detector) Checkout Using a Packed or Purged Packed ............ 139 Column Inlet NPD (Nitrogen Phosphorus Detector) Checkout Using a Split-Only or Split/Splitless .......... 153 (in Split Mode) Capillary Column Inlet NPD (Nitrogen Phosphorus Detector) Checkout Using a Cool On-Column Capillary ........... 167 Column Inlet
Overview
The following procedures are protocols and criteria developed by Hewlett-Packard as part of the quality system used for the HP 6890 Series gas chromatograph (GC) manufacturing process. The intent is to recommend a means for the user to review if a given HP 6890 Series GC continues to perform according to the original chemical checkout testing expectations. In performing these protocols, please be aware that the following procedures were developed and tested on new instruments that were free from the effects of usage and time. Under normal operating conditions, these instrument checkout testing expectations should serve as a useful guideline or model for integrating performance operating procedures into individual laboratory standard operating procedures (SOPs). However, these SOPs alone cannot determine completely if an instrument is not performing to its intended capabilities. This book is not intended to be used as a substitute for any regulatory requirements. They should be addressed by the user in his/her perspective laboratory environment. It should, however, serve as a useful reference document when creating SOPs based on individual preventive maintenance practices surrounding the HP 6890 Series GC instrument. As a single-point measurement method, meeting acceptance criteria described in these SOPs does not necessarily assure performance capability required for any given analytical method the user may wish to use. Performance capability for any given analytical method must be demonstrated separately within the context of that method. Therefore, the SOPs given in this book are written as suggested guidelines that are independent of any method for performance checks. For specific operating or maintenance questions, please refer to the HP 6890 Series Gas Chromatograph Operating Manual (HP part no. G1530-90310) or the HP 6890 Series Gas Chromatograph Maintenance and Troubleshooting Manual (HP part no. G1530-90320).
Using This Handbook

This handbook contains standard operating procedures (SOPs) for the HP 6890 Series gas chromatograph (GC). These SOPs include procedures and good laboratory practices (GLPs) that apply to operation and maintenance of the HP 6890 Series GC. The SOPs carry the following information on each page: Date of issue Page number Number of pages in the SOP The SOPs have open fields for you to add information specific to your company. On each page of the SOPs, you can add a procedure number. On the first page of the SOPs you can add: Company name and official stamp Procedure number Revision number Replacement revision number Authorizing person Reviewing person Effective date Distribution list
3 Column Adapter/Makeup Gas Fitting, Installation
Standard Operating Procedure

Title: Column Adapter/Makeup Gas Fitting, Installation
Procedure Number: ___________________________________________________________________ Revision Number: ____________________________________________________________________ Replaces Revision: ___________________________________________________________________ Approved by: ________________________________________________________________________ Reviewed by: ________________________________________________________________________ Effective Date: _______________________________________________________________________ Company Stamp:
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Revision Date 9-Jan-98 Hewlett-Packard Company
Page 1 of 6
Procedure no.:________________
Scope
Use the following procedure to install an appropriate column or makeup gas adapter properly in various inlet and detector types.
Instrumentation
This SOP applies to all HP 6890 Series GCs and standard inlet and detector options.
General Overview
All the detectors are normally shipped with the hardware installed for capillary column use. With the capillary-only bases for the flame ionization detector (FID) and nitrogenphosphorus detector (NPD), it is not possible to install packed columns. However, with the thermal conductivity detector (TCD), electron capture detector (ECD), and the packed FID and NPD detector bases, packed columns can be used by changing (or removing) the adapter to accommodate a variety of column types. The following Comments, General section is for both general considerations and those associated with specific inlet and detector types.
Related SOPs
Liner/insert, installation, SOP no. _____________ Column, installation, SOP no. _____________
References
HP 6890 Series Gas Chromatograph Operating Manual, Column Installation section, HP part no. G1530-90310
Comments, General
With the exception of the TCD, all adapters have a 1/4-inch in outer diameter. Those for the TCD have a 1/8-inch outer diameter. All adapters are inserted fully into the inlet or detector in installation. In all cases, installation of a nut and ferrule to obtain a gas tight seal is best done by first finger tightening to ensure no cross-threading occurs. If the nut does not turn easily by fingers, it is often evidence of distorted threads caused by overtightening and/or by extended high-temperature exposure in prior installations.
Revision Date 9-Jan-98 Hewlett-Packard Company Page 2 of 6 Procedure no.:________________
5 Column Adapter/Makeup Gas Fitting, Installation Overtightening the nut during installation may distort/damage the sealing ferrule to the point where a leak-free seal cannot be achieved no matter how tight. Follow vendor recommendations for the particular ferrule. Note that tightening recommendations are often different for installation of an adapter with a new ferrule as opposed to those for reinstalling an adapter with an existing ferrule from a previous installation. Generally, you do not tighten a preset ferrule to the same degree as for a new ferrule. A variety of types of ferrules exist to provide a gas-tight seal. Each type has its own particular set of advantages and disadvantages: 1. Stainless steel nut and ferrules are used in applications requiring extended exposure to very high temperatures. In selecting stainless steel, be aware of the following: The ferrules will form a permanent seal to the given adapter and, therefore, cannot be removed later. If leakage occurs despite reasonable tightening, a new adapter is the best solution. In cases of overtightening, a stainless steel nut and ferrules can harden enough to distort threads permanently on the inlet/detector body. 2. Brass nut and ferrules are used in applications requiring more moderate temperatures or less extended exposure to very high temperatures. In selecting brass, be aware of the following: The ferrules will form a permanent seal to the given adapter and, therefore, cannot be removed later. If leakage occurs despite reasonable tightening, a new adapter is the best solution. Over long periods of usage, brass can both oxidize and distort in shape leading to increasing difficulty in installation or removal of an adapter. A new adapter is the best solution. 3. Composite material ferrules (Vespel, graphitized Vespel, graphite, etc) are used in applications requiring moderate temperatures or short-duration exposure to high temperatures. They have an advantage over metal ferrules in that they are easily removed from the adapter when necessary. In selecting such ferrules, be aware of the following: Vespel-type ferrules may fail immediately if overtightened (by splitting, being crushed, etc.); soft graphite ferrules may extrude into the fitting if overtightened. In such failure cases, inspect both the nut and fitting for pieces of ferrule, and remove any found. In usage, Vespel-type ferrules can degrade thermally giving eventual failure by leakage and thereby leading to the need of replacement.
Vespel-type ferrules tend to shrink upon first exposure to typical gas chromatographic temperatures. One should plan to recheck tightness after initial usage of a new ferrule or, alternatively, the ferrule may be preshrunk before installation by placing it in an oven at 250C for at least 4 hours. When tightening or loosening the nut on the adapter while securing the adapter into the inlet/detector body, use of two wrenches in opposition to each other is strongly recommended. NOTE: Depending upon the given HP 6890 instrument and its specific configuration, the particular inlet or detector may have an insulating cup present that prevents access to the base of the inlet or detector body. In these cases, access is achieved in final tightening of the nut and ferrule by removing the cup temporarily and allowing it to hang on the connected column. d. If using metal ferrules (brass or stainless steel) where torque forces are relatively high, one wrench should be placed on the nut portion of the inlet/detector body to prevent it from being twisted during tightening or loosening performed with the second wrench on the nut that secures the adapter and ferrules into the inlet/detector body. e. If using a composite ferrule (Vespel-type, graphite, etc) where torque forces are relatively mild, one wrench should be placed on the nut portion of the adapter body to prevent it from rotation during tightening or loosening performed by the second wrench on the nut that secures the adapter and ferrule into the inlet/detector body. Rotation of the adapter within a composite ferrule system may damage the ferrule. NOTE: If installing the capillary column makeup gas adapter in either the TCD or ECD, it is especially important to use a second wrench to prevent rotation of the adapter. Rotation of the makeup gas adapter may break the gas line where it is welded to the adapter.
Specific Comments, Purged Packed Column Inlet

1. The inlet body without any adapter is designed to accommodate a 1/4-inch glass packed column where the column itself can be inserted fully to serve as a liner. 2. Some adapters provided for these inlets are designed to accommodate a drop-in glass insert. The insert should be present in these adapters to provide proper expansion volume at sample injection time. They are mostly used to trap nonvolatiles and should be replaced when they get dirty or as prescribed by local procedures.
Specific Comments, FIDs and NPDs with Packed Column Bases

1. The detector makeup gas function is internal and, therefore, no separate makeup gas adapter is provided.
Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:________________ Page 4 of 6
7 Column Adapter/Makeup Gas Fitting, Installation 2. The detector body without any adapter is designed to accommodate a 1/4-inch glass packed column where the column itself can be inserted fully to serve as a liner. 3. Some adapters provided for these detectors may require a jet exchange to optimize detector performance for the particular column type being installed.
Specific Comments, TCD

1. The detector makeup gas function is internal and, therefore, no separate makeup gas adapter is provided. 2. The detector body without any adapter is designed to accommodate a 1/8-inch metal packed column.
Specific Comments, ECD

1. The detector makeup gas function is externally provided by a separate makeup gas adapter located inside the oven next to the detector and designed to accommodate capillary columns only. No makeup gas is used in packed column applications. 2. The detector body without any adapter is designed to accommodate a 1/4-inch glass packed column where the column itself can be inserted fully to serve as a liner.
Page 5 of 6
Procedure no.:________________
Page 6 of 6
Procedure no.:________________

Title: Column, Installation
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 8
Procedure no.:________________
10 Column, Installation
Scope
Use the following procedure to install a column properly in various inlet and detector types, and/or to condition or bakeout a column.
Instrumentation
This SOP applies to all HP 6890 Series GCs and standard inlet and detector options.
General Overview
The split/splitless and cool on-column capillary inlets are designed for use with capillary columns. The purged-packed inlet is adaptable for use with packed or capillary columns. The flame ionization detector (FID), nitrogen-phosphorus detector (NPD), thermal conductivity detector (TCD), and electron capture detector (ECD) are available with adaptable bases that can be used with packed or capillary columns. The FID and NPD are also available with a capillary-optimized base that accepts capillary columns only. When an adapter is required, the type is determined by the type and size of the column. The following comments assume you have already selected the correct adapters for your inlet/column/detector combination. If you are unsure about which adapter to use, consult your user documentation section on column installation.
Related SOPs
Column adapter/makeup gas fitting, installation, SOP no. ____________
References
HP 6890 Series Gas Chromatograph Operating Manual, HP part no. G1530-90310
Comments, General
Adaptable inlets and detectors, with the exception of the TCD, are designed to accept 1/4-inch or 6-mm od glass packed columns without use of any adapter. Other column types require an adapter for installation. The TCD accepts 1/8-inch columns with no adapter but requires adapters for all others. Instruments are normally shipped with the appropriate adapters for capillary columns. The column connection at each end is made with a nut and ferrule to obtain a gas tight
11 Column, Installation seal. In all cases, installation of nuts and ferrules to obtain a gas tight seal is best done by first tightening by fingers to ensure no cross-threading occurs. If the nut does not turn easily by fingers, it is often evidence of distorted threads caused by over-tightening and/or by extended high-temperature exposure in prior installations. Over-tightening the nut during installation may distort or damage the sealing ferrule to the extent that a leak-free seal cannot be achieved no matter how tight. In the case of glass or fused silica column types, the column itself can be broken if the fitting is overtightened. Follow vendor recommendations for the chosen sealing ferrules. Note that tightening recommendations are often different for installation of a column with new ferrules as opposed to those for reinstallation with existing ferrules. Generally, you do not tighten preset ferrules to the same degree as for new ferrules. A variety of types of ferrules exist to provide a gas-tight seal. Each type has its own particular set of advantages and disadvantages in usage: 1. Stainless steel nuts and ferrules are used in metal packed column applications requiring extended exposure to very high temperatures. In selecting stainless steel, be aware of the following: The ferrules will form a permanent seal to the given column and, therefore, cannot be removed later. If leakage occurs despite reasonable tightening, a new column or cutting off the bad section of an existing column is the best solution. In cases of overtightening, a stainless steel nut and ferrules can harden enough to distort threads permanently on the inlet/detector body. 2. Brass nuts and ferrules are used in metal packed column applications requiring more moderate temperatures or less extended exposure to very high temperatures. In selecting brass, be aware of the following: The ferrules will form a permanent seal to the given column and, therefore, cannot be removed later. If leakage occurs despite reasonable tightening, a new column or cutting off the bad section of an existing column is the best solution. Over long periods of usage, brass can both oxidize and distort in shape leading to increasing difficulty in installation or removal of a column. A new column or cutting off the bad section of an existing column are the best solutions.
Page 3 of 8 Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:________________
12 Column, Installation 3. Composite material ferrules (Vespel, graphitized Vespel, graphite, etc.) that are compatible with virtually any column type are used in applications where operating temperatures do not exceed the temperature limit of the ferrule material. They have an advantage over metal ferrules in that they are easily removed from the adapter when necessary. In selecting such ferrules, be aware of the following: Vespel-type ferrules may fail immediately if overtightened (by splitting, being crushed, etc); soft graphite ferrules may extrude into the fitting if overtightened. In such failure cases, inspect both the nut and fitting for pieces of ferrule, and remove any found. In usage, Vespel-type ferrules can degrade thermally giving eventual failure by leakage and thereby leading to the need of replacement. Vespel-type ferrules tend to shrink upon first exposure to typical gas chromatographic temperatures. You should plan to recheck tightness after initial usage of a new ferrule, or alternatively, the ferrule may be preshrunk before installation by placing it in an oven at 250C for at least 4 hours. When tightening or loosening the nut securing the column onto the column adapter or inlet/detector body, use of two wrenches in opposition to each other is strongly recommended. NOTE: Depending upon the given HP 6890 instrument and its specific configuration, the particular inlet or detector may have an insulating cup present that prevents access to the base of the inlet or detector body. In these cases, access is achieved in final tightening of the nut and ferrule(s) by removing the cup temporarily and allowing it to hang on the connected column. If using metal ferrules (brass or stainless steel) where torque forces are relatively high, one wrench should be placed on the nut portion of the column adapter or inlet/detector body to prevent rotation during tightening or loosening performed with the second wrench on the nut that secures the column and ferrules onto the column adapter or inlet/detector body. If using a composite ferrule (Vespel-type, graphite, etc) where torque forces are relatively mild, one wrench should be placed on the nut portion of the column adapter or inlet/detector body to prevent rotation during tightening or loosening performed by the second wrench on the nut that secures the column and ferrule onto the column adapter or inlet/detector body. Rotation within a composite ferrule system may damage the ferrule. NOTE: If installing a capillary column in the ECD, it is especially important to use a second wrench to prevent rotation of the already installed makeup gas adapter. Rotation of the makeup gas adapter may break the gas line connected to it.
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Procedure no.:________________
Specific Comments, Installing Packed Columns

To minimize both dead volume and mechanical distortion of the column and ferrules in installing a metal column with new metal ferrules, the column should be pushed fully into the receiving fitting, then withdrawn by approximately 1 mm before the nut is tightened to set the ferrules permanently to form the gas tight seal. A reference mark made on the column to aid in maintaining its position during tightening is recommended. For convenience, the column may be positioned properly and its new ferrules preset outside the GC by the procedure described in the user documentation.
Specific Comments, Installing Capillary Columns

To assure a gas tight seal without undue tightening of the nut, the inner diameter of the chosen ferrule should match the outer diameter of the column to be installed as closely as possible. In some installation situations, it is necessary to make a reference mark on the column. For these cases, suitable marking fluid should be readily available. In placing the column nut and new ferrule onto a capillary column, ferrule material may enter the column. It is, therefore, recommended that 23 cm of the column end be broken off at a scribe mark made by a suitable, sharp scribing tool. The freshly cut end should be inspected for burrs and other irregularities and should be at right angles to the column length. The following are comments related to installation of a column with a new ferrule into specific inlet and detector types: 1. NOTE: Purged packed column inlet: Packed column and purged packed column inlets are not suitable for use with capillary columns with internal diameters less than 0.32 mm. For use with capillary columns, the purged packed inlet should be used at column flows 5 mL/min. a. On a suitable work surface, adjust the column position so that 3 1 mm (a length suitable for most applications) extends beyond the threaded portion of the column nut. The end of the column should be 12 mm above the ferrule. b. Using a suitable marking fluid, mark the column at the opposite end of the column nut as a reference aid during installation. a. While maintaining the column position in reference to the nut, install the column and nut into the inlet column fitting.
Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:________________ Page 5 of 8
14 Column, Installation b. Using fingers only, tighten the column nut just enough to feel resistance in moving the column, then if necessary, position the column correctly in reference to the nut and previously made mark on the column. c. Tighten the column nut further following vendor recommendations to avoid ferrule damage from overtightening.
2.
Split/splitless capillary column inlet: a. On a suitable work surface, adjust the column position so that 9 1 mm (a length suitable for most applications) extends beyond the threaded portion of the column nut. The end of the column should be 58 mm above the ferrule. (Check your local procedures, and use the recommendation in your procedures if different from this.) b. Using a suitable marking fluid, mark the column at the opposite end of the column nut as a reference aid during installation. c. While maintaining the column position in reference to the nut, install the column and nut into the inlet column fitting. d. Using fingers only, tighten the column nut just enough to feel resistance in moving the column, then, if necessary, position the column correctly in reference to the nut and previously made mark on the column. e. Tighten the column nut further following vendor recommendations to avoid ferrule damage through overtightening.
3. NOTE:
On-column capillary column inlets: The on-column inlet and the HP 7673 automatic injector require hardware changes for different internal and outside diameter columns. Before you proceed, confirm that the correct hardware is installed. The inlet requires changes to the insert and septum nut, while the injector requires changes to the needle guide. It is also necessary to use the correct syringe with the correct syringe needle. Check the HP 6890 Series Gas Chromatograph Operating Manual and the HP Automatic Liquid Sampler Operating Manual for further details. a. Install the column by gently inserting the column fully into the detector fitting until you first feel resistance to further insertion. a. Tighten the column nut following vendor recommendations to avoid ferrule damage from overtightening.
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Procedure no.:________________
15 Column, Installation 4. FIDs, NPDs, and TCDs: a. Install the column by gently inserting the column fully into the column fitting until it stops. b. Using fingers only, tighten the column nut just enough to feel resistance in moving the column. c. Withdraw the column by 1 mm from its fully inserted position. A suitable reference mark made on the column is recommended as an aid in judging the 1-mm withdrawal. d. Tighten the column nut further following vendor recommendations to avoid ferrule damage from overtightening.
5. NOTE:
ECDs: Some HP 6890 instruments use an ECD makeup gas adapter that provides a hard stop to column insertion. More recent instruments use a makeup gas adapter that is open-ended. The following process accommodates either situation. a. On a suitable work surface, adjust the column position so that 53 1 mm extends beyond the threaded portion of the column nut. b. Using a suitable marking fluid, mark the column at the opposite end of the column nut as a reference aid during installation. c. While maintaining the column position in reference to the nut, install the column and nut into the detector column fitting. d. Using fingers only, tighten the column nut just enough to feel resistance in moving the column, then gently attempt to insert the column further by an additional 1 to 2 mm: If further insertion is possible, withdraw the column and position it correctly in reference to the nut and previously made mark on the column. If a hard stop is encountered preventing further insertion, withdraw the column by 1 mm from the fully inserted position. If necessary, an additional reference mark can be made on the column as an aid in judging the 1-mm withdrawal. a. Tighten the column nut further following vendor recommendations to avoid ferrule damage from overtightening.
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Procedure no.:________________
Column Conditioning/Bakeout
New columns often exhibit high levels of stationary phase bleed. Older columns may exhibit bleed problems from slow-moving sample components accumulated in the column over many injections. Either situation typically causes increasing drift and/or wander in the chromatographic baseline as column temperature increases during temperature-programmed analyses. In either case, a simple procedure may be used to condition the column to improve its bleed behavior when returned to normal service. 1. Install the column at the inlet only. In leaving the detector unconnected, material exiting the column is prevented from contaminating the detector. The detector column connection fitting should be plugged to prevent entry of other foreign material from the oven as well. Provide carrier gas flow through the column. Any flow rate normal for the type of column in its intended application is acceptable. If hydrogen is the normal carrier gas choice, due to a possible explosion hazard within the oven, temporarily switch the inlet to a supply of helium or nitrogen. It is advisable to purge the column with carrier flow for 2030 minutes at room temperature to remove oxygen. Some liquid phases are especially sensitive to oxidation and may be damaged by heating before complete equilibration with carrier gas. 3. NOTE: Set the oven to a temperature at or somewhat greater than the highest temperature to which the column is exposed in its analytical applications. Do not exceed the vendor-specified isothermal temperature limit for the specific column to be conditioned. Permanent damage to the column and/or its stationary phase may occur.
2. WARNING: NOTE:
4.
Shortest time of exposure to elevated temperature is obtained through experience, depending upon the type of column, type and thickness of stationary phase, usage in applications, etc. Usually several hours exposure is a sufficient starting point. The process may be repeated if needed. To minimize thermal shock to the column, at the end of the conditioning time, allow the oven and column to cool gradually while maintaining carrier flow. Gradual cooling may be achieved simply by switching the oven off.
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5.
Procedure no.:________________
17

Title: Liner/Insert, Installation
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 6
Procedure no.:________________
18 Liner/Insert, Installation
Scope
Use the following procedure to properly install an insert.
Frequency
Liner/insert replacement frequency is highly dependent upon working variables, such as sample cleanliness, sample composition, temperature, etc. Therefore, frequency must be a local (user) decision based upon experience. As a general guideline, however, you should be conservative, changing the glass insert/liner more frequently than might be necessary. An alignment insert, used in cool on-column capillary column inlets, serves to align the column and syringe needle. Therefore, it is replaced only if the present column is to be replaced by a column of different outer diameter.
Instrumentation
This SOP applies to all HP 6890 Series GCs with standard inlet options.
General Overview
Section A describes glass insert replacement applicable to purged packed column inlets. Section B describes glass liner/insert replacement applicable to all split/splitless and split-only capillary column inlets. Section C describes alignment insert replacement applicable to all cool on-column capillary column inlets. In all three cases, exchange is performed at the top of the HP 6890 Series GC.
Related SOPs
1. Column adapter/makeup gas fitting, installation, SOP no. ____________
References
1. HP 6890 Series Gas Chromatograph Operating Manual, Inlets section (HP part no. G1530-90310)
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Procedure no.:________________
19 Liner/Insert, Installation
Section A: Purged Packed Column Inlet

WARNING: WARNING: If the unit has been used recently, the inlet area may be hot enough to cause serious burns. If necessary, switch off the appropriate heated zone, and allow sufficient cooling time. If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed to flow during glass insert exchange. It is recommended that hydrogen carrier flow be switched off during the procedure. As carrier gas flow through the column ceases during glass insert exchange, it is recommended that column oven temperature be reduced to a conservative value during the procedure. If local procedures and/or the method specifies, the oven temperature should be set near ambient (35 40C).
NOTE:
Procedure
1. For the purged packed column inlet, remove the combined assembly of septum retainer nut, septum, and top insert weldment. Inspect the O-ring seal between the top insert weldment and inlet body, and replace it if necessary. Generally, the old glass insert may now be removed through the now-exposed top of the inlet body. A fibrous, cylindrical object of suitable outer diameter (such as a match stick, large-diameter tooth pick, etc) can be inserted into the insert from the top, then used to extract it from the inlet body. If the old glass insert cannot be extracted through the top of the inlet body, then from inside the oven, the column adapter containing the insert must be removed from the inlet body. This may require disconnecting the column first to prevent possible damage and/or loss of gas-tight sealing. 3. Install the glass insert simply by placing it gently into the column adapter oriented with its unflared end entering the adapter first. Note that if the column adapter was never removed from the inlet body in extracting the old glass insert, the new insert should disappear entirely from view at the top of the inlet body. If its flared end is too large to pass through the top of the inlet body, try a different insert. If necessary, the column adapter must be removed from the inlet body. This may require disconnecting the column first to prevent possible damage and/or loss of gas-tight sealing. 4. Replace items removed to exchange glass inserts. Restore inlet gas flow rate(s) and temperature setpoints. Check the flow rate through the injection port. If the carrier flow rate is higher than expected, the adapter fitting in the oven will have to
Page 3 of 6 Procedure no.:________________
2.
20 Liner/Insert, Installation be tightened. Tighten if necessary.
Section B: Split/Splitless Capillary Column Inlets

WARNING: WARNING: If the unit has been used recently, the inlet area may be hot enough to cause serious burns. If necessary, switch off the appropriate heated zone, and allow sufficient cooling time. If hydrogen is used as the carrier gas, possible fire or explosion hazard exists if it is allowed to flow during glass liner exchange. It is recommended that hydrogen carrier flow be switched off during the procedure. For split/splitless capillary column inlets, if either the old glass liner to be replaced or the new glass liner to be installed contains unsecured material (for example, glass wool), the material may become dislodged if carrier gas is allowed to flow during exchange. In this case, it is recommended that carrier flow be switched off and allowed to drop to zero before starting the procedure. As carrier gas flow through the column ceases during glass liner exchange, it is recommended that column oven temperature be reduced to a conservative value during the procedure.
NOTE:
NOTE:
Procedure
1. Remove the combined assembly of septum retainer nut, septum, and split/splitless insert weldment. Carefully bend the attached tubing just enough to gain access to the top of the inlet body and to the liner to be replaced. Carefully remove the old liner and its O-ring seal. If fragments of O-ring material adhere to the metal surfaces (often a sign of lengthy service at high temperature), they must be removed. Avoid allowing fragments of either the O-ring seal or liner (if broken) from entering the inlet itself. Having a vacuum cleaner available is also recommended in this situation.
2.
NOTE:
3.
Install the new liner with an appropriate seal; the inner diameter of the new seal should closely match the outer diameter of the replacement liner. The new seal should never be loose on the liner or have to be forced onto the liner. Leakage may occur if an inappropriately sized seal is used. Also note that some liner styles may require a specific orientation in installation, especially those containing unsecured material (for example, glass wool). Follow vendor recommendations, bearing in mind that gas flow through the liner is always from the top of the inlet (septum location) to its bottom (column location).
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21 Liner/Insert, Installation 4. Carefully replace the inlet top assembly that was removed to exchange liners, tightening firmly the nut portion of the split/splitless insert weldment. Restore inlet gas flow rate(s) and temperature setpoints, and check the pressure.
Section C: Cool On-Column Capillary Column Inlets

WARNING: If the unit has been used recently, the oven and inlet area may be hot enough to cause serious burns. If necessary, switch off the oven (and inlet heated zone if applicable) and allow sufficient cooling time. If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed to flow during alignment insert exchange. It is recommended that hydrogen carrier flow be switched off during the procedure. The cool on-column capillary column inlet has a small coil spring located in the inlet body just below the septum location. The spring is removed in this procedure and can be easily lost. It is an integral part of the inlet assembly, helping to maintain correct column and syringe needle alignment. Proceed with vigilance. As carrier gas flow through the column ceases during alignment insert exchange, it is recommended that the column oven temperature be reduced to a conservative value during the procedure.
WARNING:
NOTE:
NOTE:
Procedure
1. If not already done, remove the column. If the diameter is different on the column to be installed, the insert will have to be replaced. Depending upon the inlet configuration, remove the cooling tower or septum nut base assembly located at the top of the inlet. Carefully remove the small coil spring now visible, extending just above the top of the inlet body. Place the spring in a safe place. Remove the old alignment insert by pushing it out at the top of the inlet body from the inlet column fitting inside the oven. A piece of straight wire of suitable diameter, such as a syringe plunger, can be used. Place the removed insert in a safe place to be used again if needed.
2.
3.
4.
Page 5 of 6
Procedure no.:________________
22 Liner/Insert, Installation 5. Select the replacement alignment insert according to the diameter of the column to be installed, and simply drop it into the inlet body from the top. Orientation does not matter. Consult your user documentation for information about selecting an alignment insert appropriate for the outer diameter of the column to be installed. 6. Replace the coil spring and cooling tower or septum nut base assembly, and tighten the nut fully using your fingers only. Install the new column, restore the inlet gas flow, and check the pressure and temperature setpoints.
7.
Page 6 of 6
Procedure no.:________________
23

Title: Inlet Septum, Installation
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 4
Procedure no.:________________
24 Inlet Septum, Installation
Scope
Use the following procedure to install a septum into an inlet properly.
Frequency
Septum replacement frequency is highly dependent upon working variables, such as septum temperature, septum material, syringe needle quality, injection methodology and/or technique, etc. Therefore, frequency must be a local (user) decision based upon experience. As a general guideline, however, you should be conservative, changing the septum more frequently than might be necessary.
Instrumentation
This SOP applies to all HP 6890 Series GCs and standard inlet options.
General Overview
Septum replacement is described in two separate sections: Section A is applicable to all purged packed and split/splitless capillary column inlets. Section B is applicable to all cool on-column capillary column inlets.
Parts/Equipment Referenced
The following tools and parts are used for replacement of the septum in the inlets. Septum nut wrench (HP part no. 19251-00100) 11-mm septum (HP part no. 5181-1263) 5-mm septum (HP part no. 5181-1261) A nonmetallic (plastic or wood) tool with a sharp tip to remove septum from the inlet Forceps or tweezers
References
HP 6890 Series Gas Chromatograph Maintenance and Troubleshooting Manual (HP part no. G1530-90320)
Page 2 of 4
Procedure no.:________________
25 Inlet Septum, Installation
Section A: Purged Packed Column and Split/Splitless Capillary Column Inlets

WARNING: WARNING: If the unit has been used recently, the inlet area may be hot enough to cause serious burns. If necessary, switch off the appropriate heated zone, and allow sufficient cooling time. If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed to flow during septum exchange. It is recommended that hydrogen carrier flow be switched off during the procedure. For split/splitless capillary column inlets, if a liner is present containing unsecured material (for example, glass wool), the material may become dislodged if carrier gas is allowed to flow during septum exchange. In this case, it is recommended that carrier flow be switched off and allowed to drop to zero before starting the procedure. As carrier gas flow through the column ceases during septum exchange, it is recommended that column oven temperature be reduced to a conservative value during the procedure. If local procedures and/or the method specifies, the oven temperature should be set near ambient (35 40C)
NOTE:
NOTE:
Procedure
1. 2. Remove the septum retainer nut located at the top of the inlet. Remove the old septum. If fragments of septum material adhere to the metal surfaces (often a sign of lengthy service at high temperature), they must be removed. Do not let septum material fragments enter the inlet. If necessary, temporarily block the inlet opening with a piece of aluminum foil. Having a vacuum cleaner available is also recommended in this situation.
NOTE:
3.
Install the new septum. a. For an 11-mm diameter septum, the septum must be pressed evenly into place, working around its edges. b. Replace the septum retainer nut and tighten it using your fingers only until you first begin to feel resistance. Then tighten further by 1/4- to 1/2-turn. Note that fully tightening the nut with an 11-mm diameter septum may compress the septum material to an extent that it is not easily pierced by a syringe needle. This could cause a bent needle or septum "coring" whereby the needle carries
Page 3 of 4
Procedure no.:________________
26 Inlet Septum, Installation small pieces of septum material into the inlet. 4. Restore the inlet gas flow rate(s), and allow the carrier gas to purge the inlet and column thoroughly. Restore temperature setpoints.
5.
Section B: Cool On-Column Capillary Column Inlets

WARNING: If hydrogen is used as the carrier gas, a possible fire or explosion hazard exists if it is allowed to flow during septum exchange. It is recommended that hydrogen carrier flow be switched off during the procedure. The cool on-column capillary column inlet has a small coil spring located in the inlet body just below the septum location. Although the spring is not removed in this procedure, it can be easily lost. It is an integral part of the inlet assembly, helping to maintain correct column and syringe needle alignment. Proceed with vigilance. As carrier gas flow through the column ceases during septum exchange, it is recommended that the column oven temperature be reduced to a conservative value during the procedure.
NOTE:
NOTE:
Procedure
1. 2. Depending upon the inlet configuration, remove the cooling tower or septum nut base assembly located at the top of the inlet. Remove the old septum from the underside of the removed cooling tower or septum base assembly. A pointed tool, such as a bamboo skewer, may be needed to pry out the old septum. Any remaining fragments of septum material must be removed. Insert the replacement septum into the cooling tower or septum nut base assembly. Note that if a "duck bill" septum is being installed (for manual injection use only), the septum "bill" must be oriented to point into the inlet body (toward the column). Replace the cooling tower or septum nut base assembly containing the new septum, and tighten the nut fully using fingers only. Restore the inlet gas flow rate(s) and temperature setpoints.
3.
4. 5.
Page 4 of 4
Procedure no.:________________
27

Title: FID (Flame Ionization Detector) Checkout Using a Purged Packed Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Procedure no.:________________
28 FID (Flame Ionization Detector), Purged Packed
Scope
Use the following procedure to verify proper FID operation with the purged packed inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 10-l syringe, HP part no. 9301-0810 or equivalent Disposable glass inserts, HP part no. 5080-8732 Septum, HP part no. 5181-1263 Liner for wide-bore capillary columns, HP part no. 19244-80540 Viton O-ring, HP part no. 5080-8898 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent FID flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gases: helium as carrier, nitrogen as makeup, air, and hydrogen
Analog Input
HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable, HP part no. G1530-60570 (2-meter, 6-pin) HP 6890A-to-HP 3396B remote start cable, HP part no. G1530-61020 (9-pin/15-pin) HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 3396-61010 (9-pin/15-pin)
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator INET communication card, HP 6890 Option 510 (accessory HP G1553A)
Procedure no.:________________
29 FID (Flame Ionization Detector), Purged Packed HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
HP GC ChemStation software loaded as part of the HP multitechnique ChemStation on an IBM-compatible personal computer with an HP-IB interface and the proper amount of memory for applications to be run. (See the HP Multitechnique ChemStation Manual for requirements.) HP-IB cable, HP part no. 8120-3445 (1 meter)
Related SOPs
Inlet septum, installation, SOP no. _____________ Liner/insert, installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the packed column inlet, install a new septum, a capillary column adapter, new liner, and the HP 6890 evaluation column. b. At the FID, install a 0.28-mm (0.011-in.) jet and/or the capillary column adapter, if needed, and the remaining end of the HP 6890 evaluation column.
2.
At the HP 6890, verify that the FID to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu.
3.
After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
Procedure no.:________________
30 FID (Flame Ionization Detector), Purged Packed a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the FID to be evaluated:
[Signal 1] [Front Detector] {or [Back Detector]}
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the FID to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz.
Procedure no.:________________
31 FID (Flame Ionization Detector), Purged Packed 4. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following values :
Column pressure = 25 psi
Verify that the column is operating in constant flow mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant flow by pressing the [Mode/Type] key and selecting Constant Flow. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the FID, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40 C.
5.
Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Inlet Temperature: 250C Detector Temperature: 300C
Oven Program :
Temperature: 40C Initial time: 0 min Rate 1: 25C/min Final temperature: 90C Final time: 0 min Rate 2: 15C/min Final temperature: 170C Final time: 2 min
Allow the unit at least 30 minutes to stabilize thermally.
6.
After thermal stabilization, set the following values according to the appropriate instrument. a. For an electronic pressure and flow controlled FID, input the following values by pressing the appropriate detector key to open the control screen and then entering the following flow setpoint values:
Hydrogen flow = 30 mL/min Air flow = 400 mL/min Makeup flow (nitrogen) = 25 mL/min
Procedure no.:________________
32 FID (Flame Ionization Detector), Purged Packed Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. If the detector flow rates are checked, the values should be within the limits set in step 6b for a manual flow controlled FID. b. For a manual flow controlled FID, establish the following flow rates by inserting the flow measurement adapter fully onto the FID collector and connecting the flowmeter:
Hydrogen flow = 30 mL/min + 2 mL/min Air flow = 400 mL/min + 30 mL/min Makeup flow (nitrogen) = 25 mL/min + 2 mL/min
After setting the flows above, remove the flowmeter and FID flow measurement adapter.
7.
At the HP 6890, turn on the FID electrometer by pressing [Configure] [Front Detector] {or [Back Detector]}. Turn the electrometer on by scrolling to the electrometer line and pressing [ON]. Press [Signal 1] to display its flame-off background offset. A stable value, <2.0 display units, is acceptable criteria to continue. If not met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
8.
Ignite the FID flame by going to the appropriate Detector Control Table, scrolling down to Flame, and pressing [ON]. a. Observe the FID flame signal at the display. Successful flame ignition typically results in a permanent increase in signal output. If no appreciable increase is observed, perform the next check; otherwise, continue to step 9. b. Hold a cool, shiny, metal object, such as a chrome-plated wrench, just above the FID chimney. Any observed water condensation signifies the flame is indeed ignited. c. If the flame has not ignited, recheck all flow rates, and attempt ignition again. If the flame cannot be lit even though flow rates are correct, consult your HP 6890 service and user documentation for additional information. If necessary, contact your Hewlett-Packard service representative.
9.
With the flame lit, observe the FID signal at the display. This is the flame-on background offset. A stable value between 5 and 20 display units is acceptable criteria to continue to step 10. If an air cleaning system is being used, it is possible that the value will stabilize to a value below 5.
Procedure no.:________________
33 FID (Flame Ionization Detector), Purged Packed Typically, the value may be >20 display units indicating system bakeout is necessary: a. Turn the detector off, remove the column from the detector, and cap the detector fitting. b. Reset the oven and heated zone temperature to the following values:
Front detector (or back detector) temperature: 400C Oven temperature: 250C
c. Reignite the detector, and monitor the displayed detector signal; it should rise quickly to some higher value as the FID heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. d. Reinstall the column in the detector. e. Restore the original setpoint temperatures specified in step 4, and allow the unit at least 2 hours to stabilize thermally. Observe the displayed detector signal to determine it is now within the acceptable range of between 5 and 20 display units, verify all gas flow rates, then continue to step 10. f. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
10. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the HP integrator, enter the following setpoint values:
[ATT 2^] [-] [2] [ENTER] [ZERO] [5] [0] [ENTER] [CHT SP] [1] [ENTER]
Press [PLOT] to begin plotting the FID signal. At an elapsed time of 1 minute, enter the following key sequence at the integrator, and allow plotting to continue for another 10 minutes:
[ATT 2^] [0] [ENTER]
Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:________________
34 FID (Flame Ionization Detector), Purged Packed Using the method shown, measure the plot to check for the following: Noise in the first 1-minute portion of the plot should be <24 mm in width. Wander over any given 2-minute period in the 10-minute portion of the plot should be <14 mm in width. Drift over any given 5-minute period in the 10-minute portion of the plot should be <30 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scaling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
This will give the HP 6890 method listing. At the bottom of the listing is the range value for signal 1 and 2. This is the range set at the MIO (INET) card. Normally this value is set to 5. The noise can be plotted with the integrator range value (this range is designated as SIG1RANGE) set to 5. The next bulleted step is to be used with a SIG1RANGE = 5. The attenuation values have been adjusted to give the same amplitude plot as the analog. It is permissible for the user to change the SIG1RANGE value to 0 (zero) and use the same integrator settings as in step 10a. The user is referred to the HP 3396 manual for further details in how to change the SIG1RANGE value. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the FID signal. At an elapsed time of 1 minute, enter the following key sequence at the HP 3396B/C or HP 3397A, and allow plotting to continue for another 10 minutes:
[ATT 2^] [-] [5] [ENTER]
Using the method shown, measure the plot to check for the following:
Procedure no.:________________
35 FID (Flame Ionization Detector), Purged Packed When plotted at [ATT 2^] [-] [7], noise in the first 1-minute portion of the plot should be <30 mm in width. Wander over any given 5-minute portion of the plot should be <17.5 mm in width. Drift over the full 30-minute plot should be <37.5 mm in width. c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 2.0 minutes and 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis.
36 FID (Flame Ionization Detector), Purged Packed Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0382 pA. Wander (for a 2-minute time window) should be <0.0892 pA. Drift (for a 5-minute time window) should be <0.1911 pA. 11. To perform chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range.
FID1 B, of FIDNOISE\NOISE001.D pA 4.5
4.25
3.75
3.5
3.25
2.75
10
12
14
min
At the integrator, enter the following setpoint values:

[ZERO] [ATT 2^] [CHT SP] [PK WD] [THRSH] [TIME] [1] [0] [4] [1] [.] [0] [4] [3] [8] [.] [7] [5] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [STOP]
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run.
37 FID (Flame Ionization Detector), Purged Packed The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >125,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.1. MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measured with the range 2^8 and the noise in mm at attn 2^0 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 5 for Signal 1 or (Signal 2) by pressing [Signal 1] and scaling down the control table to Range. NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range value is five by pressing:
[LIST] [OPTION] [8]
which displays the integrator range value. At the integrator, enter the following setpoint values:
[ZERO] [ATT 2^] [CHT SP] [PK WD] [THRSH] [AR REJ] [TIME] [1] [0] [4] [1] [.] [0] [4] [3] [0] [8] [.] [7] [5] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [STOP]
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >1,250,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.1.
Procedure no.:________________
38 FID (Flame Ionization Detector), Purged Packed MDL(C) = (694,000 x (Noise))/(Area C16) <= 4 pg/s with the noise measured in mm at attn 2^-6 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to HP GC ChemStation Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >4,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.1. MDL(C) = (436,000 x Noise)/(Area C16) <= 4 pg/s (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Procedure no.:________________
2000 1800 1600 1400 1200 1000 800 600 400 200 0 2 4 Time (min.) 6 8
C14
C15 C16
Procedure no.:________________
Procedure no. :________________
41

Title: FID (Flame Ionization Detector) Checkout Using a Split/Splitless Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 14
Procedure no.:________________
42
FID (Flame Ionization Detector), Split/Splitless
Scope
Use the following procedure to verify proper FID operation with the split/splitless inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 10-l syringe, HP part no. 9301-0810 or equivalent Septum, HP part no. 5181-1263 O-ring, HP part no. 5180-4182 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent FID flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gases: hydrogen, helium, nitrogen, and air
Data Handling Devices, Parts and Equipment

Analog Input
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator INET communication card, HP 6890 Option 510 (accessory HP G1553A) HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
Page 2 of 14
Procedure no.:________________
43
ChemStation Input
Related SOPs
Inlet septum, installation, SOP no. _____________ Liner/insert, installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________ Calculation of chromatographic performance factors for the HP 6890 with different data systems
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the capillary column inlet, install a new septum, a new split liner, O-ring seal, and the HP 6890 evaluation column. b. At the FID, install a 0.28-mm (0.011-in.) jet and/or the capillary column adapter, if needed, and the remaining end of the HP 6890 evaluation column. 2. At the HP 6890, verify that the FID to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
3.
Page 3 of 14
Procedure no.:________________
44
FID (Flame Ionization Detector), Split/Splitless a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the FID to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrators. At the HP 6890, assign Signal 1 to the FID to be evaluated:
Page 4 of 14
Procedure no.:________________
FID (Flame Ionization Detector), Split/Splitless 4.
45
Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [Back Inlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key and selecting Splitless. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following values:
Column pressure = 25 psi helium Purge flow = 60.0 mL/min Purge time = 0.75 min
5.
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure by pressing the [Mode/Type] key and selecting Constant Pressure. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the FID, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40 C. Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to 5070 mL/min. Record this value As measured at the inlet vent using the flowmeter, set the septum purge flow rate at 5 1 mL/min. 6. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Oven Program:
Temperature: 40C Initial time: 0 min Rate 1: 25C/min. Final temperature: 90C Final time: 0 min Rate 2: 15C/min Final temperature: 170C Final time: 2 min
Page 5 of 14
Procedure no.:________________
46
FID (Flame Ionization Detector), Split/Splitless 7. After thermal stabilization, set the following values according to the appropriate instrument: a. For an electronic pressure and flow controlled FID, input the following values by pressing the appropriate detector key to open the control screen and then entering the following flow values:
Hydrogen at 30 Air at 400 Makeup (nitrogen) at 25
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. If detector flow rates are checked, the values should be within the limits set in step 7b for a manual flow controlled FID. b. For a manual flow controlled FID, establish the following flow rates by inserting the flow measurement adapter fully onto the FID collector and connecting the flowmeter.
Hydrogen at 30 + 2 mL/min Air at 400 + 30 mL/min Makeup (nitrogen) at 25 + 2 mL/min
After setting the flows above, remove the flowmeter and flow measurement adapter. 8. At the HP 6890, turn on the FID electrometer by pressing [Configure] [Front Detector] {or [Back Detector]}. Turn the electrometer on by scrolling to the electrometer line and pressing [ON]. Press [Signal 1] to display its flame-off background offset. A stable value, <2.0 display units, is acceptable criteria to continue. If not met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. Ignite the FID flame by going to the appropriate Detector Control Table, scrolling down to Flame, and pressing [ON]. a. Observe the FID flame signal at the display. Successful flame ignition typically results in a permanent increase in signal output. If no appreciable increase is observed, perform the next check; otherwise, continue to step 10. b. Hold a cool, shiny, metal object, such as a chrome-plated wrench, just above the FID chimney. Any observed water condensation signifies the flame is indeed ignited. a. If the flame has not ignited, recheck all flow rates, and attempt ignition again. If the flame cannot be lit even though the flow rates are correct, consult your
9.
FID (Flame Ionization Detector), Split/Splitless HP 6890 service and user documentation for additional information. If necessary, contact your Hewlett-Packard service representative.
47
10. With the flame lit, observe the FID signal at the display. This is the flame-on background offset. A stable value between 5 and 20 display units is acceptable criteria to continue to step 11. If an air cleaning system is being used, it is possible that the value will stabilize to a value below 5. Typically, the value may be >20 display units indicating system bakeout is necessary: a. Turn the detector off, remove the column from the detector, and cap the detector fitting. b. Reset the oven and heated zone temperature to the following values:
c. Reignite the detector, and monitor the displayed detector signal; it should rise quickly to some higher value as the FID heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. d. Reinstall the column in the detector. e. Restore the original setpoint temperatures specified in step 5, and allow the unit at least 2 hours to stabilize thermally. Observe the displayed detector signal to determine it is now within the acceptable range of between 5 and 20 display units, verify all gas flow rates, then continue to step 11. f. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. 11. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
48

[ATT 2^] [-] [2] [ZERO] [5] [0] [CHT SP] [1] [ENTER] [ENTER] [ENTER]
Press [PLOT] to begin plotting the FID signal. At an elapsed time of 1 minute, enter the following key sequence at the integrator, and allow plotting to continue for another 10 minutes:
Using the method shown, measure the plot to check for the following: Noise in the first 1-minute portion of the plot should be <24 mm in width. Wander over any given 2-minute period in the 10-minute portion of the plot should be <14 mm in width. Drift over any given 5-minute period in the 10-minute portion of the plot should be <30 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
Press [PLOT] to begin plotting the FID signal.

FID (Flame Ionization Detector), Split/Splitless At an elapsed time of 1 minute, enter the following key sequence at the HP 3396B/C or HP 3397A, and allow plotting to continue for another 10 minutes:
[ATT 2^] [-] [5] [ENTER]
49
Using the method shown, measure the plot to check for the following: When plotted at [ATT 2^] [-] [7], noise in the first 1-minute portion of the plot should be <30 mm in width. Wander over any given 5-minute portion of the plot should be <17.5 mm in width. Drift over the full 30-minute plot should be <37.5 mm in width. c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking on OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 2.0 minutes and 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen.
Page 9 of 14
Procedure no.:________________
50
FID (Flame Ionization Detector), Split/Splitless Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0382 pA. Wander (for a 2-minute time window) should be <0.0892 pA. Drift (for a 5-minute time window) should be <0.1911 pA.
4.25
3.75
3.5
3.25
2.75
10
12
14
min
12. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:

51
Press [Prep Run] to prepare the inlet for splitless injection. Press [Status] and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start]. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >125,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measured with the range 2^8 and the noise in mm at attn 2^0 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range value is five by pressing:
[LIST] [OPTION] [8]
Press [Prep Run] to prepare the inlet for splitless injection. Press [Status] and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start].
52
FID (Flame Ionization Detector), Split/Splitless The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >1,250,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (694,000 x (Noise*2^-6))/(Area C16) <= 4 pg/s with the noise measured in mm at attn 2^-6 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation Press [Prep Run] to prepare the inlet for splitless injection. Press [Status] and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start]. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >4,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (436,000 x Noise)/(Area C16) <= 4 pg/s (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 12 of 14
Procedure no.:________________

2000 1800 1600 1400 1200 1000 800 600 400 200 0 2 4 Time (min.) 6 8 C14 C15 C16
53
Page 13 of 14
Procedure no.:________________
54
Page 14 of 14
Procedure no.:________________
FID (Flame Ionization Detector), Cool On-Column
55

Title: FID (Flame Ionization Detector) Checkout Using a Cool On-Column Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no. :________________
56
Scope
Use the following procedure to verify proper FID operation with the Cool On-Column inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 5-l syringe (without needle), HP part no. 5182-0836 Needles for 0.32-mm columns (3/pk), HP part no. 5182-0831 Plunger button (10/pk) that converts HP 7673 syringes for manual use, HP part no. 5181-8866 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent FID flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gases: air and hydrogen to support the FID, helium as carrier, and nitrogen or helium as makeup 320-m capillary column on-column insert, HP part no. 19245-20525 Septum, HP part no. 5181-1261

Analog Input
Procedure no. :________________
57
INET Input
ChemStation Input
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the cool on-column capillary column inlet, install a new septum, a 320-m capillary column on-column insert, and the HP 6890 evaluation column. b. At the FID, install a 0.28-mm (0.011 in.) jet and/or the capillary column adapter, if needed, and the remaining end of the checkout column.
Page 2 of 12
Procedure no. :________________
58 2.
FID (Flame Ionization Detector), Cool On-Column At the HP 6890, verify that the FID to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
3.
Page 3 of 12
Procedure no. :________________
FID (Flame Ionization Detector), Cool On-Column a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator.
59
Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the FID to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the FID to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB Output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz. 4. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established:
Page 4 of 12 Procedure no. :________________
60
FID (Flame Ionization Detector), Cool On-Column a. For an instrument with electronic pressure and flow control, enter the following value:
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure by pressing the [Mode/Type] key and selecting Constant Pressure. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the FID, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40 C. 5. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Inlet Temperature: Oven Track Detector Temperature: 300C
Oven Program:
Allow the unit at least 30 minutes to stabilize thermally. 6. After thermal stabilization, set the following values according to the appropriate instrument. a. For an electronic pressure and flow controlled FID, input the values below by pressing the appropriate detector key to open the control screen and then entering the following flow values:
Hydrogen at 30 Air at 400 Makeup (nitrogen) at 25
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. If the detector flow rates are checked, the values should be within the limits set in step 6b for a manual flow controlled FID. b. For a manual flow controlled FID, establish the following flow rates by inserting
Revision Date 9-Jan-98 Hewlett-Packard Company Page 5 of 12 Procedure no. :________________
FID (Flame Ionization Detector), Cool On-Column the flow measurement adapter fully onto the FID collector and connecting the flowmeter:
Hydrogen at 30 2 mL/min Air at 400 30 mL/min Makeup (nitrogen) at 25 2 mL/min
61
After setting the flows above, remove the flowmeter and flow measurement adapter. 7. At the HP 6890, turn on the FID electrometer by pressing [Configure] [Front Detector] {or [Back Detector]}. Turn the electrometer on by scrolling to the electrometer line and pressing [ON]. Press [Signal 1] to display its flame-off background offset. A stable value, <2.0 display units, is acceptable criteria to continue. If not met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local HewlettPackard service representative. Ignite the FID flame by going to the appropriate Detector Control Table, scrolling down to Flame, and pressing [ON]. a. Observe the FID flame signal at the display. Successful flame ignition typically results in a permanent increase in signal output. If no appreciable increase is observed, perform the next check; otherwise, continue to step 9. b. Hold a cool, shiny, metal object, such as a chrome-plated wrench, just above the FID chimney. Any observed water condensation signifies the flame is indeed ignited. c. If the flame has not ignited, recheck all flow rates, and attempt ignition again. If the flame cannot be lit even though the flow rates are correct, consult your HP 6890 service and user documentation for additional information. If necessary, contact your Hewlett-Packard service representative. 9. With the flame lit, observe the FID signal at the display. This is the flame-on background offset. A stable value between 5 and 20 display units is acceptable criteria to continue to step 9. If an air cleaning system is being used, it is possible that the value will stabilize to a value below 5. Typically, the value may be >20 display units indicating system bakeout is necessary: a. Remove the column from the detector, and replace the cap detector fitting. b. Reset the oven and heated zone temperature to the following values:
8.
62
FID (Flame Ionization Detector), Cool On-Column c. Monitor the displayed detector signal; it should rise quickly to some higher value as the FID heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. d. Reinstall the column in the detector. e. Restore the original setpoint temperatures specified in step 4, and allow the unit at least 2 hours to stabilize thermally. Observe the displayed detector signal to determine if it is now within the acceptable range of between 5 and 20 display units, verify all gas flow rates, then continue to step 10. f. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
10. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the HP 3396B/C or HP 3397A integrator, enter the following setpoint values:
Using the method shown, measure the plot to check for the following: Noise in the first 1-minute portion of the plot should be <24 mm in width. Wander over any given 2-minute portion of the plot should be <14 mm in width.
Page 7 of 12
Procedure no. :________________
FID (Flame Ionization Detector), Cool On-Column Drift over any given 5-minute period in the 10-minute portion of the plot should be <30 mm in width.
63
If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 5 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
[ATT 2^] [-] [5] [ENTER]
Using the method shown, measure the plot to check for the following: When plotted at [ATT 2^] [-] [7] noise in the first 1-minute portion of the plot should be <30 mm in width. Wander over any given 5-minute portion of the plot should be <17.5 mm in width. Drift over the full 30-minute plot should be <37.5 mm in width.
64
FID (Flame Ionization Detector), Cool On-Column c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking on OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 2.0 minutes and 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0382 pA.
Page 9 of 12
Procedure no. :________________
FID (Flame Ionization Detector), Cool On-Column Wander (for a 2-minute time window) should be <0.0892 pA. Drift (for a 5-minute time window) should be <0.1911 pA.
65
4.25
3.75
3.5
3.25
2.75
10
12
14
min
11. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >125,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (86,800 x (Noise))/(Area C16) <= 4 pg/s with the area measured
66
FID (Flame Ionization Detector), Cool On-Column with the range 2^8 and the noise in mm at attn 2^0 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396C or HP 3397A integrator, ensure that the range value is five by pressing:
[LIST] [OPTION] [8]
[ZERO] [ATT 2^] [CHT SP] [PK WD] [THRSH] [AR REJ] [TIME] [1] [0] [7] [1] [.] [0] [4] [3] [0] [8] [.] [7] [5] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [STOP]
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >1,250,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (694,000 x (Noise*2^-6))/(Area C16) <= 4 pg/s with the noise measured in mm at attn 2^-6 (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 11 of 12
Procedure no. :________________
FID (Flame Ionization Detector), Cool On-Column c. HP 6890 HP-IB output to HP GC ChemStation
67
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >4,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.05. MDL(C) = (436,000 x Noise)/(Area C16) <= 4 pg/s (noise measured peak to peak). If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
2000 1800 1600 1400 1200 1000 800 600 400 200 0 2 4 Time (min.) 6 8 C14 C15 C16
Page 12 of 12
Procedure no. :________________
67

Title: TCD (Thermal Conductivity Detector) Checkout Using a Purged Packed Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
68 TCD (Thermal Conductivity Detector), Purged Packed
Scope
Use the following procedure to verify proper TCD operation with the purged packed inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent TCD flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gas: helium as carrier, reference, and makeup Disposable glass inserts, HP part no. 5080-8732 Septum, HP part no. 5181-1263

Analog Input
INET Input
69 TCD (Thermal Conductivity Detector), Purged Packed HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required) ChemStation Input HP GC ChemStation software loaded as part of the HP multitechnique ChemStation on an IBM-compatible personal computer with an HP-IB interface and the proper amount of memory for applications to be run. (See the HP Multitechnique ChemStation Manual for requirements.) HP-IB cable, HP part no. 8120-3445 (1 meter)
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the purged packed column inlet, install a new septum, a new O-ring (if needed), a capillary column adapter, a new insert, and the HP 6890 evaluation column. b. At the TCD, install the capillary column fitting, if necessary, and the remaining end of the checkout column.
2.
At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to helium by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to helium by pressing the [Mode/Type] key and choosing helium from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
3.
70 TCD (Thermal Conductivity Detector), Purged Packed a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the TCD to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the TCD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB Output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 5 Hz.
71 TCD (Thermal Conductivity Detector), Purged Packed 4. If present, remove the protective cap found installed on the TCD exhaust vent at the top of the detector. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control enter the following values:
5.
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant flow by pressing the [Mode/Type] key and selecting Constant Flow. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the TCD, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40C. 6. Insert the flow measurement adapter fully onto the TCD exhaust vent, and connect the flowmeter: a. For an electronic pressure and flow controlled TCD, establish the following flow rates:
Carrier (helium) at 7.7 (+ 0.5) mL/min TCD reference (helium) at 20 (+ 1) mL/min TCD makeup (helium) at 2 (+ 0.5) mL/min
Input the above values by pressing the appropriate detector key to open the control screen and then entering the flow values given above. Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. b. For a manual flow controlled TCD, establish the following flow rates:
Then remove the flowmeter and flow measurement adapter. 7. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
72 TCD (Thermal Conductivity Detector), Purged Packed

Oven Program:
Allow the unit at least 30 minutes to stabilize thermally. 8. After thermal stabilization, at the HP 6890, turn on the TCD electrically by pressing the appropriate detector key to open the control screen. Turn the filament on by toggling down to the filament line in the screen and pressing [ON]. Allow about 3 minutes for stabilization. Display the signal output to determine background offset by pressing [Signal 1]. If the detector is not assigned properly, move the cursor to the signal line. Change the signal by pressing the [Mode/Type] key, and then select the proper detector from the signal list. a. A stable offset at any value between 0.5 and 30 display units (inclusive) is acceptable. Continue to step 10. b. If offset is <0.5 display unit, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. If offset is >30 display units, there may be chemical contamination contributing to the signal. Continue to step 9.
9.
Perform a bakeout of the TCD in the following manner: a. Remove the column from the detector, and cap the detector fitting. b. Reset the TCD temperature to 400 C, and allow at least 30 minutes for thermal stabilization. c. Monitor the displayed detector signal; for chemical contamination, it should rise quickly to some higher value as the TCD heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value.
Page 6 of 12
Procedure no.:________________
73 TCD (Thermal Conductivity Detector), Purged Packed a. Restore the original setpoint temperature of 300 C, and allow at least 30 minutes for thermal stabilization. b. Observe the displayed detector signal to determine if it is now within the acceptable range of between 0.5 and 30 display units, verify all gas flow rates, then continue to step 10. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
10. To check signal noise, wander, and drift, perform the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
[ATT 2^] [0] [ENTER] [ZERO] [5] [0] [ENTER] [CHT SP] [1] [ENTER]
Press [PLOT] to begin plotting the TCD signal. Allow plotting to continue for at least 15 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <9.0 mm in width. Up to four spikes (not exceeding 18 mm) are allowed in any given portion provided they do not exceed limits. Drift or wander over any given 5-minute portion of the plot should be <22 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 7 of 12
Procedure no.:________________
74 TCD (Thermal Conductivity Detector), Purged Packed b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
Press [PLOT] to begin plotting the TCD signal. (Allow plotting to continue for at least 15 minutes.) Using the method shown, measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <11.25 mm in width. Up to four spikes (not exceeding 27.5 mm) are allowed in any given portion provided they do not exceed the limits. Drift or wander over any given 5-minute portion of the plot should be <27.5 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 8 of 12
Procedure no.:________________
75 TCD (Thermal Conductivity Detector), Purged Packed c. For HP 6890 HP-IB output to the HP ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measurements for noise (peak to peak, 6 * sd, and ASTM) and for drift and
76 TCD (Thermal Conductivity Detector), Purged Packed wander. ASTM noise should be <0.05733 display units (25 V/display unit for TCD). Wander or drift (for a 5-minute time window) should be <0.14 display units.
TCD1 A, of TCDNOISE\NOISE002.D 25 uV 13.25
13
12.75
12.5
12.25
12
11.75
11.5
10
12
14
min
11. To perform chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be
77 TCD (Thermal Conductivity Detector), Purged Packed >515,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C16 pg/mL) = (57,300,000 x Noise)/(Area C16) <= 1,000 pg/mL. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >20,130. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C16 pg/mL) = (1,790,000 x Noise)/(Area C16) <= 1,000 pg/mL. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to HP GC ChemStation Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >65.
78 TCD (Thermal Conductivity Detector), Purged Packed The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL (C16, pg/mL) = (1,125,000 x Noise)/(Area C16) <= 1,000 pg/mL. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
60
50
C14
40
C15 C16
30
20
10
0 2 4 Time (min.) 6 8
Page 12 of 12
Procedure no.:________________
79

Title: TCD (Thermal Conductivity Detector) Checkout Using a Split/Splitless Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
80
TCD (Thermal Conductivity Detector), Split/Splitless
Scope
Use the following procedure to verify proper TCD operation with the split/splitless inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent TCD flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gases: helium as carrier, makeup, and reference

Analog Input
INET Input
ChemStation Input
HP GC ChemStation software loaded as part of the HP multitechnique ChemStation
TCD (Thermal Conductivity Detector), Split/Splitless on an IBM-compatible personal computer with an HP-IB interface and the proper amount of memory for applications to be run. (See the HP Multitechnique ChemStation Manual for requirements.) HP-IB cable, HP part no. 8120-3445 (1 meter)
81
Related SOPs
Inlet septum, installation, SOP no. _____________ Liner/insert installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the capillary column inlet, install a new septum, a new split liner, an O-ring seal, and the HP 6890 evaluation column. b. At the TCD, install the capillary column, if necessary, and the remaining end of the HP 6890 evaluation column. 2. At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to helium by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to helium by pressing the [Mode/Type] key and choosing helium from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination: a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the TCD to be evaluated:
3.
Switch on the integrator.

82
TCD (Thermal Conductivity Detector), Split/Splitless b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator At the HP 6890, assign Signal 1 to the TCD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 5 Hz. 4. If present, remove the protective cap found installed on the TCD exhaust vent at the top of the detector. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [Back Inlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key and selecting Splitless. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following values:
5.
6.

Column pressure = 25 psi Purge flow = 60 Purge time = 0.75 min
83
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure by pressing the [Mode/Type] key and selecting Constant Pressure. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the TCD, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40 C. Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to 50 70 mL/min. Record this value. As measured at the inlet vents using the flowmeter, set the septum purge flow rate at 5 1 mL/min. 7. Insert the flow measurement adapter fully onto the TCD exhaust vent, and connect the flowmeter: For an electronic pressure and flow controlled TCD, input the values by pressing the appropriate detector key to open the control screen and then entering the flow values given:
Carrier (helium) at 7.7 ( 0.5) mL/min TCD reference (helium) at 20 ( 1) mL/min TCD makeup (helium) at 2 ( 0.5) mL/min
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. b. For a manual flow controlled TCD, establish the following flow rates:
Carrier (helium) at 7.7 ( 0.5) mL/min TCD reference (helium) at 20 ( 1) mL/min TCD makeup (helium) at 2 ( 0.5) mL/min
Then remove the flowmeter and flow measurement adapter. 8. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Page 5 of 12
Procedure no.:________________
84
TCD (Thermal Conductivity Detector), Split/Splitless Oven Program:

9.
After thermal stabilization, at the HP 6890, turn on the TCD electrically by pressing the appropriate detector key to open the control screen. Turn the filament on by toggling down to the filament line in the screen and pressing [ON]. Allow about 3 minutes for stabilization. Display the signal output to determine background offset by pressing [Signal 1]. If the detector is not assigned properly, move the cursor to the signal line. Change the signal by pressing [Mode/Type], and then select the proper detector from the signal list. a. A stable offset at any value between 0.5 and 30 display units (inclusive) is acceptable. Continue to step 11. b. If offset is <0.5 display units, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. If offset is >30 display units, there may be chemical contamination contributing to the signal. Continue to step 10.
10. Perform a bakeout of the TCD in the following manner: a. Remove the column from the detector, and cap the detector fitting. b. Reset the TCD temperature to 400 C, and allow at least 30 minutes for thermal stabilization. c. Monitor the displayed detector signal; for chemical contamination, it should rise quickly to some higher value as the TCD heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. a. Restore the original setpoint temperature of 300 C, and allow at least 30 minutes for thermal stabilization. b. Observe the displayed detector signal to determine if it is now within the acceptable range of between 0.5 and 30 display units, verify all gas flow rates, then continue to step 11.
85
c. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. 11. To check signal noise, wander, and drift, perform the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the TCD signal. Allow plotting to continue for at least 15 minutes. Measure the plot to check for the following: Noise over any given 1 minute portion of the plot should be <9.0 mm in width. Up to four spikes (not exceeding 18 mm) are allowed in any given portion provided they do not exceed limits. Drift or wander over any given 5-minute portion of the plot should be <22 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard Service representative. b. For HP 6890 INET output to the integrator At the HP 6890, enter a range vale of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
This will give the HP 6890 method listing. At the bottom of the listing is the
86
TCD (Thermal Conductivity Detector), Split/Splitless range value for signal 1 and 2. This is the range set at the MIO (INET) card. Normally this value is set to 5. The noise can be plotted with the integrator range value (this range is designated as SIG1RANGE) set to 5. The next bulleted step is to be used with a SIG1RANGE = 5. The attenuation values have been adjusted to give the same amplitude plot as the analog. It is permissible for the user to change the SIG1RANGE value to 0 (zero) and use the same integrator settings as in step 10a. The user is referred to the HP 3396 manual for further details in how to change the SIG1RANGE value. At the integrator, enter the following setpoint values:
[ATT 2^] [-] [5] [ZERO] [5] [0] [CHT SP] [1]
Press [PLOT] to begin plotting the TCD signal. Using the method shown, measure the plot to check for the following: Noise in the first 1-minute portion of the plot should be <11.25 mm in width. Up to 4 spikes (not exceeding 27.5 mm) are allowed in any given portion provided they do not exceed limits. Wander over any given 5-minute portion of the plot should be <27.5 mm in width. Drift over the full 30-minute plot should be <53.75 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard Service representative. c. For HP 6890 HP-IB output to the HP ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK.
Page 8 of 12
Procedure no.:________________
87
From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.05733 display units (25 V/display unit for TCD). Wander or drift (for a 5-minute time window) should be <0.14 display units.
Page 9 of 12
Procedure no.:________________
88
13
12.75
12.5
12.25
12
11.75
11.5
10
12
14
min
Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >585,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C16 pg/mL) = (64,800,000 x Noise)/(Area C16) <= 1,000 pg/mL. If these criteria are not met, repeat the test. If after repeated testing the
89
criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 8 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range.
[Signal 1] [Range ^ ( )] [0] [ENTER]
At the integrator, enter the following setpoint values:

Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >23,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C16 pg/mL) = (2,025,000 x Noise)/(Area C16) <= 1,000 pg/mL. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of FID chemical checkout: Area counts for components labeled C14, C15, and C16 should each be
90
TCD (Thermal Conductivity Detector), Split/Splitless >73. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C16,pg/mL) = (1,272,000 x Noise)/(Area C16) <= 1,000 pg/mL. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
70 C14 60
C15
C16
50
40
30
20 2 4 Time (min.) 6 8
Page 12 of 12
Procedure no.:________________
91

Title: TCD (Thermal Conductivity Detector) Checkout Using a Cool On-Column Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
92 TCD (Thermal Conductivity Detector), Cool On-Column
Scope
Use the following procedure to verify proper TCD operation with the cool on-column inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 FID/TCD performance evaluation ("checkout") sample, HP part no. 18710-60170 5-l syringe (without needle), HP part no. 5182-0836 Needles for 0.32-mm columns (3/pk), HP part no. 5182-0831 Plunger button (10/pk) that converts HP 7673 syringes for manual use, HP part no. 5181-8866 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent TCD flow measurement adapter, HP part no. 19301-60660 Chromatographic-grade purity gases: helium as carrier, reference, and makeup 320-m capillary column on-column insert, HP part no. 19245-20525

Analog Input
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator
Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:__________
93 TCD (Thermal Conductivity Detector), Cool On-Column INET communication card, HP 6890 Option 510 (accessory HP G1553A) HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the cool on-column capillary column inlet, install a new septum, a 320-m capillary column on-column insert, and the HP 6890 evaluation column. b. At the TCD, install the capillary column fitting, if necessary, and the remaining end of the checkout column. 2. At the HP 6890, verify that the TCD to be evaluated has its Gas Type set to H2/He and its Sensitivity set to HIGH: a. Locate the Gas Type switch at the top of the HP 6890, adjacent to the TCD to be evaluated. If needed, set the switch to its H2/He position. b. Depending upon the particular HP 6890, do one of the following to set Sensitivity: On some HP 6890s, TCD sensitivity is set by a switch adjacent to the Gas Type switch. If a sensitivity switch is present, set it to the HIGH position.
Revision Date 9-Jan-98 Hewlett-Packard Company Page 3 2 of 12 Procedure no.:_________
94 TCD (Thermal Conductivity Detector), Cool On-Column For other HP 6890s, there is no TCD Sensitivity switch; the function is set through the keyboard. If no switch is present, enter the following key sequence to set the TCD to be evaluated to high sensitivity:
[gold] [DET] [A] {or [B]} [ON]
3.
After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination: a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the TCD to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator At the HP 6890, assign Signal 1 to the TCD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB Output to HP GC ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the
Revision Date 9-Jan-98 Hewlett-Packard Company Page 4 of 12 Procedure no.:__________
95 TCD (Thermal Conductivity Detector), Cool On-Column setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 5 Hz. 4. If present, remove the protective cap found installed on the TCD exhaust vent at the top of the detector. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following value:
Column Pressure = 25 psi
5.
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure using the [Mode/Type] key and selecting Constant Pressure. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi. Insert the flow measurement adapter onto the TCD, connect the flowmeter and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min (at an oven temperature of 40 C).
6.
Insert the flow measurement adapter fully onto the TCD exhaust vent, and connect the flowmeter: a. For an electron pressure and flow controlled TCD, establish the following flow rates:
Input the above values by pressing the appropriate detector key to open the control screen and then entering the flow values given above. Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. b. For a manual flow controlled TCD, establish the following flow rates:
Revision Date 9-Jan-98 Hewlett-Packard Company Page 5 of 12 Procedure no.:_________
96 TCD (Thermal Conductivity Detector), Cool On-Column Then remove the flowmeter and flow measurement adapter.
7.
Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values.
Inlet Temperature: Oven Track Detector Temperature: 300C
Oven Program:
Temperature: 40C Initial time: 0 min Rate 1: 25C/min Final Temperature: 90C Final Time: 0 min Rate 2: 15C/min Final temperature: 170C Final Time: 2 min
8.
After thermal stabilization, at the HP 6890, turn on the TCD electrically by pressing the appropriate detector key to open the control screen. Turn the filament on by toggling down to the filament line in the screen and pressing [ON]. Allow about 3 minutes for stabilization. Display the signal output to determine background offset by pressing [Signal 1]. If the detector is not assigned properly, move the cursor to the signal line. Change the signal by pressing the [Mode/Type] key, and then select the proper detector from the signal list. a. A stable offset at any value between 0.5 and 30 display units (inclusive) is acceptable. Continue to step 10. b. If offset is <0.5 display unit, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. If offset is >30 display units, there may be chemical contamination contributing to the signal. Continue to step 9.
9.
Perform a bakeout of the TCD in the following manner: a. Remove the column from the detector, and cap the detector fitting. a. Reset the TCD temperature to 400 C, and allow at least 30 minutes for thermal stabilization. b. Monitor the displayed detector signal; it should rise quickly to some higher
Page 6 of 12
Procedure no.:__________
97 TCD (Thermal Conductivity Detector), Cool On-Column value as the TCD heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. c. Restore the original setpoint temperature of 300 C, and allow at least 30 minutes for thermal stabilization. d. Observe the displayed detector signal to determine if it is now within the acceptable range of between 0.5 and 30 display units, verify all gas flow rates, then continue to step 10. e. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable signal level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. 10. To check signal noise, wander, and drift, perform the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] by scrolling down the control table to Range: At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the TCD signal. Allow plotting to continue for at least 15 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <9.0 mm in width. Up to four spikes (not exceeding 18 mm) are allowed in any given portion provided they do not exceed limits. Wander over any given 5-minute portion of the plot should be <22 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
98 TCD (Thermal Conductivity Detector), Cool On-Column b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
[ZERO] [5] [0] [ENTER] [ATT 2^] [-] [5] [ENTER] [CHT SP] [1] [ENTER]
Press [PLOT] to begin plotting the TCD signal. Using the method shown, measure the plot to check for the following: Noise in the first 1-minute portion of the plot should be <11.25 mm in width. Up to four spikes (not exceeding 27.5) are allowed in any given portion provided they do not exceed the limits. Wander over any given 5-minute portion of the plot should be <27.5 mm in width. Drift over the full 30-minute plot should be <53.75 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. For HP 6890 HP-IB output to the HP ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report
Revision Date 9-Jan-98 Hewlett-Packard Company Page 8 of 12
menu, choose Specify Report.

99 TCD (Thermal Conductivity Detector), Cool On-Column On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 40 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.05733 display units (25 V/display unit for TCD). Wander or drift (for a 5-minute time window) should be <0.14 display units.
Page 9 of 12
Procedure no.:_________
100 TCD (Thermal Conductivity Detector), Cool On-Column
13
12.75
12.5
12.25
12
11.75
11.5
10
12
14
min
11. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >585,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C) = (64,800,000 x (Noise*2^0))/(Area C16) <= 1,000 pg/mL with the area measured with the range 2^0 and the noise in mm at attn 2^0. If these criteria are not met, repeat the test. If after repeated testing the
Revision Date 9-Jan-98 Hewlett-Packard Company Page 10 of 12 Procedure no.:__________
101 TCD (Thermal Conductivity Detector), Cool On-Column criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >23,000. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL(C) = (2,025,000 x (Noise*2^0))/(Area C16) <= 1,000 pg/mL with the area measured with the range 2^0 and the noise in mm at attn 2^0. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to HP GC ChemStation Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the TCD chemical checkout: Area counts for components labeled C14, C15, and C16 should each be >73. The area counts ratio calculated as C14/C16 should be 1.00 + 0.10. MDL (C16, pg/mL) = (1,272,000 x Noise)/(Area C16)<= 1,000 pg/mL.
102 TCD (Thermal Conductivity Detector), Cool On-Column If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
70 C14 60
C15
C16
50
40
30
20 2 4 Time (min.) 6 8
Page 12 of 12
103

Title: ECD (Electron Capture Detector) Checkout Using a Purged Packed Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
104 ECD (Electron Capture Detector), Purged Packed
Scope
Use the following procedure to verify proper ECD operation with the purged packed inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 ECD performance evaluation ("checkout") sample, HP part no. 18713-60040 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent ECD flow measurement adapter, HP part no. 5020-8231 Chromatographic-grade purity gas: helium as carrier and nitrogen as makeup Deactivated glass insert, HP part no. 5181-3382 Disposable glass inserts, HP part no. 5080-8732 Septum, HP part no. 5181-1263

Analog Input
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series integrator INET communication card, HP 6890 Option 510 (accessory HP G1553A)
105 ECD (Electron Capture Detector), Purged Packed HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the purged packed column inlet, install a new septum, a new O-ring (if needed), a capillary column adapter, a new glass insert, and the HP 6890 evaluation column. b. At the ECD, install the makeup gas fitting and remaining end of the HP 6890 evaluation column. 2. At the HP 6890, verify that the ECD to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu.
3.
After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
Page 3 2 of 12 Procedure no.:________________
106 ECD (Electron Capture Detector), Purged Packed a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the ECD to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the ECD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the key-board. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz
Page 4 of 12
Procedure no.:________________
4.
To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following values:
Verify that the column is operating in constant flow mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant flow by pressing the [Mode/Type] key and selecting Constant Flow. Verify that the correct gas type (helium) is chosen for the inlet. Change to helium following the steps outlined in item 2. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the ECD, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40 C.
5.
If present, remove the vent line found installed on the ECD exhaust vent at the top of the detector, then insert the flow measurement adapter fully onto the ECD exhaust vent, and connect the flowmeter. a. For an electron pressure and flow controlled ECD, input the values by pressing the appropriate detector key to open the control screen and then entering the flow values:
ECD makeup (nitrogen) at 60 ( 3) mL/min ECD anode purge (nitrogen) at 6 ( 1) mL/min
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. b. For a manual flow controlled ECD establish the following flow rates by inserting the flow measurement adapter fully onto the ECD collector and connecting the flowmeter:
After setting the values above, remove the flowmeter and flow measurement adapter, and reconnect the vent line. Error! Not a valid link..
Page 5 of 12
Procedure no.:________________
108 ECD (Electron Capture Detector), Purged Packed 6. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Oven Program:
Temperature: 80C Initial time: 0 min Rate 1: 15C/min Final temperature: 180C Final time: 10 min
7.
At the HP 6890, turn on the ECD by:

[Configure] [Front Detector] {or [Back Detector]}
a. Then under the configuration screen:

Electrometer [ON]
b. Check the reference current value by [Front Detector] {or [Back Detector]}. Scroll to Reference Current, and set the value to 1.0. c. A stable value, <100 display units, is acceptable criteria to continue to step 9. The value may be much higher indicating system bakeout is necessary; continue to step 8.
8.
Perform a bakeout of the ECD in the following manner: a. Remove the column from the detector, and cap the detector fitting. b. Reset the detector, oven, and inlet temperatures to the following values using the appropriate Inlet and Detector Control Tables on the HP 6890:
Inlet Temperature: 250 C Oven Temperature: 250 C Detector Temperature: 375 C
c. Monitor the displayed detector signal; for chemical contamination, it should rise quickly to some higher value as the ECD heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. a. Restore the original setpoint temperatures specified in step 6, and allow the unit at least 30 minutes stabilize thermally.
109 ECD (Electron Capture Detector), Purged Packed b. Observe the displayed detector signal to determine if it is now less than 100 display units; if so, reinstall the column and allow at least 30 minutes for thermal stabilization. c. If the displayed signal remains below 100 display units, verify all gas flow rates, then continue to step 9. d. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
9.
To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the ECD signal and continue for at least 10 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <9 mm in width. Wander or drift over any given 10-minute portion of the plot should be <90 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 7 of 12
Procedure no.:________________
110 ECD (Electron Capture Detector), Purged Packed b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
Press [PLOT] to begin plotting the ECD signal and continue for at least 10 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <11.25 mm in width. Wander or drift over any given 10-minute portion of the plot should be <112.5 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report.
111 ECD (Electron Capture Detector), Purged Packed From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 10.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 80 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.05733. Wander or drift (for a 10-minute time window) should be <0.5733.
Page 9 of 12
Procedure no.:________________

5 Hz
75
70
65
60
55
50 0 2 4 6 8 min
10. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the integrator, enter the following setpoint values:
[ZERO] [ATT 2^] [CHT SP] [PK WD] [THRSH] [TIME] [1] [0] [ENTER] [7] [ENTER] [1] [ENTER] [.] [0] [4] [ENTER] [7] [ENTER] [1] [1] [STOP]
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD chemical checkout. MDL (lindane, pg/s) = (3366 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
[ZERO]
[1] [0]
[ENTER]

[ATT 2^] [CHT SP] [PK WD] [THRSH] [TIME] [7] [ENTER] [1] [ENTER] [.] [0] [4] [ENTER] [7] [ENTER] [1] [1] [STOP]
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD chemical checkout. MDL (lindane, pg/s) = (105.1 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s c. HP 6890 HP-IB output to the HP GC ChemStation If you are not in the Method and Run Control view, choose Method and Run Control under View. Under method, choose Save Method As, and change the name of the method file. Under the Instrument menu, choose Edit Parameters. Click on the oven icon, and input the oven program outlined in step 6. Check other parameters by choosing the appropriate icon. Exit the screen by choosing OK. Under Run Control, choose Sample Information, and change the file name. Inject 1 l of sample. If using manual injection, press Start on the GC keyboard. When the run is completed, print by going to Data Analysis view. Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of ECD chemical checkout MDL (lindane, pg/s) = (66 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s
Page 11 of 12
Procedure no.:________________
arbs
300
250
Lindane
200
Aldrin
150
100
50 0 2 4 6 8 10 min
Page 12 of 12
Procedure no.:________________
115

Title: ECD (Electron Capture Detector) Checkout Using a Split/Splitless Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
116 ECD (Electron Capture Detector), Split/Splitless
Scope
Use the following procedure to verify proper ECD operation with the split/splitless inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 ECD performance evaluation ("checkout") sample, HP part no. 18713-60040 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent ECD flow measurement adapter, HP part no. 5020-8231 Chromatographic-grade purity gases: helium as carrier and nitrogen as makeup

Analog Input
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series integrator INET communication card, HP 6890 Option 510 (accessory HP G1553A) HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the capillary column inlet, install a new septum, a new liner, an O-ring seal, and the HP 6890 evaluation column. b. At the ECD, install the makeup gas fitting and remaining end of the HP 6890 evaluation column.
2.
At the HP 6890, verify that the ECD to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu.
3.
After choosing one data handling device for the test, setup the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
Procedure no.:________________
118 ECD (Electron Capture Detector), Split/Splitless a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the ECD to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator At the HP 6890, assign Signal 1 to the appropriate ECD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the keyboard. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz.
Page 4 3 of 12
Procedure no.:________________
119 ECD (Electron Capture Detector), Split/Splitless 4. Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [Back Inlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key and selecting Splitless. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established: a. For an instrument with electronic pressure and flow control, enter the following values:
Column pressure = 25 psi Purge flow = 60 mL/min Purge Time = 0.75 min
5.
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure by pressing the [Mode/Type] key and selecting Constant Pressure. Change to helium following the steps outlined in item 3. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the ECD, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40C. Connect the flowmeter to the inlet split flow vent, and adjust the flow rate to 50 70 mL/min. Record this value. Then calculate the split ratio by dividing the split vent flow by the column flow. As measured at the inlet vent using a flowmeter, set the septum purge flow rate at 5 + 1 mL/min.
6.
If present, remove the vent line found installed on the ECD exhaust vent at the top of the detector, then insert the flow measurement adapter fully onto the ECD exhaust vent, and connect the flowmeter. a. For an electronic pressure and flow controlled ECD, input the values by pressing the appropriate detector key to open the control screen and then entering the flow values:
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow.
Procedure no.:________________
120 ECD (Electron Capture Detector), Split/Splitless b. For a manual flow controlled ECD, establish the following flow rates by inserting the flow measurement adapter fully onto the ECD collector and connecting the flowmeter.
After setting the flows above, remove the flowmeter and flow measurement adapter, and reconnect the vent line.
WARNING: 7.
Ensure the ECD is properly vented before beginning this procedure. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Oven Program:
8.

a. Then under the configuration screen:

Electrometer [ON]
b. Check the reference current value by [Front Detector] {or [Back Detector]}. Scroll to Reference Current, and set the value to 1.0. c. A stable value, <100 display units, is acceptable criteria to continue to step 10. The value may be much higher indicating a system bakeout is necessary; continue to step 9.
9.
Perform a bakeout of the ECD in the following manner: a. Remove the column from the detector, and cap the detector fitting. b. Reset oven and inlet temperatures to the following values using the appropriate Inlet and Detector Control Tables on the HP 6890:
Page 6 5 of 12
Procedure no.:________________

Inlet Temperature: 250C Oven Temperature: 250C Detector Temperature: 375C
c. Monitor the displayed detector signal; it should rise quickly to some higher value as the ECD heats to the higher temperature. Then, over a longer time, the signal should decrease to some reasonably constant value. d. Restore the original setpoint temperatures specified in step 7, and allow the unit at least 30 minutes to stabilize thermally. e. Observe the displayed detector signal to determine if it is now less than 100 display units; if so, reinstall the column and allow at least 30 minutes for stabilization. f. If the displayed detector signal remains below 100 display units, verify all gas flow rates, then continue to step 10. g. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
10. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the ECD signal, and continue for at least 10 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <9.0 mm in width.
Page 7 of 12
Procedure no.:________________
122 ECD (Electron Capture Detector), Split/Splitless Wander or drift over any given 10-minute portion of the plot should be <90 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
Press [PLOT] to begin plotting the ECD signal and continue for at least 10 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <11.25 mm in width. Wander or drift over any given 10-minute portion of the plot should be <112.5 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
123 ECD (Electron Capture Detector), Split/Splitless c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 10 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 80 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis.
Page 9 of 12
Procedure no.:________________
124 ECD (Electron Capture Detector), Split/Splitless Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed,
5 Hz
75
70
65
60
55
50 0 2 4 6 8 min
print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.05733. Wander or drift (for a 10-minute time window) should be <0.5733.
11. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range At the integrator, enter the following setpoint values:
Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run.
125 ECD (Electron Capture Detector), Split/Splitless The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD checkout. MDL (lindane, pg/s) = (3366 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD chemical checkout. MDL (lindane, pg/s) = (105.1 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation
Page 11 of 12
Procedure no.:________________
126 ECD (Electron Capture Detector), Split/Splitless If you are not in the Method and Run Control view, choose Method and Run Control under View. Under method, choose Save Method As, and change the name of the method file. Under the Instrument menu, choose Edit Parameters. Click on the oven icon, and input the oven program outlined in step 6. Check other parameters by choosing the appropriate icon. Exit the screen by choosing OK. Under Run Control, choose Sample Information, and change the file name. Inject 1 l of sample. If using manual injection, press Start on the GC keyboard. When the run is completed, print by going to Data Analysis view. Press [Prep Run] at the HP 6890 to prepare the inlet for splitless injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of ECD chemical checkout. MDL (lindane, pg/s)= (66 x Noise)/(Area Lindane) MDL (lindane) <= 0.04 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
arbs
300
Lindane
250
200
Aldrin
150
100
50 0 2 4 6 8 10 min
Page 12 of 12
Procedure no.:________________
127

Title: ECD (Electron Capture Detector) Checkout Using a Cool On-Column Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 12
Procedure no.:________________
128 ECD (Electron Capture Detector), Cool On-Column
Scope
Use the following procedure to verify proper ECD operation with the cool on-column inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 ECD performance evaluation ("checkout") sample, HP part no. 18713-60040 5-l syringe (without needle), HP part no. 5182-0836 Needles for 0.32-mm columns (3/pk), HP part no. 5182-0831 Plunger button (10/pk) converts HP 7673 syringes for manual use, HP part no. 5181-8866 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent ECD flow measurement adapter, HP part no. 5020-8231 Chromatographic-grade purity gas: helium as carrier and nitrogen as makeup 320-m capillary column on-column insert, HP part no. 19245-20525

Analog Input
INET Input
129 ECD (Electron Capture Detector), Cool On-Column HP 3396B/C or HP 3397A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Procedure
WARNING: 1. If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off the heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the cool on-column capillary inlet, install a new septum, a 320-m capillary column on-column insert, and the HP 6890 evaluation column. b. At the ECD, install the makeup gas fitting and remaining end of the HP 6890 evaluation column. 2. At the HP 6890, verify that the ECD to be evaluated has its Gas Type set to nitrogen by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to nitrogen by pressing the [Mode/Type] key and choosing nitrogen from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination:
3.
Page 3 of 12
Procedure no.:________________
130 ECD (Electron Capture Detector), Cool On-Column a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 and the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the ECD to be evaluated:
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the ECD to be evaluated:
131 ECD (Electron Capture Detector), Cool On-Column 4. To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established. a. For an instrument with electronic pressure and flow control, enter the following value:
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary change to constant pressure by pressing the [Mode/Type] key and selecting Constant Pressure. Verify that the correct gas type (helium) is chosen for the inlet. Change to helium following the steps outlined in item 2. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure to 25 psi, insert the flow measurement adapter onto the ECD, connect the flowmeter, and measure the carrier flow rate. It should be between 7.5 and 7.9 mL/min at an oven temperature of 40C.
5.
If present, remove the vent line found installed on the ECD exhaust vent at the top of the detector, then insert the flow measurement adapter fully onto the ECD exhaust vent, and connect the flowmeter: a. For an electronic pressure and flow controlled ECD input the values by pressing the appropriate detector key to open the control screen and then entering the flow values:
Check that the detector is in constant makeup mode. If it is not, scroll to Mode, press the [Mode/Type] key, and select Constant Makeup Flow. b. For a manual flow controlled ECD establish the following flow rates by inserting the flow measurement adapter fully onto the ECD collector and connecting the flowmeter:
After setting the flows above, remove the flowmeter and flow measurement adapter, and reconnect the vent line.
Error! Not a valid link..
Page 5 of 12
Procedure no.:________________
132 ECD (Electron Capture Detector), Cool On-Column 6. Using the appropriate Inlet and Detector Control Tables on the HP 6890 set the following heated zone and oven setpoint values:
Inlet Temperature: Oven track Detector Temperature: 300C
Oven Program:
7.

a. Then under the configuration screen

Electrometer [ON]
b. Check the reference current value by [Front Detector] {or [Back Detector]}. Scroll to Reference Current, and set the value to 1.0 c. A stable value, <100 display units, is acceptable criteria to continue to step 9. The value may be much higher indicating system bakeout is necessary; continue to step 8.
8.
Perform a bakeout of the ECD in the following manner: a. Remove the column from the detector, and cap the detector fitting. b. Reset the detector, oven, and inlet temperatures to the following values using the appropriate Inlet and Detector Control Tables on the HP 6890.
Inlet Temperature: Oven Track Oven Temperature: 250C Detector Temperature: 375C
c. Monitor the displayed detector signal; it should rise quickly to some higher value as the ECD heats to the higher temperatures. Then, over a longer time, the signal should decrease to some reasonably constant value. a. Restore the original setpoint temperatures specified in step 6, and allow the unit at least 30 minutes to stabilize thermally.
Page 6 of 12
Procedure no.:________________
133 ECD (Electron Capture Detector), Cool On-Column b. Observe the displayed detector signal to determine if it is now less than 100 display units; if so, reinstall the column, and allow at least 30 minutes for stabilization. c. If the displayed detector signal remains below 100 display units, verify all gas flow rates, then continue to step 9. d. If the displayed detector signal is still too great to continue, repeat the bakeout process. If repeated bakeout cycles fail to give the acceptable signal level, it may be an indication that the gases are impure. Higher purity gases and/or traps may be necessary. If cleaning the gases fails to give an acceptable level, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
9.
To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. For HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the ECD signal, and continue for at least 10 minutes. Measure the plot to check for the following: Noise over any given 1-minute portion of the plot should be <9.0 mm in width. Wander or drift over any given 10-minute portion of the plot should be <90 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 7 of 12
Procedure no.:________________
134 ECD (Electron Capture Detector), Cool On-Column b. For HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
Press [PLOT] to begin plotting the ECD signal and continue for at least 10 minutes. Noise over any given 1-minute portion of the plot should be < 11.25 mm in width. Wander or drift over any given 10 minute portion of the plot should be <112.5 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative c. For HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report.
135 ECD (Electron Capture Detector), Cool On-Column On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 10.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 80 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measure-ments for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.05733. Wander or drift (for a 10-minute time window) should be <0.5733.
Page 9 of 12
Procedure no.:________________

5 Hz
75
70
65
60
55
50 0 2 4 6 8 min
10. To perform a chemical checkout, choose the appropriate data handling device: a. HP 6890 analog output to the integrator At the integrator, enter the following setpoint values:
Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD chemical checkout. MDL (lindane, pg/s) = (3366 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 [or Signal 2] by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:

Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of the ECD chemical checkout. MDL (lindane, pg/s) = (105.1 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s c. HP 6890 HP-IB output to the HP GC ChemStation
If you are not in the Method and Run Control view, choose Method and Run Control under View. Under method, choose Save Method As, and change the name of the method file. Under the Instrument menu, choose Edit Parameters. Click on the oven icon, and input the oven program outlined in step 6. Check other parameters by choosing the appropriate icon. Exit the screen by choosing OK. Under Run Control, choose Sample Information, and change the file name. Inject 1 l of sample. If using manual injection, press Start on the GC keyboard. When the run is completed, print by going to Data Analysis view. Inject 1 l of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicates successful completion of ECD chemical checkout. MDL (lindane, pg/s) = (66 x Noise)/(Area Lindane) MDL (lindane) < = 0.04 pg/s
Page 11 of 12
Procedure no.:________________

arbs
300
250
Lindane
200
Aldrin
150
100
50 0 2 4 6 8 10 min
Page 12 of 12
Procedure no.:________________
139

Title: NPD (Nitrogen Phosphorus Detector) Checkout Using a Purged Packed Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ _____________________________________________________________
Page 1 of 14
Procedure No.:________________
140 NPD (Nitrogen Phosphorus Detector), Purged Packed
Scope
Use the following procedure to verify proper NPD operation with the purged packed inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 NPD performance evaluation ("checkout") sample, HP part no. 18789-60060 O-ring, HP part no. 5080-8898 HP Series 530 m liner, HP part no. 19244-80540 Disposable glass inserts, HP part no. 5080-8732 Septum, HP part no. 5181-1263 NPD bead/source, HP part no. G1534-60570 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent NPD flow measurement adapter, HP part no. G1534-60640 Chromatographic-grade purity gases: air and hydrogen to support the NPD, helium as carrier and as makeup
Data Handling Devices, Parts and Equipment Analog Input

HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable HP part no. G1530-60570 (2-meter, 6-pin) HP 6890A-to-HP 3396B remote start cable, HP part no. G1530-61020 (9-pin/15-pin) HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 03396-61010 (9pin/15-pin)
Revision Date 9-Jan-98 Hewlett-Packard Company Procedure No.:________________
INET Input
ChemStation Input
Related SOPs
Inlet septum, installation, SOP no. _____________ Liner/insert, installation, SOP no. _____________ NPD flow measurement adapter, installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________
Procedure
WARNING:
If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off heated zones and the oven, and allow the unit sufficient time to cool. 1. Following the SOPs cited above in the Related SOPs section, do the following: a. At the purged packed inlet, install a new septum, a new glass insert, a new O-ring (if needed), and the HP 6890 evaluation column. b. At the NPD, install an 0.011-inch jet and/or the capillary column adapter, if needed, and the remaining end of the HP 6890 evaluation column. a. If needed, install a new NPD bead/source.
Page 3 2 of 14
Procedure No.:________________
142 NPD (Nitrogen Phosphorus Detector), Purged Packed 2. At the HP 6890, verify that the NPD to be evaluated has its gas type set to helium by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to helium by pressing the [Mode/type] key and choosing helium from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination. a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 to the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 to the integrator. At the HP 6890, assign Signal 1 to the NPD to be evaluated:
3.
Switch on the integrator. b. HP 6890 INET output to the integrator Install the INET signal cables between the INET I/O connectors on the HP 6890 and the integrator. At the HP 6890, assign Signal 1 to the NPD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on
143 NPD (Nitrogen Phosphorus Detector), Purged Packed [OK] to leave the screen. This will allow you to enter setpoints from the keyboard. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz.
4.
To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established. a. For an instrument with electronic pressure and flow control, enter the following value :
Verify that the column is operating in constant flow mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure using the [Mode/Type] key and selecting Constant Flow. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure of the inlet to 25 psi. Connect the flowmeter to the exit tube of the detector. The flow should be between 5.5 and 7.0 mL/min at an oven temperature of 40 C. (The detector leaks so that all the flow does not go through the exit tube.) Connect the flowmeter to the inlet split flow vent and adjust the flow rate 60 10 mL/min
5.
After thermal stabilization, set the following flow rate values: a. For an electron pressure and flow controlled NPD, set mode to Constant Column plus Makeup, and input the following values.
Hydrogen at 3 ( 1) mL/min Air at 60 ( 5) mL/min Column plus Make-Up (Helium) at 10 ( 1) mL/min
b. To measure flows properly for the manual NPD, the bead must be removed and the NPD flow measurement adapter inserted. Connect the flowmeter. Set the following:
Hydrogen flow = 3 mL/min ( 1) mL/min Air flow = 60 mL/min ( 5) mL/min Makeup plus column flow = 10 ( 1) mL/min
Revision Date 9-Jan-98 Hewlett-Packard Company Page 5 4 of 14 Procedure No.:________________
144 NPD (Nitrogen Phosphorus Detector), Purged Packed After all flow rates are set, remove the flowmeter and flow-measurement adapter, then turn on all gas flows. 6. Using the appropriate Inlet and Detector Control Tables on the HP 6890, set the following heated zone and oven setpoint values:
Inlet Temperature: 250 C Detector Temperature: 300C Oven Temperature: 250 C
Wait 30 minutes, then reset values as shown:

Inlet Temperature: 200 C
Oven Program:
Allow the unit at least 30 minutes to stabilize thermally. 7. At the HP 6890, turn on the NPD electrometer by pressing [Configure] [Front Detector] {or [Back Detector]}. Turn the electrometer on by scrolling to the Electrometer line and pressing [ON]. Press [Signal 1] to display its background
offset. A stable value, < 3.0 display units, is acceptable criteria to continue. If not met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. When powering up the NPD, use the Auto Adjust feature of the NPD to bring the baseline(offset) up.
[Front Detector] {or [Back Detector]} [Det Control] [ON]
8.
(If the default baseline setting is not 50, key in 50 now,)

[5] [0] [ENTER]
a. If no increase in signal output has been observed even though the bead voltage line reads 4.095, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. a. If after an extended time period no stable offset can be achieved, gas flow rates may be incorrect, a new bead/source may be required, or service is required. Turn off the auto adjusting process (press the [OFF] key while the cursor is on the Adjust offset line), recheck gas flow rates and replace the bead/source. If
Revision Date 9-Jan-98 Hewlett-Packard Company Page 6 of 14 Procedure No.:________________
145 NPD (Nitrogen Phosphorus Detector), Purged Packed necessary, consult your HP 6890 service and user documentation for additional information. If still necessary, contact your local Hewlett-Packard service representative. 9. Bakeout may be required to improve baseline quality after extended storage, service, or part replacement. If necessary, perform bakeout of the NPD in the following manner. a. Turn the detector off, remove the column from the detector, and cap the detector fitting. b. For an electronic pressure and flow controlled NPD, set the mode to Constant Makeup, and set Makeup to 10 mL/min. For a manual pressure and flow controlled NPD, attach the flowmeter to the NPD vent, and adjust Makeup to approximately 9 mL/min. c. Use the Auto Adjust feature of the NPD to bring the offset up. When it approximates the target value, press [Delete] to abort the adjustment process. d. Reset the detector, oven, and inlet temperatures to the flowing values using the appropriate Inlet and Detector Control tables on the HP 6890.
e. Monitor the displayed detector signal. It should rise quickly to some higher value as the NPD heats to the higher temperature. Then oven a longer time (typically 1 hour or more), the signal should decrease to some reasonable constant value. f. Restore the original setpoints, and allow at least 30 minutes for thermal stabilization. g. Proceed to step 10 to check signal noise, wander and drift with no column installed. If results are acceptable, turn the detector off, reinstall the column, and restore the original Makeup flow parameters. Then continue the process with the column reinstalled starting with step 10. h. If the results are not acceptable, repeat the bakeout process. If repeated bakeout cycles fail to give acceptable results, install a new bead/source and repeat the process starting with step 8. If neither bakeout nor bead/source replacement is effective, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Procedure No.:________________
146 NPD (Nitrogen Phosphorus Detector), Purged Packed 10. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890:
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Procedure No.:________________
147 NPD (Nitrogen Phosphorus Detector), Purged Packed a. HP 6890 analog output to the integrator At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range At the integrator, enter the following setpoint values:
[ZERO] [ATT 2^] [CHT SP] [5] [0] [0] [1] [ENTER] [ENTER] [ENTER]
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [2] [ENTER]. Measure the plot to check for the following: Noise of the plot (first 2 minutes only) should be < 12 mm in width. Wander over any given 2-minute period (after first 2 minutes) should be <15 mm in width Drift over any given 5-minute period (after first 2 minutes) should be <30 mm in width. If these criteria are not met, repeat the test. Some adjustments to hydrogen and air flow may be necessary for optimal results. If, after repeated testing, the criteria cannot be met, stop here and consult your 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard Service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
This will give the HP 6890 method listing. At the bottom of the listing is the range value for signal 1 and 2. This is the range set at the MIO (INET) card. Normally this value is set to 5. The noise can be plotted with the integrator range value (this range is designated as SIG1RANGE) set to 5. The next bulleted step is to be used with a SIG1RANGE = 5. The attenuation values have been adjusted to give the same amplitude plot as the analog. It is permissible for the user to change the SIG1RANGE value to 0 (zero) and use the same integrator settings as in step 10a. The user is referred to the HP 3396
148 NPD (Nitrogen Phosphorus Detector), Purged Packed manual for further details in how to change the SIG1RANGE value. At the integrator, enter the following setpoi nt values:
[ZERO] [5] [0] [ENTER] [ATT 2^] [5] [ENTER] [CHT SP] [1] [ENTER]
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [-] [3] [Enter]. Measure the plot to check for the following: Noise of the plot (first 2 min only) should be < 15 mm in width. Wander over any given 2-minute period (after first 2 min) should be <18.75 mm in width. Drift over any given 5-minute period (after first 2 min) should be < 37.5 mm in width. If these criteria are not met, repeat the test. Some adjustments to hydrogen and air flow may be necessary for optimal results. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 2.0 minutes and 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK.
Revision Date 9-Jan-98 Hewlett-Packard Company Page Page10 9 of of14 14 Procedure No.:________________
149 NPD (Nitrogen Phosphorus Detector), Purged Packed Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 60 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measurements for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0765 pA. Wander (for a 2-minute time window) should be <0.0956 pA. Drift (for a 5-minute time window) should be <0.1911 pA.
NPD1 A, of NPDNOISE\NPDN0002.D pA
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Procedure No.:________________
[ZERO] [ATT 2^] [CHT SP] [AR REJ] [THRSH] [PK WD] [TIME] [1] [7] [1] [1] [7] [.] [1] [0] [0] [0] [0] [0] [4] [2] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [ENTER] [STOP]
Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >306,000 MDL (azobenzene) = 10,200*Noise/Area MDL (azobenzene) should be <0.4 pg/s Area counts for the component labeled malathion should be 575,000 MDL (malathion) = 9,600*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
[ZERO] [ATT 2^]
[1] [0] [7]

11 of 14 Page 12
[ENTER] [ENTER]
Procedure No.:________________

[CHT SP] [AR REJ] [THRSH] [PK WD] [TIME] [1] [1] [0] [0] [0] [7] [.] [0] [4] [1] [2] [ENTER] [ENTER] [ENTER] [ENTER] [STOP]
Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >12,000. MDL (azobenzene) = 319*Noise/Area MDL (azobenzene) should be <0.4 pg/s Area counts for the component labeled malathion should be >22,500. MDL (malathion) = 300*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >38. MDL (azobenzene) = 200 * Noise/Area MDL (azobenzene) should be <= 0.4 pg/s Area counts for the component labeled malathion should be >71. MDL (malathion) = 188 * Noise/Area MDL (malathion) should be <= 0.2 pg/s
152 NPD (Nitrogen Phosphorus Detector), Purged Packed If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
arbs 12
Malathion
11 10
90
Azobenzene
80
70
60
50
Octadecane
40 0 2.5 5 7.5 1 12 min
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Procedure No.:________________
153

Title: NPD (Nitrogen Phosphorus Detector) Checkout Using a Split/Splitless Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 14
Procedure No.:________________
154 NPD (Nitrogen Phosphorus Detector), Split/Splitless
Scope
Use the following procedure to verify proper NPD operation with the split/splitless inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 NPD performance evaluation ("checkout") sample, HP part no. 18789-60060 Deactivated splitless liner, HP part no. 5062-3587 Septum, HP part no. 5181-1263 NPD bead/source, HP part no. G1534-60570 10-l syringe, HP part no. 9301-0810 or equivalent Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent NPD Flow-Measurement Adapter, P/N G1534-60640 Chromatographic-grade purity gases: air and hydrogen to support the NPD, helium as carrier and as makeup

HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable HP part no. G1530-60570 (2-meter, 6-pin) HP 6890A-to-HP 3396B remote start cable, HP part no. G1530-61020 (9-pin/15-pin) HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 03396-61010 (9-pin/15-pin)
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator
155 NPD (Nitrogen Phosphorus Detector), Split/Splitless INET communication card, HP 6890 Option 510 (accessory HP G1553A) HP 3396B/C or HP 3396A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Inlet septum, installation, SOP no. _____________ Liner/insert, installation, SOP no. _____________ NPD flow measurement adapter, installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________
Procedure
WARNING:
If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off heated zones and the oven, and allow the unit sufficient time to cool. Following the SOPs cited above in the Related SOPs section, do the following: a. At the capillary column inlet, install a new septum, a new splitless liner, a new O-ring seal, and an HP 6890 evaluation column. b. At the NPD, install an 0.011-inch jet, capillary column adapter (if the detector is not capillary only), and remaining end of the HP 6890 evaluation column. c. If needed, install a new NPD bead/source.
1.
2.
At the HP 6890, verify that the NPD to be evaluated has its gas type set to helium by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to helium by pressing the [Mode/type] key and choosing nitrogen from the menu.
Page 3 of 14 Procedure No.:________________
3.
After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination. a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 to the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 to the integrator. At the HP 6890, assign Signal 1 to the NPD to be evaluated:
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the keyboard. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation.
157 NPD (Nitrogen Phosphorus Detector), Split/Splitless Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz.
4.
Verify the inlet is operating in splitless mode by pressing the [Front Inlet] or [Back Inlet] key. If not, change to the splitless mode by pressing the [Mode/Type] key and selecting Splitless.
5.
To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established. a. For an instrument with electronic pressure and flow control, enter the following values:
Column pressure (He) = 25 psi Purge Flow = 60 mL/min Purge Time = 0.75 min
Verify that the column is operating in constant pressure mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant pressure using the [Mode/Type] key and selecting Constant Pressure. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure of the inlet to 25 psi. Connect the flow meter to the exit tube of the detector. The flow should be between 5.5 and 7.0 mL/min at an oven temperature of 60 C. (The detector leaks so that all the flow does not go through the exit tube.) Connect the flowmeter to the inlet split flow vent and adjust the flow rate 60 10 mL/min.
6.
Set the following flow rates according to the appropriate instrument: a. For an electronic pressure and flow controlled NPD, input the following values by pressing the appropriate detector key to open the control screen and then entering the following flow values:
Hydrogen flow = 3 ( 1) mL/min Air flow = 60 ( 5) mL/min Makeup plus column flow (helium) = 10 mL/min

Hydrogen flow = 3 ( 1) mL/min Air flow = 60 ( 5) mL/min Makeup plus column flow = 10 mL/min
After all flow rates are set, remove the flow meter and NPD flow measurement adapter, reinstall bead/source, and turn on all detector gases.
7.
Inlet Temperature: 250C Detector Temperature: 300C Oven Temperature: 250C
Wait 30 minutes; then reset the values as shown:

Inlet Temperature: 200 C
Oven Program:
Allow the unit at least 30 minutes to stabilize thermally. 8. Press [Signal 1] to display its background offset. A stable value < 3.0 display units should be attained within 1 hour. If not, stop here and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. When powering up the NPD, use the Auto Adjust feature of the NPD to bring the baseline (offset) up.
9.
(If the default baseline setting is not 50, key in 50 now.)

[5] [0] [ENTER ]
a. If no increase in signal output has been observed even though the Bead voltage line reads 4.095, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. If after an extended time period no stable offset can be achieved, gas flow rates may be incorrect, a new bead/source may be required or service is required. Turn off the auto adjusting process (press the [OFF] key while the cursor is on the Adjust offset line), recheck gas flow rates, and replace the bead/source. If
159 NPD (Nitrogen Phosphorus Detector), Split/Splitless necessary, consult your HP 6890 service and user documentation for additional information. If still necessary, contact your local Hewlett-Packard service representative. 10. Bakeout may be required to improve baseline quality after extended storage, service, or part replacement. If necessary, perform bakeout of the NPD in the following manner. a. Turn the detector off, remove the column from the detector, and cap the detector fitting. b. For an electronic pressure and flow controlled NPD, set the mode to Constant Makeup, and set Makeup to 10 mL/min. For a manual pressure and flow controlled NPD, attach the flowmeter to the NPD vent, and adjust Makeup to approximately 9 mL/min. c. Use the Auto Adjust feature of the NPD to bring the offset up. When it approximates the target value, press [Delete] to abort the adjustment process. d. Reset the detector, oven, and inlet temperatures to the flowing values using the appropriate Inlet and Detector Control tables on the HP 6890.
e. Monitor the displayed detector signal. It should rise quickly to some higher value as the NPD heats to the higher temperature. Then oven a longer time (typically 1 hour or more), the signal should decrease to some reasonable constant value. f. Restore the original setpoints, and allow at least 30 minutes for thermal stabilization. g. Proceed to step 11 to check signal noise, wander and drift with no column installed. If results are acceptable, turn the detector off, reinstall the column, and restore the original Makeup flow parameters. Then continue the process with the column reinstalled starting with step 11. e. If the results are not acceptable, repeat the bakeout process. If repeated bakeout cycles fail to give acceptable results, install a new bead/source and repeat the process starting with step 9. If neither bakeout nor bead/source replacement is effective, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. 11. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890:
160 NPD (Nitrogen Phosphorus Detector), Split/Splitless a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [2] [Enter] Measure the plot to check for the following: Noise of the plot (first 2 minutes only) should be < 12 mm in width. Wander over any given 2-minute period (after first 2 minutes) should be < 15 mm in width Drift over any given 5-minute period (after first 2 minutes) should be <30 mm in width. If these criteria are not met, repeat the test. Some adjustments to hydrogen and air flow may be necessary for optimal results. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
This will give the HP 6890 method listing. At the bottom of the listing is the range value for signal 1 and 2. This is the range set at the MIO (INET) card. Normally this value is set to 5. The noise can be plotted with the integrator range value (this range is designated as SIG1RANGE) set to 5. The next bulleted step is to be used with a SIG1RANGE = 5. The attenuation values have been adjusted to give the same amplitude plot as the analog. It is permissible for the user to change the SIG1RANGE value to 0 (zero) and use the same integrator settings as in step 11a. The user is referred to the HP 3396 manual for further details in how to change the SIG1RANGE value.
161 NPD (Nitrogen Phosphorus Detector), Split/Splitless At the integrator, enter the following setpoint values:
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [-] [3] [Enter]. Measure the plot to check for the following: Noise of the plot (first 2 min only) should be < 15 mm in width. Wander over any given 2-minute period (after first 2 min) should be < 18.75 mm in width. Drift over any given 5-minute period (after first 2 min) should be < 37.5 mm in width. If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report menu, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time range of 2.0 minutes and 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen
162 NPD (Nitrogen Phosphorus Detector), Split/Splitless for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 60 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measurements for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0765 pA. Wander (for a 2-minute time window) should be <0.0956 pA. Drift (for a 5-minute time window) should be <0.1911 pA.
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12. To perform chemical checkout, choose the appropriate data handling device:
163 NPD (Nitrogen Phosphorus Detector), Split/Splitless a. HP 6890 analog output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Press [Prep Run] at the HP 6890 to prepare the inlet for split less injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >306,000 MDL (azobenzene) = 10,200*Noise/Area MDL (azobenzene) should be <0.4 pg/s Area counts for the component labeled malathion should be >575,000 MDL (malathion) = 9,600*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Page 11 of 14
Procedure No.:________________

Press [Prep Run] at the HP 6890 to prepare the inlet for split less injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >12,000. MDL (azobenzene) = 319*Noise/Area MDL (azobenzene) should be <0.4 pg/s Area counts for the component labeled malathion should be >22,500. MDL (malathion) = 300*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation Press [Prep Run] at the HP 6890 to prepare the inlet for split less injection. Press [Status], and wait for the message Ready for Injection. Then inject 1 L of the checkout sample, and press [Start] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >38. MDL (azobenzene) = 200 * Noise/Area MDL (azobenzene) should be <= 0.4 pg/s
165 NPD (Nitrogen Phosphorus Detector), Split/Splitless Area counts for the component labeled malathion should be >71. MDL (malathion) = 188 * Noise/Area MDL (malathion) should be <= 0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
arbs 12
Malathion
11 10
90
Azobenzene
80
70
60
50
Octadecane
40 0 2.5 5 7.5 1 12. min
Page 14 13 of 14
Procedure No.:________________
Procedure No.:________________
167 NPD (Nitrogen Phosphorus Detector), Cool On-Column

Title: NPD (Nitrogen Phosphorus Detector) Checkout Using a Cool On-Column Capillary Column Inlet
Distribution List:
__________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________ __________________________________________________________________
Page 1 of 14
Procedure No.:________________
Scope
Use the following procedure to verify proper NPD operation with the cool on-column inlet.
HP 6890 evaluation column, 30 m x 0.320 mm x 0.25 m HP-5, HP part no. 19091J-413 NPD performance evaluation ("checkout") sample, HP part no. 18789-60060 NPD bead/source, HP part no. G1534-60570 5-l syringe, HP part no. 5182-0836 (barrel), 5182-0831 (needle) Needles for 0.32-mm columns (3/pk), HP part no. 5182-0831 Plunger button (10/pk) converts HP 7673 syringes for manual use, HP part no. 5181-8866 Soap film flowmeter (500-mL volume, multirange), HP part no. 9301-0981 or equivalent NPD flow measurement adapter, HP part no. G1534-60640 Chromatographic-grade purity gases: air and hydrogen to support the NPD, helium as carrier and as makeup 320-m capillary column on-column insert (HP part no. 19245-20525

HP 3395B, HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), and HP 6890 Series (HP 3397A) integrator HP 6890A-to-HP 3396B/C or HP 3397A analog signal cable HP part no. G1530-60570 (2-meter, 6-pin) HP 6890A-to-HP 3396B remote start cable, HP part no. G1530-61020 (9-pin/15-pin) HP 6890A-to-HP 3396C or HP 3397A remote start cable, HP part no. 03396-61010 (9-pin/15-pin)
Procedure No.:________________
INET Input
HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A integrator INET communication card, HP 6890 Option 510 (accessory HP G1553A) HP 3396B/C or HP 3396A INET cable, HP part no. 82167-60003 (5-meter, two required)
ChemStation Input
Related SOPs
Inlet septum, installation, SOP no. _____________ NPD flow measurement adapter, installation, SOP no. _____________ Column adapter/makeup gas fitting, installation, SOP no. _____________ Column, installation, SOP no. _____________
Procedure
WARNING:
If the unit has been previously in operation, areas may be hot enough to cause serious burns. Switch off heated zones and the oven, and allow the unit sufficient time to cool. 1. Following the SOPs cited above in the Related SOPs section, do the following: a. At the cool on-column capillary column inlet, install a new septum, a 320-m capillary column on-column insert, and the HP 6890 evaluation column. b. At the NPD, install a 0.011-inch jet, capillary column adapter, if needed, and the remaining end of the HP 6890 Evaluation Column. c. If needed, install a new NPD bead/source.
Page 2 of 14
Procedure No.:________________
2.
At the HP 6890, verify that the NPD to be evaluated has its gas type set to helium by pressing the [Configure] [Front Detector] {or [Back Detector]}. If necessary, change the gas type to helium by pressing the [Mode/type] key and choosing helium from the menu. After choosing one data handling device for the test, set up the data path between the HP 6890 and the data handling device by choosing the appropriate combination. a. HP 6890 analog output to the integrator Install the analog signal cable from the Signal 1 output receptacle on the HP 6890 to the integrator. Install the remote start cable from the Remote receptacle on the HP 6890 to the integrator. At the HP 6890, assign Signal 1 to the NPD to be evaluated:
3.
Switch on the integrator. c. HP 6890 HP-IB output to the HP Multitechnique ChemStation This procedure assumes that the ChemStation is properly installed on the computer and connected to the HP 6890. If it is necessary to install and configure the ChemStation, please refer to the HP Multitechnique ChemStation Manual set, especially Installing Your GC ChemStation (HP part no. G2070-90001). Once the ChemStation is properly installed and configured, bring up the proper on-line instrument for the HP 6890 to be tested. Then at the ChemStation under the View menu, choose Run Method and Control View. On the Run Method and Control View, choose Instrument. From the Instrument menu, choose Edit Parameters. On the Edit Parameters screen, click on Options. On the Options screen, choose the radio button labeled No for the
Revision Date 9-Jan-98 Hewlett-Packard Company Page 4 3 of 14 Procedure No.:________________
171 NPD (Nitrogen Phosphorus Detector), Cool On-Column question Keep instrument keyboard locked after method is loaded? Click on [OK] to leave the screen. This will allow you to enter setpoints from the keyboard. You may remain in the Edit Parameters screen, and enter the setpoints directly from the ChemStation. Assign Signal 1 to the appropriate detector. On the ChemStation Edit Parameters screen, this is under Signals. Also choose Save Data All and a Data Rate of 20 Hz.
4.
To ensure carrier flow through the column during oven and zone heat-up, the following flow rates should be established. a. For an instrument with electronic pressure and flow control, enter the following value :
Verify that the column is operating in constant flow mode by pressing the [Column 1] or [Column 2] key. Toggle down to the Mode line to check the mode. If necessary, change to constant flow by pressing the [Mode/Type] key and selecting Constant Flow. b. For an instrument with manual pressure and flow control for the inlet: Set the pressure of the inlet to 25 psi. Connect the flowmeter to the exit tube of the detector. The flow should be between 5.5 and 7.0 mL/min at an oven temperature of 40 C. (The detector leaks so that all the flow does not go through the exit tube.
5.
Set the following flow rate values: a. For an electronic pressure and flow controlled NPD, set the mode to Constant Column plus Makeup, and input the following values.
Hydrogen at 3 ( 1) mL/min Air at 60 ( 5) mL/min Column plus Make-Up (Helium) at 10 mL/min
Hydrogen at 3 ( 1) mL/min Air at 60 ( 5) mL/min Column plus Make-Up (Helium) at 10 ( 1) mL/min
After all flow rates are set, remove the flowmeter and flow-measurement adapter, reinstall bead/source, then turn on all gas flows.
6.
Inlet Temperature: Oven Track Detector Temperature: 300C Oven Temperature: 250 C
Wait 30 minutes, then reset the values as shown: Oven Program:

Allow the unit at least 30 minutes to stabilize thermally. 7. At the HP 6890, turn on the NPD electrometer by pressing [Configure] [Front Detector] {or [Back Detector]}. Turn the electrometer on by scrolling to the Electrometer line and pressing [ON]. Press [Signal 1] to display its background offset. A stable value, < 3.0 display units, is acceptable criteria to continue. If not met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. When powering up the NPD, use the Auto Adjust feature of the NPD to bring the baseline(offset) up.
8.
(If the default baseline setting is not 50, key in 50 now.)

[5] [0] [ENTER]
a. If no increase in signal output has been observed even though the bead voltage line reads 4.095, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. If after an extended time period no stable offset can be achieved, gas flow rates may be incorrect, a new bead/source may be required, or service is required. Turn off the auto adjusting process (press the [OFF] key while the cursor is on the Adjust offset line), recheck gas flow rates and replace the bead/source. If necessary, consult your HP 6890 service and user documentation for additional information. If still necessary, contact your local Hewlett-Packard service representative.
9.
Bakeout may be required to improve baseline quality after extended storage, service, or part replacement. If necessary, perform bakeout of the NPD in the following manner. a. Turn the detector off, remove the column for the detector, and cap the detector fitting. b. For an electronic pressure and flow controlled NPD, set the mode to Constant Makeup, and set Makeup to 10 mL/min. For a manual pressure and flow controlled NPD, attach the flowmeter to the NPD vent, and adjust Makeup to approximately 9 mL/min. c. Use the Auto Adjust feature of the NPD to bring the offset up. When it approximates the target value, press [Delete] to abort the adjustment process. d. Reset the detector, oven, and inlet temperatures to the flowing values using the appropriate Inlet and Detector Control tables on the HP 6890.
e. Monitor the displayed detector signal. It should rise quickly to some higher value as the NPD heats to the higher temperature. Then oven a longer time (typically 1 hours or more), the signal should decrease to some reasonable constant value. f. Restore the original setpoints, and allow at least 30 minutes for thermal stabilization. g. Proceed to step 10 to check signal noise, wander and drift with no column installed. If results are acceptable, turn the detector off, reinstall the column, and restore the original Makeup flow parameters. Then continue the process with the column reinstalled starting with step 10. h. If the results are not acceptable, repeat the bakeout process. If repeated bakeout cycles fail to give acceptable results, install a new bead/source and repeat the process starting with step 8. If neither bakeout nor bead/source replacement is effective, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
Page 7 of 14
Procedure No.:________________
174 NPD (Nitrogen Phosphorus Detector), Cool On-Column 10. To check signal noise, wander, and drift, perform one of the following steps according to the data handling device connected to the HP 6890: a. HP 6890 analog output to the integrator At the HP 6890, enter a Range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range.
At the integrator, enter the following setpoint values: [ATT 2^] [0] [ENTER] [ZERO] [5] [0] [ENTER] [CHT SP] [1] [ENTER]
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [2] [ENTER]. Measure the plot to check for the following: Noise of the plot (first 2 minutes only) should be < 12 mm in width. Wander over any given 2-minute period (after first 2 minutes) should be <15 mm in width Drift over any given 5-minute period (after first 2 minutes) should be <30 mm in width. If these criteria are not met, repeat the test. Some adjustments to hydrogen and air flow may be necessary for optimal results. If, after repeated testing, the criteria cannot be met, stop here and consult your 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 (zero) for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. NOTE: For the HP 3396 Series II (HP 3396B), HP 3396 Series III (HP 3396C), or HP 6890 Series (HP 3397A) integrator, the range value can be determined by entering:
[LIST] [OP#] [6]
This will give the HP 6890 method listing. At the bottom of the listing is the range value for signal 1 and 2. This is the range set at the MIO (INET) card. Normally this value is set to 5. The noise can be plotted with the integrator range value (this range is designated as SIG1RANGE) set to 5. The next bulleted step is to be used with a SIG1RANGE = 5. The attenuation values have been adjusted to give the same amplitude plot as the analog. It is
175 NPD (Nitrogen Phosphorus Detector), Cool On-Column permissible for the user to change the SIG1RANGE value to 0 (zero) and use the same integrator settings as in step 10a. The user is referred to the HP 3396 manual for further details in how to change the SIG1RANGE value. At the integrator, enter the following setpoint values:
[ATT 2^] [ZERO] [CHT SP] [5] [5] [0] [1] [ENTER] [ENTER] [ENTER]
Press [PLOT] to begin plotting the NPD signal. After approximately 2 minutes, press [ATT 2^] [-] [3] [Enter]. Measure the plot to check for the following: Noise of the plot (first 2 min only) should be < 15 mm in width. Wander over any given 2-minute period (after first 2 min) should be <18.75 mm in width Drift over any given 5-minute period (after first 2 min) should be < 37.5 mm in width. If these criteria are not met, repeat the test. Some adjustments to hydorgen and air flow may be necessary for optimal results. If after repeated testing the criteria cannot be met, stop here, and consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation At the ChemStation under the View menu, choose Full Menu then Data Analysis. On the Data Analysis View, choose Report. From the Report menu, choose Specify Report. On the Specify Report window, choose the performance + noise Report Style for the report format. Close the window by clicking OK. From the Report menu, choose System Suitability, which will bring up a second menu. On the second menu, choose Edit Noise Ranges. (If System Suitability does not appear under the Report menu, go to the View menu, and choose Full Menu.) Once Edit Noise Ranges has been chosen, a window will appear that allows time ranges to be entered. The ChemStation calculates several different noise calculations. The ASTM noise will be used in the MDL calculation later. The ASTM noise measurement requires that the noise range be 1.01 minutes. Enter several time ranges that are 1.01 minutes. A time
176 NPD (Nitrogen Phosphorus Detector), Cool On-Column range of 5.0 minutes should also be entered. These ranges can overlap with the other ranges. Close the window by choosing OK. Under View, choose Method and Run Control. Under the Method menu, choose Save Method As, which will allow a unique method name to be chosen for the noise measurement. Once a method name has been assigned, go to the Instrument menu, and choose Edit Parameters. On the Edit Parameters screen, select the oven icon, and check that the oven temperature is 60 C. Set the initial time to 12 minutes and rate 1 to 0 C/min. (This sets up a 12-minute isothermal run.) Check the other parameters in steps 4 through 6 by choosing the appropriate icon. Then click on OK to close the Edit Parameters screen. Under Run Control, choose Sample Information. Enter a directory name and, if you choose, a file name. (This will allow you to have the file as a unique file and not as the default.) Once this is completed, close the window. Press start at the HP 6890 keyboard. This will start the noise measurement once the run is completed. (If the method has not been set up to print the report, go to Data Analysis View.) See the ChemStation manual for more instructions on Data Analysis. Under View, choose Data Analysis. Load the data file for the blank run just completed. Under Report, choose Specify Report. Choose printer and screen. Under Integration, choose Integrate. After integration is completed, print the report by choosing Print Report under Report. The report will list measurements for noise (peak to peak, 6 * sd, and ASTM) and for drift and wander. ASTM noise should be <0.0765 pA. Wander (for a 2-minute time window) should be <0.0956 pA. Drift (for a 5-minute time window) should be <0.1911 pA.
Page 10 of 14
Procedure No.:________________

54
52
50
48
46
10
min
Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >306,000. MDL (azobenzene) = 10,200*Noise/Area MDL (azobenzene) should be <0.4 pg/s
178 NPD (Nitrogen Phosphorus Detector), Cool On-Column Area counts for the component labeled malathion should be >575,000. MDL (malathion) = 9,600*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. b. HP 6890 INET output to the integrator At the HP 6890, enter a range value of 0 for Signal 1 (or Signal 2) by pressing [Signal 1] and scrolling down the control table to Range. At the integrator, enter the following setpoint values:
Inject 1 L of the checkout sample, and press [START] at the HP 6890 to begin the checkout run. The resulting chromatogram should appear similar to that shown in the chromatogram figure. The following criteria indicate successful completion of the NPD chemical checkout: Area counts for the component labeled azobenzene should be >12,000. MDL (azobenzene) = 319*Noise/Area MDL (azobenzene) should be <0.4 pg/s Area counts for the component labeled malathion should be >22,500. MDL (malathion) = 300*Noise/Area MDL (malathion) should be <0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative. c. HP 6890 HP-IB output to the HP GC ChemStation
179 NPD (Nitrogen Phosphorus Detector), Cool On-Column Area counts for the component labeled azobenzene should be >38. MDL (azobenzene) = 200 * Noise/Area MDL (azobenzene) should be <= 0.4 pg/s Area counts for the component labeled malathion should be >71. MDL (malathion) = 188 * Noise/Area MDL (malathion) should be <= 0.2 pg/s If these criteria are not met, repeat the test. If after repeated testing the criteria cannot be met, consult your HP 6890 service and user documentation for additional information. If necessary, contact your local Hewlett-Packard service representative.
arbs 120
Malathion
110 100
90
Azobenzene
80
70
60
50
Octadecane
40 0 2.5 5 7.5 10 12.5 min
Page 13 of 14
Procedure No.:________________
Page 14 of 14
Procedure No.:________________

6890 Standard Operating Procedures G1530-90380

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6890 Standard Operating Procedures G1530-90380

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Standard Operating Procedures

The HP 6890 Series Gas Chromatograph

Liner/Insert, Installation ............................................................................................................. 17 Inlet Septum, Installation............................................................................................................ 23

Using This Handbook

3 Column Adapter/Makeup Gas Fitting, Installation

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

Specific Comments, Purged Packed Column Inlet

Specific Comments, FIDs and NPDs with Packed Column Bases

Specific Comments, TCD

Specific Comments, ECD

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

Page 3 of 8 Revision Date 9-Jan-98 Hewlett-Packard Company Procedure no.:________________

Revision Date 9-Jan-98 Hewlett-Packard Company

Specific Comments, Installing Packed Columns

Specific Comments, Installing Capillary Columns

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Section A: Purged Packed Column Inlet

Revision Date 9-Jan-98 Hewlett-Packard Company

20 Liner/Insert, Installation be tightened. Tighten if necessary.

Section B: Split/Splitless Capillary Column Inlets

Revision Date 9-Jan-98 Hewlett-Packard Company

Section C: Cool On-Column Capillary Column Inlets

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

24 Inlet Septum, Installation

Revision Date 9-Jan-98 Hewlett-Packard Company

25 Inlet Septum, Installation

Section A: Purged Packed Column and Split/Splitless Capillary Column Inlets

Revision Date 9-Jan-98 Hewlett-Packard Company

Section B: Cool On-Column Capillary Column Inlets

Revision Date 9-Jan-98 Hewlett-Packard Company

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

28 FID (Flame Ionization Detector), Purged Packed

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Allow the unit at least 30 minutes to stabilize thermally.

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

At the integrator, enter the following setpoint values:

Revision Date 9-Jan-98 Hewlett-Packard Company

Revision Date 9-Jan-98 Hewlett-Packard Company

39 FID (Flame Ionization Detector), Purged Packed

Revision Date 9-Jan-98 Hewlett-Packard Company

40 FID (Flame Ionization Detector), Purged Packed

Revision Date 9-Jan-98 Hewlett-Packard Company

Procedure no. :________________

Standard Operating Procedure

Revision Date 9-Jan-98 Hewlett-Packard Company

FID (Flame Ionization Detector), Split/Splitless

Data Handling Devices, Parts and Equipment