You are on page 1of 50

O

Thermal Desorber
Sampling System
IPN 074-531-P1A

Thermal Desorber
Sampling System
IPN 074-531-P1A

www.inficon.com
2010 INFICON

re achus@inficon.com

Trademarks
The trademarks of the products mentioned in this manual are held by the companies that
produce them.
INFICON and HAPSITE ER are registered trademarks of INFICON GmbH.
Viton is a registered trademark of E. I. du Pont de Nemours and Company or its affiliates.
LEMO is a registered trademark of LEMO SA.
Teflon is a registered trademark of DuPont Co.
Tygon is a registered trademark of Saint-Gobain Performance Plastics
All other brand and product names are trademarks or registered trademarks of their respective companies.

Disclaimer
The information contained in this manual is believed to be accurate and reliable. However, INFICON assumes
no responsibility for its use and shall not be liable for any special, incidental, or consequential damages related
to the use of this product.
Due to our continuing program of product improvements, specifications are subject to change without notice.

Copyright
2010 All rights reserved.
Reproduction or adaptation of any part of this document without permission is unlawful.

Warranty
WARRANTY AND LIABILITY - LIMITATION: Seller warrants the products
manufactured by it, or by an affiliated company and sold by it, and described on
the reverse hereof, to be, for the period of warranty coverage specified below, free
from defects of materials or workmanship under normal proper use and service.
The period of warranty coverage is specified for the respective products in the
respective Seller instruction manuals for those products but shall not be less than
one (1) year from the date of shipment thereof by Seller. Seller's liability under this
warranty is limited to such of the above products or parts thereof as are returned,
transportation prepaid, to Seller's plant, not later than thirty (30) days after the
expiration of the period of warranty coverage in respect thereof and are found by
Seller's examination to have failed to function properly because of defective
workmanship or materials and not because of improper installation or misuse and
is limited to, at Seller's election, either (a) repairing and returning the product or
part thereof, or (b) furnishing a replacement product or part thereof, transportation
prepaid by Seller in either case. In the event Buyer discovers or learns that a
product does not conform to warranty, Buyer shall immediately notify Seller in
writing of such non-conformity, specifying in reasonable detail the nature of such
non-conformity. If Seller is not provided with such written notification, Seller shall
not be liable for any further damages which could have been avoided if Seller had
been provided with immediate written notification.
THIS WARRANTY IS MADE AND ACCEPTED IN LIEU OF ALL OTHER
WARRANTIES, EXPRESS OR IMPLIED, WHETHER OF MERCHANTABILITY OR
OF FITNESS FOR A PARTICULAR PURPOSE OR OTHERWISE, AS BUYER'S
EXCLUSIVE REMEDY FOR ANY DEFECTS IN THE PRODUCTS TO BE SOLD
HEREUNDER. All other obligations and liabilities of Seller, whether in contract or
tort (including negligence) or otherwise, are expressly EXCLUDED. In no event
shall Seller be liable for any costs, expenses or damages, whether direct or
indirect, special, incidental, consequential, or other, on any claim of any defective
product, in excess of the price paid by Buyer for the product plus return
transportation charges prepaid.
No warranty is made by Seller of any Seller product which has been installed,
used or operated contrary to Seller's written instruction manual or which has been
subjected to misuse, negligence or accident or has been repaired or altered by
anyone other than Seller or which has been used in a manner or for a purpose for
which the Seller product was not designed nor against any defects due to plans or
instructions supplied to Seller by or for Buyer.
This manual is intended for private use by INFICON Inc. and its customers.
Contact INFICON before reproducing its contents.
NOTE: These instructions do not provide for every contingency that may arise in
connection with the installation, operation or maintenance of this equipment.
Should you require further assistance, please contact INFICON.

www. inficon.com

re achus@inficon.com

Thermal Desorber Sampling System Operating Manual

Table Of Contents
Chapter 1
Introduction
1.1
1.2
1.2.1
1.2.2
1.2.3
1.2.4
1.2.5
1.3
1.3.1

Thermal Desorption Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1


Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Adsorbents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Thermal Desorber Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Sample Collection Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
HAPSITE Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Quantitation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
Using this Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Symbols and their Definitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4

Chapter 2
Specifications
2.1
2.2

Physical Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1


Operating Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1

Chapter 3
Default Methods
3.1
3.2
3.3

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
TD Survey Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
TD Analyze Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

Chapter 4
IPN 074-531-P1A

Thermal Desorber Sampling


4.1
4.2
4.3

Thermal Desorber Tube Selection and Conditioning . . . . . . . . . . . . . . . . . . 4-1


Sample Collection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Sample Desorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3

Chapter 5
Setup
5.1
5.2
5.2.1

Thermal Desorber Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1


Setup Procedure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1

Chapter 6
Operation
6.1
6.2
6.3

Thermal Desorber Survey Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1


Thermal Desorber Analyze Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
Method Development and Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11

TOC - 1

Thermal Desorber Sampling System Operating Manual

Chapter 7
Maintenance
7.1
7.2
7.3

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
O-ring Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
Nylon Ferrule Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3

Chapter 8
Part Numbers
8.1
8.2

Thermal Desorption System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1


Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1

Chapter 9
Customer Support
How To Contact Customer Support . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1

IPN 074-531-P1A

9.1

TOC - 2

Thermal Desorber Sampling System Operating Manual

Chapter 1
Introduction
1.1 Thermal Desorption Analysis
The Thermal Desorber Sampling System is a high sensitivity device for the
HAPSITE ER used for air sampling and analysis of volatile organic compounds
(VOCs). A small hand-held pump is used to draw the air sample through a thermal
desorption tube while collecting the VOCs onto an adsorbent packing material. The
pump flow can be adjusted for rapid, large-volume sample collection or slowed for
longer term averaging of the sampling conditions. Several thermal desorption
tubes and sample pumps can be used for simultaneous sampling of multiple sites.
Following sample collection, the thermal desorption tube is placed in the HAPSITE
accessory for thermal desorption and analysis of the collected VOCs.
Figure 1-1 Labelled Thermal Desorber Accessory
Thumbwheel

Thermal Desorber Heater

IPN 074-531-P1A

Rear Thumbwheel

LEMO
Connection

Carrier Gas Tube

1.2 Theory
1.2.1 Adsorbents
The most popular adsorbents for VOC collection are Tenax TA and several
carbon materials. Tenax TA is a polymer (2,6-diphenylene oxide) that is commonly
used for trapping compounds >C6, but smaller and more volatile molecules will
usually break through the bed and be lost. Carbon materials offer a variety of
adsorption capabilities and can be packed into the thermal desorption tube as a
single or multiple bed (up to three) in the same tube. Sorbent strength is usually

1-1

Thermal Desorber Sampling System Operating Manual

described as weak to strong, referring to the attraction and trapping of VOCs.


Multi-bed carbon tubes are packed in the order of weakest to strongest adsorbent
in the direction of sample flow. Tenax TA is a fairly weak adsorbent compared to
most carbon adsorbents. Sampling flow is always in the direction of weakest to
strongest adsorbent so the highest boiling compounds are trapped on the weaker
adsorbent and the lowest boiling compounds are trapped on the stronger
adsorbents. It is just as important the adsorbent be able to release the collected
VOCs during the desorption process. Thermal desorption occurs in the opposite
flow direction from sample collection, thus all collected VOCs are efficiently
released by passing through the same or weaker adsorbent(s).

1.2.2 Thermal Desorber Tubes

Thermal desorption tubes are purchased pre-packed with adsorbent(s) and usually
pre-conditioned to remove impurities. Initial conditioning is best performed by the
vendor as this is a fairly long process requiring a dedicated heating manifold and
nitrogen supply. The Thermal Desorber accessory is not designed to be used as a
substitute for the initial vendor conditioning. Prior to initial use of a pre-conditioned
tube, it is advisable to evaluate any background response from the tube by
analyzing it as a blank. The maximum temperature limit for the adsorbent should
never be exceeded during the conditioning or analysis process. Excessively high
temperatures will result in adsorbent breakdown that will render the thermal
desorption tube unusable and could contaminate the HAPSITE.

1.2.3 Sample Collection Process


The sample collection process begins by selecting the thermal desorption tube
packed with the appropriate adsorbent(s) to efficiently collect the VOCs of interest.
The air sample is pulled through the adsorbent(s) using a small sampling pump
connected to the thermal desorption tube. The tube must be oriented in the proper
direction as indicated by the markings on the thermal desorption tube. The sample
volume, determined by multiplying sampling flowrate by time or direct volume
readout, is used to convert quantitative HAPSITE results to analyte concentrations
in the air sample.

1-2

IPN 074-531-P1A

Volatile organic compounds can be trapped (adsorbed) on a variety of chemically


adsorbent materials. These materials exhibit unique trapping characteristics based
on composition, attractive forces and surface area. Most adsorbents also exhibit
water rejection (hydrophobic) which reduces the amount of water trapped on the
adsorbent bed and the amount of water entering the chromatography system. This
characteristic is especially important when sampling in high moisture
environments. The trapped VOCs will be released upon heating. The adsorbent
materials are packed into a tube and air samples are collected using a flow
calibrated sampling pump. The thermal desorption tube is placed in the Thermal
Desorber (TD) accessory where the collected VOCs are thermally desorbed, or
released, into an inert gas flow and transported to the HAPSITE for analysis.

Thermal Desorber Sampling System Operating Manual

Two important sampling considerations are breakthrough losses and sampling


velocity. Breakthrough losses occur when the sampling volume exceeds the
volume for which a VOC migrates through the entire adsorbent bed and the VOC
exits the thermal desorption tube. Low boiling point or highly volatile compounds
are most susceptible to breakthrough. Excessive sampling velocity (high flowrate)
through the thermal desorption tube reduces trapping efficiency and may also
contribute to breakthrough. Additional sources of breakthrough losses can occur
when either using the wrong adsorbent packing, using too large of a sampling
volume, or sampling at high ambient temperature.

1.2.4 HAPSITE Analysis


Sample analysis is a two-stage thermal desorption process. First, the thermal
desorption tube is installed in the TD accessory in the reverse direction of the
sample collection flow. With nitrogen flowing, the thermal desorption tube is heated
to desorb and transfer the collected analytes to be re-adsorbed onto the HAPSITE
concentrator. In the next step, a typical HAPSITE analysis begins by rapidly
heating the concentrator to thermally desorb and transfer a narrow band of
analytes to the head of the analytical column. As the GC/MS analysis continues,
the thermal desorption tube cools until it can be safely removed from the accessory
and resealed in the holder. The thermal desorption tube is now purged and ready
to collect the next sample.

1.2.5 Quantitation

IPN 074-531-P1A

For quantitative results, the Thermal Desorber/HAPSITE system response must


first be calibrated by analyzing standard analyte concentrations. The resulting
calibration plot of Concentration vs. Peak Area response for each analyte is used
to determine the analyte concentrations in the samples.
Standards may be purchased or prepared in the liquid or gas phase, but must be
in the gas phase for loading on the thermal desorption tube for analysis. Standards
in the gas phase, such as from a compressed gas cylinder, can be transferred to a
sampling bag and then sampled onto the thermal desorption tube using a flow
calibrated sampling pump.
Standards in the liquid phase must be converted to the gas phase to be loaded on
the thermal desorption tube. A couple of techniques for making this conversion are
injecting and volatilizing in a bag containing a known volume of nitrogen or injecting
into a heated nitrogen gas stream that volatilizes the aliquot while transferring it
onto the thermal desorption tube. A gas standard could also be transferred on to
the TD tube using this technique. See the HAPSITE ER Operating Manual Chapter
11 for more information.

1-3

Thermal Desorber Sampling System Operating Manual

1.3 Using this Manual


Please take a moment to read the following.

1.3.1 Symbols and their Definitions


NOTE: Notes provide additional information about the current topic.

CAUTION
This caution paragraph cautions against actions which
may bring about a malfunction or the loss of data.

WARNING

IPN 074-531-P1A

This warning paragraph warns of actions that may result


in physical injury.

1-4

Thermal Desorber Sampling System Operating Manual

Chapter 2
Specifications
2.1 Physical Specifications
Weight . . . . . . . . . . . . . . . . . . . . . . . 1 lb (450 g)
Dimensions (LxWxH) . . . . . . . . . . . . 7.3 in x 3.6 in x 2.9 in
(186 mm x 91 mm x 74 mm)

2.2 Operating Specifications


Operating Conditions . . . . . . . . . . . . 5 to 45C, 0-95% RH (non-condensing)
Maximum Desorption Temperature . See literature provided with thermal
desorption tubes for adsorbent limitations
Thermal Desorption
Oven Temperature Range . . . . . . . . 40 to 330C
Safety
Oven LED Green . . . . . . . . . . . . <50C, safe to remove TD tube
Oven LED Red (flashing) . . . . . . >50C, unsafe to remove TD tube
Nitrogen Carrier Gas . . . . . . . . . . . . Standard HAPSITE (700 kPa)
5 L disposable canister

IPN 074-531-P1A

Accessory Flow - 20 ml/min (head pressure


controlled, factory set)
Power Requirements
DC Power . . . . . . . . . . . . . . . . . . 24 V (dc) 5% via HAPSITE Power Adapter
80 W maximum, supplied from the HAPSITE
ER
Battery Power . . . . . . . . . . . . . . . Standard 19.2 V (dc) HAPSITE battery,
supplied from the HAPSITE ER
Software . . . . . . . . . . . . . . . . . . . . . . HAPSITE ER IQ Software
Optional Sampling Pump
Pump . . . . . . . . . . . . . . . . . . . . . SKC Pocket Pump, 20-225 ml/min
Runtime (NiMH battery) . . . . . . . 12 hours at 100 ml/min up to 20 inches water
backpressure
Sensitivity . . . . . . . . . . . . . . . . . . . . . 100 ml sample volume
Trichloroethylene (TCE) low ppbv

2-1

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

2-2

Thermal Desorber Sampling System Operating Manual

Chapter 3
Default Methods
3.1 Introduction
INFICON provides default survey and qualitative GC/MS methods. A brief
description is provided below to aid in proper method selection. The methods are
organized and named by the type of thermal desorption tube (Tenax or Carbon
adsorbents) and HAPSITE concentrator (Tenax or carbon Tri-Bed) used.
The methods are further divided by "Standard" temperature and "HT" (High
Temperature) HAPSITE parameters. Most VOCs can be analyzed using the
standard temperatures, but higher boiling point VOCs or more active compounds
may require HT settings to efficiently travel through the HAPSITE system.

3.2 TD Survey Methods


TDCarbon_Survey_Standard.mth and TDTenax_Survey_Standard.mth are
survey methods using the standard HAPSITE temperature settings for rapidly
screening VOCs.
TDCarbon_Survey_HT.mth and TDTenax_Survey_HT.mth are survey methods
using the high temperature HAPSITE settings for rapidly screening VOCs.

IPN 074-531-P1A

3.3 TD Analyze Methods


TDCarbon_Tribed_Standard.mth and TDCarbon_Tribed_HT.mth methods
provide the most versitility by utilizing carbon adsorbents for collecting and
desorbing a wide boiling point range of VOCs. Samples are collected on a carbon
adsorbent(s) single or multi-bed and desorbed with refocusing on the HAPSITE
Tri-Bed concentrator.
TDTenax_Tribed_Standard.mth and TDTenax_Tribed_HT.mth methods for
adsorbing higher boiling compounds (>C6) onto the Tenax adsorbent while
maintaining easy thermal desorption with refocusing on the HAPSITE Tri-Bed
concentrator.
TDCarbon_Tenax_Standard.mth and TDCarbon_Tenax_HT.mth methods
provide efficient sample collection on carbon adsorbents with refocusing on the
HAPSITE Tenax concentrator.
TDTenax_Tenax_Standard.mth and TDTenax_Tenax_HT.mth methods for
collecting higher boiling compounds (>C6) with refocusing on the HAPSITE Tenax
concentrator.

3-1

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

3-2

Thermal Desorber Sampling System Operating Manual

Chapter 4
Thermal Desorber Sampling
4.1 Thermal Desorber Tube Selection and Conditioning
A successful thermal desorption analysis begins with selecting a thermal
desorption tube packed with application-appropriate adsorbent(s). The target
compounds must be efficiently trapped and thermally desorbed. Packing options
include single beds of Tenax TA or several carbon adsorbents or two and three bed
combinations of carbon adsorbents. Sorbent tube selection guidelines are primarily
based on target compound carbon number (volatility). Regulatory method (for
example, EPA and NIOSH) recommendations are also useful.
Adsorbent selection guidelines:
Tenax TA. . . . . . . . . . . . . . . . . weak . . . . . . . . .(n-C7 to n-C19)
Carbopack sorbents . . . . . . . stronger . . . . . . . .(n-C3 to n-C12)
Carboxen sorbents . . . . . . . strongest . . . . . . . . (n-C2 to n-C5)
Notes:
1. Carbon number ranges are provided as a general guideline. The available
Carbopack and Carboxen sorbents will typically perform within these broad
categories.

IPN 074-531-P1A

2. Multi-bed sorbent tubes are packed in the order of the weakest to the
strongest bed in the direction of sampling flow. This sequence adsorbs the least
volatile compounds (high boiling) on the weakest sorbent bed while allowing
only the most volatile compounds to reach the strongest sorbent beds.
The thermal desorption tubes are packed, conditioned and sealed by the vendor in
individual storage containers. See Figure 4-1. Although TD tubes are ready for use
as received, it is advisable to perform a "blank" analysis to verify the tube is
VOC-free prior to sample collection. This is especially true if the tube has been
stored for an extended period of time. Performing a method analysis is usually an
effective reconditioning tool. The storage time can be extended if the conditioned
tubes are stored in a VOC-free environment.
Figure 4-1 TD Storage Container

4-1

Thermal Desorber Sampling System Operating Manual

4.2 Sample Collection


Using a short length of Tygon tubing, connect the thermal desorption tube in the
proper orientation (flow direction arrow on the tube) to a small portable sampling
pump. The air sample will be drawn directly into the thermal desorption tube. See
Figure 4-2.

Breakthrough Volume (BV) is the volume of air which may be sampled through a
thermal desorption tube before a detectable level of the analyte elutes from the
back end of the tube. The BV can be determined by placing two sorbent tubes in
series and sampling air containing a constant analyte concentration to determine
the volume at which the analyte can be detected on the back-up tube in the series.
Environmental conditions of temperature and humidity usually reduce the BV and
should also be considered. For a margin of safety against exceeding the BV, the
Safe Sampling Volume (SSV) is taken as 2/3 or 66% of the BV.
The suggested sampling flowrate limits are 20-200 mL/minute for -inch sample
tubes with the preferred range being 20-100 mL/minute. Higher sampling flow rates
and proportionally higher sampling velocities through the sorbent tube may reduce
adsorption efficiency. Regulatory methods may require the sampling pump flowrate
to be measured at the start of the sampling period and retested at the end of the
sampling period to ensure a constant flowrate was maintained. The average
flowrate should be used for calculating air concentrations.

4-2

IPN 074-531-P1A

Figure 4-2 Sampling Pump and TD Tube

Thermal Desorber Sampling System Operating Manual

Relative humidity will affect the trapping efficiency of some adsorbent packings.
Sampling may be conducted at 0-95% RH (non-condensing), but breakthrough
volume may be reduced for some compounds in high humidity conditions.
When sampling in high particulate areas, it may be necessary to install a filter
(2 m Teflon) or short length of tubing loosely packed with glass wool at the front
of the sorbent tube. The filter should be replaced frequently as it could be a source
or trap for some volatiles.
The thermal desorption tube should be sealed immediately after sampling and
analyzed as soon as possible. If not analyzed immediately, the tube should be
stored in a clean environment at 4C.

4.3 Sample Desorption


The sorbent tube is thermally desorbed in the opposite direction of the sample
collection flow (opposite direction of the arrow shown on the side of the tube) See
Figure 4-3. This orientation promotes a more efficient desorption by passing the
analytes through the same or weaker sorbent strength bed. A desorption time of
five minutes is sufficient for most applications, but can be extended in the method
if necessary. Recommended desorption temperatures are 200-300C for Tenax TA
and 250-330C for Carbon sorbents for most applications. The lowest effective
desorption temperature for the application should be used to minimize background.

CAUTION
Never exceed the temperature maximum of the least
stable sorbent in the tube.

IPN 074-531-P1A

Figure 4-3 Sample Flow Through the TD Tube

4-3

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

4-4

Thermal Desorber Sampling System Operating Manual

Chapter 5
Setup
5.1 Thermal Desorber Setup
The following procedure explains how to attach the Thermal Desorber Accessory
and install / remove thermal desorption tubes.

5.2 Setup Procedure


5.2.1 Installation
1 Unscrew the Universal Bulkhead connector and pull out the LEMO
connection to remove the air probe. See Figure 5-1.

IPN 074-531-P1A

Figure 5-1 Removing the Universal Bulkhead Connector and LEMO Connector

5-1

Thermal Desorber Sampling System Operating Manual

2 Attach the Thermal Desorber Accessory (thermal desorption tube removed) by


inserting the LEMO connection. See Figure 5-2.
Figure 5-2 Attaching the LEMO Connector to the Thermal Desorber Accessory

3 Screw in the Universal Bulkhead connector by turning clockwise until tight.


See Figure 5-3.

IPN 074-531-P1A

Figure 5-3 Attaching the Universal Bulkhead Connector to the HAPSITE

5-2

Thermal Desorber Sampling System Operating Manual

4 Touch Thermal Desorber from the pop-up box on the front panel. See Figure
5-4.
Figure 5-4 Thermal Desorber Accessory Selection

5 To verify the Thermal Desorber accessory is properly attached, touch the


Accessories icon (Figure 5-5) and make sure the Thermal Desorber
accessory is present (Figure 5-6).
Figure 5-5 Accessory Icon

IPN 074-531-P1A

Figure 5-6 Verifying Thermal Desorber Accessory is Properly Attached

5-3

Thermal Desorber Sampling System Operating Manual

6 Confirm the correct HAPSITE concentrator is installed before selecting the


method. Touch Select Method. See Figure 5-7.
Figure 5-7 Touch Select Method

7 Select the method to initiate the method preparation (heat-up, autotune and
concentrator cleanout) and touch Select. See Figure 5-8.

IPN 074-531-P1A

Figure 5-8 Select the Thermal Desorber Method

5-4

Thermal Desorber Sampling System Operating Manual

8 Allow the method to prepare. Once the method is ready, gently pull back the
Carrier Gas tube (Figure 5-9) and rotate away from the Thermal Desorber
heater.
Figure 5-9 Gently Pull Carrier Gas Tube Away From Heater

IPN 074-531-P1A

Figure 5-10 Rotate Away

5-5

Thermal Desorber Sampling System Operating Manual

9 Install a pre-conditioned thermal desorption tube into the Rear Thumb Wheel
by matching the arrow on the Thermal Desorber tube to the arrow on top of the
Thermal Desorber heater. Tighten the thumbwheel by turning clockwise until
gently tight. See Figure 5-11.

CAUTION
Using excessive force when inserting the TD tube into
the TD heater can cause the tube to break.
Figure 5-11 Installing a Pre-conditioned Thermal Desorption Tube

10 Once the TD tube is secure in the Rear Thumb Wheel, pull the Carrier Gas tube
out (Figure 5-12).

IPN 074-531-P1A

Figure 5-12 Pull Carrier Gas Tube Out

5-6

Thermal Desorber Sampling System Operating Manual

11 Rotate towards the TD heater (Figure 5-13), and gently push the thermal
desorption tube (frit end) into the TD heater until seated into the internal O-ring
(the TD tube will not go any further).

IPN 074-531-P1A

Figure 5-13 Rotate Carrier Gas to Towards Heater

5-7

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

5-8

Thermal Desorber Sampling System Operating Manual

Chapter 6
Operation
6.1 Thermal Desorber Survey Operation
TD Survey quickly provides tentative results to determine the detectability of a
compound. When the sample characteristics are unknown, a carbon thermal
desorption tube is recommended. See Chapter 4, Thermal Desorber Sampling for
instructions on analyte collection.

1 Select the Survey Method to be used. The screen will display a PREPARING
SYSTEM message. See Figure 6-1.

IPN 074-531-P1A

Figure 6-1 Preparing System

6-1

Thermal Desorber Sampling System Operating Manual

2 When the screen prompts, SYSTEM READY, install the thermal desorption
tube and touch RUN SURVEY. See Figure 6-2.
Figure 6-2 System Ready

3 During a Survey method, the thermally desorbed analytes will bypass the GC
column and be detected directly by the mass spectrometer. See Figure 6-3.

IPN 074-531-P1A

Figure 6-3 Running Survey

6-2

Thermal Desorber Sampling System Operating Manual

4 Continue to run Survey until the TD tube is completely desorbed (at least five
minutes). Touch STOP to end the run. See Figure 6-4.
Figure 6-4 Stopping Survey

NOTE: The TD tube is considered to be clean when the baseline is flat and steady.

5 To ensure the TD tube is cleaned, run a GCMS blank before storage or


sampling.

6 The TD tube can be removed when the oven temperature LED is green (see
Figure 6-5).

WARNING

IPN 074-531-P1A

DO NOT remove the TD tube while the temperature LED


is flashing red.

CAUTION
More that one quarter turn will dislodge the nylon ferrule.
Figure 6-5 Green LED

6-3

Thermal Desorber Sampling System Operating Manual

7 Pull back the Carrier Gas tube to remove the TD tube from the internal O-ring
(Figure 6-6) and rotate away from the TD heater (Figure 6-7).
Figure 6-6 Remove TD Tube from Heater

IPN 074-531-P1A

Figure 6-7 Rotate TD Tube Away From the Heater

6-4

Thermal Desorber Sampling System Operating Manual

8 Loosen the Rear Thumbwheel a quarter turn on the connector to remove the
tube (Figure 6-8).
Figure 6-8 Loosen Back Thumbwheel Counterclockwise

9 Seal the TD tube in its original storage container and store in a clean
environment until ready for sample collection.

IPN 074-531-P1A

Figure 6-9 TD Tube in Storage Container

6-5

Thermal Desorber Sampling System Operating Manual

6.2 Thermal Desorber Analyze Operation


Before sampling, run the TD tube as a blank if the tube has been in storage for an
extended period of time or if the tube condition is uncertain.
Thermal desorber ANALYZE methods perform a sequence of analyte refocusing
on the HAPSITE concentrator, GC separation, and MS detection for analyte
identification. The Analyze mode of operation combines definitive identification
with the most sensitivity. See Chapter 4, Thermal Desorber Sampling, for
instructions on analyte collection.

1 Select the Analyze method to be used (see section 5.2.1 for how to select
methods). The screen will display a PREPARING SYSTEM message. See
Figure 6-10.

IPN 074-531-P1A

Figure 6-10 Preparing System

6-6

Thermal Desorber Sampling System Operating Manual

2 When the screen prompts, SYSTEM READY, install the TD tube and touch
RUN ANALYZE. See Figure 6-11.
Figure 6-11 System Ready

3 The Thermal Desorber will begin heating, and the LED indicator light on the
acessory will blink red.See Figure 6-12.

WARNING
DO NOT remove the TD tube while the temperature LED
is flashing red. TD tube is extremely hot and can cause
personal injury if handled.

IPN 074-531-P1A

Figure 6-12 Red LED

6-7

Thermal Desorber Sampling System Operating Manual

4 The TD tube thermal desorption will begin and the Enter Thermal Desorber
Volume screen will be displayed (Figure 6-13). The sample volume can be
directly entered in units of Liters or milliliters or calculated by the HAPSITE
ER software by entering the Flow rate and Time. The sample volume becomes
part of the data file. No Volume or Cancel can be selected when volume
information does not apply (qualitative analyses).

IPN 074-531-P1A

Figure 6-13 Volume Entry

6-8

Thermal Desorber Sampling System Operating Manual

5 The Thermal Desorber accessory will begin heating the TD tube while
simultaneously purging with nitrogen to collect the desorbed analytes onto the
HAPSITE concentrator. The sampling volume can be edited anytime during the
run by touching the current volume as displayed in the lower right corner on the
front panel. See Figure 6-14.
Figure 6-14 Desorbing

6 Once at the final temperature, the thermal desorber will maintain this
temperature for the remainder of the desorption. See Figure 6-15.

IPN 074-531-P1A

Figure 6-15 Desorption at Final Temp

7 The desorbed analytes are then loaded onto the HAPSITE concentrator,
desorbed again from the concentrator onto the GC column where they are
separated, and directed to the the mass spectrometer for identification.

6-9

Thermal Desorber Sampling System Operating Manual

8 The GRAPH view will be the default display while the method is running. See
Figure 6-16. To view the identified compounds in a list format, touch CMPD ID.
See Figure 6-17.
Figure 6-16 Running Analyze - GRAPH View

IPN 074-531-P1A

Figure 6-17 Running Analyze - CMPD ID View

6 - 10

Thermal Desorber Sampling System Operating Manual

9 Upon completion of the run, a METHOD FINISHED message will be displayed.


See Figure 6-18.
Figure 6-18 Analyze Method Finished

10 The TD tube can be removed when the oven temperature LED is green. Pull
back the Carrier Gas tube to remove the TD tube from the heater. Loosen the
Rear Thumb wheel to remove the tube. Seal the TD tube in a TDS3 storage
container and store in a clean environment until ready for sample collection.
Refer to Figure 6-5 through Figure 6-9.

IPN 074-531-P1A

WARNING
DO NOT remove the TD tube while the temperature LED
is flashing red. The TD tube is extremely hot and can
cause personal injury if handled.

6.3 Method Development and Calibration


See Chapters 10 and 11 in the 074-471 HAPSITE ER Operating Manual for more
information.

6 - 11

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

6 - 12

Thermal Desorber Sampling System Operating Manual

Chapter 7
Maintenance
7.1 Introduction
The Thermal Desorber has two seals that may wear with time and use.

In the TD heater there is a Viton O-ring that makes a seal between the Thermal
Desorber and the TD tube.

The seal in the Rear Thumbwheel is a nylon ferrule. The nylon ferrule serves
two functions. First, it seals the carrier gas supply to the TD tube. Second, it
acts as a clamp to secure the Carrier Gas Tube to the TD tube so that it can be
extracted from the Viton O-ring by pulling on the Carrier Gas Tube.

The Thermal Desorber has no internal volume that can become contaminated, all
sample is contained in the glass desorber tube.
The spare parts kit part number is 934-711-G1. It contains 5 O-rings and 5 ferrules.
Replace the seals if you suspect a leak, when the tube is difficult to be extracted,
or a tube breaks in the heater.

7.2 O-ring Replacement


1 Remove the thumbwheel from the Connector Tube assembly by loosening the
two setscrews on the side of the Thumbwheel with a 5/64" Allen wrench.

2 Remove the internal snap ring using snap ring pliers, and then the Connector
Tube assembly can easily be removed from the front end of the device. See
Figure 7-1.

IPN 074-531-P1A

Figure 7-1 Removing the Snap RIng and Connector Tube Assembly

O-ring
Nut
O-ring
Connector
Tube
Assembly
Snap Ring

Setscrews
Thumbwheel

7-1

Thermal Desorber Sampling System Operating Manual

3 Using a 1/2" and 9/16" wrench, remove the O-ring nut from the Connector Tube
assembly.

4 Remove the O-ring and clear any loose bits of O-ring from the Connector Tube
assembly.
Figure 7-2 O-Ring
Desorber tube used to
align the O-Ring when
tightening the O-ring nut

O-ring

O-ring Nut

Connector Tube Assembly

5 Install a new O-ring (refer to Figure 7-2), then insert a TD tube through the
O-ring to properly align the O-ring. Reinstall the O-ring nut with the TD tube in
place and tighten the connection.

6 Remove the TD tube and re-attach the connector tube assembly into the
desorber and reinstall the snap ring.

IPN 074-531-P1A

7 Re-attach the thumbwheel.

7-2

Thermal Desorber Sampling System Operating Manual

7.3 Nylon Ferrule Replacement


NOTE: The nylon ferrule can be replaced without tools.

1 Spin the Rear Thumbwheel off the Carrier Gas Tube assembly.
2 Replace the ferrule into the Carrier Gas Tube assembly in the orientation
shown in Figure 7-3.

CAUTION
In the tube socket there is a nylon spacer, which properly
locates the desorber tube, DO NOT disturb it.

3 Re-attach the thumbwheel.


Figure 7-3 Nylon Ferrule

Ferrule

Carrier Gas Tube Assembly

IPN 074-531-P1A

Rear Thumbwheel

7-3

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

7-4

Thermal Desorber Sampling System Operating Manual

Chapter 8
Part Numbers
8.1 Thermal Desorption System
IPN 934-708-G1 . . . . . . . . . . . . . . . . Thermal Desorber Sampling System Kit
IPN 934-296-G1 . . . . . . . . . . . . . . . . Thermal Desorber
IPN 934-448-P1 . . . . . . . . . . . . . . . . Tenax Desorber Tube
IPN 934-449-P1 . . . . . . . . . . . . . . . . Carbon Desorber Tube (Carbotrap 349)
IPN 934-710-G1 . . . . . . . . . . . . . . . . Desorber Tube Kit
IPN 934-450-P1 . . . . . . . . . . . . . . . . Thermal Desorber Shipping Case
IPN 934-451-P1 . . . . . . . . . . . . . . . . SKC Pocket Pump (Thermal Desorber
Sampling Pump)
IPN 934-452-P1 . . . . . . . . . . . . . . . . Desorber Tube Holder
IPN 934-453-P1 . . . . . . . . . . . . . . . . SKC Pocket Pump Power Adapter 120V
IPN 934-713-G1 . . . . . . . . . . . . . . . . SKC Pocket Pump Power Adapter 230V
(Europe).
IPN 934-713-G2 . . . . . . . . . . . . . . . . SKC Pocket Pump Power Adapter 230V
(UK).

IPN 074-531-P1A

IPN 934-713-G3 . . . . . . . . . . . . . . . . SKC Pocket Pump Power Adapter 230V


(China/Australia).

8.2 Maintenance
IPN 934-711-G1 . . . . . . . . . . . . . . . . Thermal Desorber Spare Parts Kit
(5 O-rings and 5 ferrules)

8-1

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

8-2

Thermal Desorber Sampling System Operating Manual

Chapter 9
Customer Support
9.1 How To Contact Customer Support
Worldwide support information regarding:

Technical Support, to contact an applications engineer with questions


regarding INFICON products and applications, or

Sales and Customer Service, to contact the INFICON Sales office nearest you,
or

Repair Service, to contact the INFICON Service Center nearest you,

is available at www.inficon.com.
If you are experiencing a problem with your instrument, please have the following
information readily available:

the serial number for your instrument,

a description of your problem,

an explanation of any corrective action that you may have already attempted,

and the exact wording of any error messages that you may have received.

IPN 074-531-P1A

To contact Customer Support, see Support at www.inficon.com.

9-1

Thermal Desorber Sampling System Operating Manual

IPN 074-531-P1A

This page is intentionally blank.

9-2

You might also like