Professional Documents
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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
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
Chapter 2
Specifications
2.1
2.2
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
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Chapter 5
Setup
5.1
5.2
5.2.1
Chapter 6
Operation
6.1
6.2
6.3
TOC - 1
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
Chapter 9
Customer Support
How To Contact Customer Support . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
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9.1
TOC - 2
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
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Rear Thumbwheel
LEMO
Connection
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 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
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1.2.5 Quantitation
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1-3
CAUTION
This caution paragraph cautions against actions which
may bring about a malfunction or the loss of data.
WARNING
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1-4
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)
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2-1
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2-2
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.
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3-1
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3-2
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.
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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
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
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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.
CAUTION
Never exceed the temperature maximum of the least
stable sorbent in the tube.
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4-3
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4-4
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.
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Figure 5-1 Removing the Universal Bulkhead Connector and LEMO Connector
5-1
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5-2
4 Touch Thermal Desorber from the pop-up box on the front panel. See Figure
5-4.
Figure 5-4 Thermal Desorber Accessory Selection
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5-3
7 Select the method to initiate the method preparation (heat-up, autotune and
concentrator cleanout) and touch Select. See Figure 5-8.
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5-4
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
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5-5
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).
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5-6
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).
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5-7
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5-8
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.
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6-1
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.
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6-2
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.
6 The TD tube can be removed when the oven temperature LED is green (see
Figure 6-5).
WARNING
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CAUTION
More that one quarter turn will dislodge the nylon ferrule.
Figure 6-5 Green LED
6-3
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
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6-4
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.
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6-5
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.
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6-6
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.
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6-7
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).
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6-8
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.
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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
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
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6 - 10
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.
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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 - 11
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6 - 12
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.
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.
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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
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
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.
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7-2
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.
Ferrule
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Rear Thumbwheel
7-3
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7-4
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
8.2 Maintenance
IPN 934-711-G1 . . . . . . . . . . . . . . . . Thermal Desorber Spare Parts Kit
(5 O-rings and 5 ferrules)
8-1
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8-2
Chapter 9
Customer Support
9.1 How To Contact Customer Support
Worldwide support information regarding:
Sales and Customer Service, to contact the INFICON Sales office nearest you,
or
is available at www.inficon.com.
If you are experiencing a problem with your instrument, please have the following
information readily available:
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.
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9-1
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9-2