074-506-P1B SPME Operating Manual

O P E R A T I N G M A N U A L

SPMESampling SystemIPN 074-506-P1B

O P E R A T I N G M A N U A L

SPMESampling SystemIPN 074-506-P1B

www.inficon.com [email protected] ©2009 INFICON

Trademarks

The trademarks of the products mentioned in this manual are held by the companies that produce them.

Carboxen™ is a trademark of Sigma-Aldrich Co.

INFICON® and HAPSITE® are registered trademarks of INFICON Inc.

LEMO® is a registered trademark of LEMO SA.

Teflon® is a registered trademark of DuPont Co.

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

©2009 All rights reserved. Reproduction or adaptation of any part of this document without permission is unlawful.

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.

Warranty

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SPME Sampling System Operating Manual

Table Of Contents

Chapter 1Introduction

1.1 Solid Phase Microextraction (SPME) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

1.2 Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

1.2.1 SPME Fibers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

1.2.2 Fibers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2

1.2.3 Desorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2

1.3 Using this Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3

1.3.1 Symbols and their Definitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3

Chapter 2Specifications

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

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

Chapter 3Default Methods

3.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.2 SPME Survey Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.3 Red Fiber Analyze Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.4 Blue Fiber Analyze Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2

3.5 Black Fiber Analyze Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2

Chapter 4Setup and Conditioning

4.1 SPME Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1

4.2 Setup Procedure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1

Chapter 5Operation

5.1 SPME Survey Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1

5.2 SPME Analyze Operation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4

Chapter 6SPME Sampling

6.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1

6.2 Sampling Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1

6.3 Sampling Cautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3

6.4 Sampling Tips. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4

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6.5 Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5

6.6 Air Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6

6.7 Aqueous Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7

6.8 Aqueous Sampling Flow Chart. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-10

Chapter 7Maintenance

7.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1

7.2 Replacing the Thermal Desorption Chamber Inner Sleeve . . . . . . . . . . . . . 7-2

Chapter 8Part Numbers

8.1 SPME Kits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1

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

Chapter 9Customer Support

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

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Chapter 1Introduction

1.1 Solid Phase Microextraction (SPME)

The Solid Phase Microextraction (SPME) Sampling System is a high sensitivity (ppb) sampling device for the HAPSITE® ER portable GC/MS used for in-situ testing of volatile organic compounds (VOCs) and semi-volatile organic compounds (SVOCs). When used in combination with the HAPSITE ER, the SPME Sampling System performs fast, qualitative analyses.

The SPME Sampling Kit consists of three fibers, a fiber holder and the SPME Sampling System which connects to the HAPSITE ER universal interface. Each SPME fiber is coated with an application specific polymer to optimize analyte collection and fibers can be interchanged as new application needs arise. The fiber, which is fixed in a lightweight, handheld holder, is exposed from its protective, needle-like housing during sample collection. After sampling, the fiber is inserted and exposed into the SPME Sampling System where analytes are desorbed from the fiber by the SPME thermal desorption chamber for analysis by the HAPSITE ER.

1.2 Theory1.2.1 SPME Fibers

Three types of fibers are used for SPME sampling: red, blue and black. The red fiber is an absorptive fiber which collects sample through analyte diffusion. (Similar to how water diffuses into a sponge.) The blue and black fibers are adsorptive and collect analytes by trapping them into pores on the fiber. The varying pore sizes on the coatings increase analyte selectivity, but these pores limit the amount of sample that can be retained. Therefore, absorptive fibers (red) are capable of higher capacity sampling than adsorptive (blue and black) fibers. However, adsorbent (blue and black) fibers are more sensitive, and in general, can detect analytes that are present in lower concentrations. This sensitivity is due the pores which increase the retention ability of the fiber.

The thickness of the coating will determine the amount of analyte that will be absorbed/adsorbed. Thicker fibers are better for retaining and trapping volatile compounds. In general, thicker fibers also have higher recoveries of analyte. Thinner fibers allow for analytes to diffuse faster onto the fiber and desorb more rapidly into the SPME Sampling System.

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The concentration of the sample is related to the amount of analyte absorbed. The relationship between the two is linear, as shown in equation [1] below.

[1]

where:

n = mass of analyte adsorbed by coating

Kfs = partition coefficient for analyte between coating and sample matrix

Vf = volume of coating

C0 = initial concentration of analyte in sample

Vs = volume of sample

1.2.2 Fibers

The red fiber is coated with polydimethylsiloxane (PDMS) for analyte absorption and has a thickness of 100 µm. It is recommended for most volatiles and semivolatiles, but nonpolar volatile analytes yield the best results. For the majority of applications, sample with the red fiber.

The blue fiber is coated with polydimethylsiloxane and divinylbenzene (PDMS/DVB) with a thickness of 65 µm to adsorb analytes. It is recommended for use with polar volatiles and for detecting chemical warfare agents, explosive taggants and explosives.

The black fiber is coated with Carboxen™ and polydimethylsiloxane with a thickness of 75 µm to adsorb analytes. It is recommended for extracting analytes with boiling points less than 220°C and molecular weights less than 90 amu due to the small size of the pores. It is also capable of sampling at low concentrations (ppb range).

1.2.3 Desorption

Once the sample has been collected, the fiber holder, when prompted by the software, should be inserted into the beige SPME holder guide located on the SPME Sampling System. The fiber will be exposed inside the thermal desorption chamber, which will heat it under flowing nitrogen to release analyte into the HAPSITE ER. The temperature of the thermal desorption chamber is method dependant. For the SPME default methods, the temperature range is between 250 and 300°C.

nKfsVfC0Vs

KfsVf Vs+----------------------------=

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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

This warning paragraph warns of actions that may result in physical injury.

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Chapter 2Specifications

2.1 Physical Specifications

SPME Sampling System

Weight . . . . . . . . . . . . . . . . . . . . 4 lb (1.8 kg)

Dimensions (L x W x H) . . . . . . . 4 in x 5 in x ¾ in(102 mm x 140 mm x 19 mm)

Red fiber. . . . . . . . . . . . . . . . . . . . . . 100 µm PDMS coating, Fused Silica/SS, 23 gauge needle

Blue fiber . . . . . . . . . . . . . . . . . . . . . 65 µm PDMS/DVB coating, Fused Silica/SS, 23 gauge needle

Black fiber. . . . . . . . . . . . . . . . . . . . . 100 µm CarboxenTM / PDMS coating, Fused Silica/SS, 23 gauge needle

2.2 Operating Specifications

Operating Conditions . . . . . . . . . . . . Operating: 5 to 45°C, 0-95% RH (non-condensing)

Fiber pH

Red fiber . . . . . . . . . . . . . . . . . . 2-10

Blue fiber . . . . . . . . . . . . . . . . . . 2-11

Black fiber . . . . . . . . . . . . . . . . . 2-11

Maximum Operating Temperature

Red fiber . . . . . . . . . . . . . . . . . . . 280°C

Blue fiber . . . . . . . . . . . . . . . . . . 270°C

Black fiber . . . . . . . . . . . . . . . . . 300°C

Thermal Desorption

Chamber Temperature . . . . . . . . 100 to 300°C

N2 Carrier Gas . . . . . . . . . . . . . . . . . Standard HAPSITE (700 kPa) 5 L disposable canister

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Internal Standard Gas . . . . . . . . . . . Standard HAPSITE (700 kPa) 5 L disposable canister: 50 ppmv Bromopentafluorobenzene and 100 ppmv 1,3,5 tris (trifluoromethyl) benzene

SPME fiber seal life (typical) . . . . . . 200 injections

SPME liner . . . . . . . . . . . . . . . . . . . . Deactivated stainless steel with intrinsic 2 µ particle filter, removable/replaceable

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

Sensitivity in Water. . . . . . . . . . . . . . Trichloroethylene (TCE) low ppb

Sensitivity in Air . . . . . . . . . . . . . . . . Trichloroethylene (TCE) low ppb

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Chapter 3Default Methods

3.1 Introduction

INFICON has developed five default qualitative SPME methods. A brief description of each method is provided below to aid the proper selection of a fiber and method.

3.2 SPME Survey Methods

Each fiber has a specific Survey method. The red fiber method, SPME_Survey_Red, is the first method that should be run when sampling an unknown compound. If a response is seen in Survey, a red fiber Analyze method will be initiated to confirm Survey results.

If there is not a response, complete the sampling procedure in Chapter 6, SPME Sampling. If no response is seen after completing the sampling procedure, a Survey method for the blue method, SPME Survey_Blue, or black method SPME_Survey_Black, can be run. If the compound is known, see the Analyze Methods sections below for advice on choosing the appropriate fibers.

3.3 Red Fiber Analyze Methods

The 100 µm PDMS red fiber has two default analysis methods:

SPME_Tri-Bed_Red_Standard.mth is 10 minute 40 second qualitative method with a Scan Range of 41-300 AMU. This method has a SPME target setting of 250°C and the maximum temperature of the GC is 180°C. This method will be used with the majority of samples, but yields the best results with nonpolar volatile analytes.

The SPME_Tri-Bed_Red_HT.mth is a 15 minute qualitative method with a Scan Range of 41-300 AMU. The HT stands for high temperature. The SPME target setting is 260°C and the maximum temperature of the GC is 200°C. This method is recommended for nonpolar volatiles with higher boiling points and semivolatiles.

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3.4 Blue Fiber Analyze Methods

The blue 65 µm PDMS/DVB fiber has a standard and high temperature method:

SPME_Tri-Bed_Blue_Standard.mth is an 10 minute 40 second qualitative method with a Scan Range of 41-300 AMU. The target setting for the SPME is 250°C and the maximum GC temperature is 180°C. This method is recommended for sampling polar volatiles with lower boiling points.

The high temperature method for the blue 65 µm PDMS/DVB fiber is SPME_Tri-Bed_Blue_HT.mth. This method is a 15 minute qualitative method with a Scan Range of 41-300 AMU. The SPME target setting is 250°C and the maximum GC temperature setting is 200°C. This method is recommended for sampling polar compounds with high boiling points, as well as CWAs, explosives and explosive taggants.

3.5 Black Fiber Analyze Method

The method for the black 75 µm Carboxen/PDMS fiber is SPME_Tri-Bed_Blue_Standard.mth. The target setting for the SPME is 290°C and the maximum temperature setting for the GC is 180°C. The black fiber is used for sampling analytes that have a boiling point of less than 220°C and a molecular weight less than 90 amu. It is also recommended for trace analysis, can detect compounds into the ppb range and can be used for both polar and non-polar compounds.

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Chapter 4Setup and Conditioning

4.1 SPME Setup

The following procedure explains how to attach the SPME Sampling System, expose and retract the fiber and condition the fiber for use. It is recommended that the fiber be conditioned prior to each use by running the Short Conditioning method. If a fiber is new or has been stored for an extended period of time, the Long Conditioning method should be run.

4.2 Setup Procedure

1 Unscrew the Universal Bulkhead connector and pull out the LEMO® connection to remove the probe. See Figure 4-1.

Figure 4-1 Disconnecting Probe

Pull outLEMO connection

Unscrew and remove Universal Bulkhead Connector

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2 Attach the SPME Sampling System by inserting the LEMO connection. See Figure 4-2.

Figure 4-2 Inserting the LEMO connection

3 Screw in the Universal Bulkhead connector by turning clockwise until tight. See Figure 4-3.

Figure 4-3 Connecting the Universal Bulkhead connector

SPME

SPME

Tighten

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4 Unscrew the adjustable depth gauge. See Figure 4-4.

5 Unscrew the retaining nut. See Figure 4-4.

6 Slide the plunger retaining screw. See Figure 4-4.

Figure 4-4 SPME Fiber Installation

7 Screw the color coded hub into barrel and finger tighten. See Figure 4-5.

8 Retract the plunger retaining screw. See Figure 4-5.

Figure 4-5 Fastening Fiber

9 Screw the retaining nut onto barrel and finger tighten. See Figure 4-6.

10 Screw the adjustable depth gauge onto barrel and finger tighten. See Figure 4-6.

Figure 4-6 Fastening Nut and Depth Gauge

11 Figure 4-7 shows a properly loaded fiber holder.

Figure 4-7 Loaded Fiber Holder

Retaining Nut

Adjustable Depth Gauge

Plunger

Plunger Retaining Screw

Barrel

Color Coded

Hub

Retaining Nut

Adjustable Depth Gauge

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12 To verify that the SPME Sampling System is properly attached, touch the Accessories icon. See Figure 4-8.

Figure 4-8 Accessories

13 Touch the SPME icon to view SPME options. See Figure 4-9.

Figure 4-9 SPME icon

14 Touch COND FIBER to start a fiber conditioning method. See Figure 4-10.

Figure 4-10 Conditioning Fiber

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15 Touch the conditioning method for the appropriate fiber. For this example, the red fiber will be selected. See Figure 4-11.

Figure 4-11 Red Fiber

16 Touch Select. See Figure 4-12.

Figure 4-12 Selecting FIber

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17 Touch either Long Condition or Short Condition. Then, touch Select. For this example, Long Condition will be selected. See Figure 4-13.

Figure 4-13 Conditioning

18 The SPME Sampling System will be heated to the temperature set point. See Figure 4-14.

Figure 4-14 Warming SPME

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19 When the system is heated, the INSERT SPME FIBER message will be displayed.

NOTE: Do not touch Run until the fiber holder has been placed into the SPME Sampling System and the fiber has been exposed. See Figure 4-15.

Figure 4-15 Insert SPME Fiber Message

20 Verify that the fiber is retracted. See Figure 4-16.Figure 4-16 Fiber Retracted

CAUTION

Inserting or removing the SPME fiber holder with the fiber exposed will damage the fiber and possibly the SPME accessory itself.

21 With the fiber retracted, insert the SPME fiber holder into the port. See Figure 4-17.

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Figure 4-17 Inserting SPME fiber holder

WARNING

The SPME Sampling System may be hot.

22 Expose the fiber while it is inside the thermal desorption chamber. When the fiber is exposed, the plunger will be positioned in the middle of the Z-slot. See Figure 4-18.

Figure 4-18 Exposing Fiber

23 Twist the fiber clockwise to lock the fiber into place while keeping it inserted into the thermal desorption chamber. See Figure 4-19.

Figure 4-19 Locking Fiber

24 Touch RUN.

SPME

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Figure 4-20 Run Button

25 The screen will display the Conditioning Fiber progress bar while the fiber is being conditioned. See Figure 4-21.

Figure 4-21 Conditioning Fiber

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26 When the conditioning method is finished, a message to REMOVE SPME FIBER will be displayed. See Figure 4-22. Please follow the fiber removal instructions below before touching OK.

Figure 4-22 SPME Fiber Removal Message

WARNING

The SPME fittings and fiber needle may be hot.

27 Unlock the fiber by twisting the plunger counterclockwise. See Figure 4-23.

Figure 4-23 Unlocking Fiber

28 Gently pull the plunger back to its original position. See Figure 4-24.

Figure 4-24 Retracting Fiber

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29 When the fiber is retracted, remove the SPME fiber holder. See Figure 4-25.

Figure 4-25 Removing SPME fiber holder

30 Touch OK when the fiber has been removed. See Figure 4-26.

Figure 4-26 Removing Fiber

SPME

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31 If conditioning more than one fiber, insert and expose another fiber. Then, touch Run. If finished with fiber conditioning, touch Finished. See Figure 4-27.

Figure 4-27 Finishing Conditioning

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Chapter 5Operation

5.1 SPME Survey Operation

SPME Survey quickly provides tentative results to determine the detectability of a compound. When the sample is unknown, sampling should first occur with the Red Fiber (which can sample the widest range of compounds). Based upon the response, additional SPME Survey runs with a different colored fiber may be necessary. See Chapter 3, Default Methods for instructions on selecting a fiber and Chapter 6, SPME Sampling for instructions on analyte collection.

1 The screen will display a PREPARING SURVEY message. See Figure 5-1.

Figure 5-1 Preparing Survey

2 When the screen prompts, SURVEY READY, touch RUN SURVEY. See Figure 5-2.

Figure 5-2 Run Survey

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3 The Survey method will begin and RUNNING SURVEY will be displayed at the top of the screen. Do not sample at this point. See Figure 5-3.

Figure 5-3 Running Survey

4 When the screen displays SAMPLING, wait for the baseline TIC to stabilize. See Figure 5-4.

Figure 5-4 TIC Stabilization

5 When the baseline TIC stabilizes, insert the fiber holder into the thermal desorption chamber and expose the fiber.

CAUTION


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6 Retract the fiber and remove the fiber holder when the TIC increases at least 2-3 times the baseline level. If the survey indicator bar enters the yellow or red regions, retract and remove the fiber immediately. See Figure 5-5.

NOTE: It may be necessary to keep the fiber inserted in the injection port for up to 2 minutes as the response may not be immediate and the TIC may increase slowly for semivolatiles.

Figure 5-5 Response in Survey

7 Continue to run Survey until the TIC returns to the baseline level. Touch STOP to turn off the sample pump and end the run. See Figure 5-6.

Figure 5-6 Returning to Baseline

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8 METHOD FINISHED will be displayed when the run has ended. See Figure 5-7.

Figure 5-7 Method Finished

5.2 SPME Analyze Operation

Before sampling, run a blank by exposing the fiber away from the sampling point to determine the environmental background and to verify that carryover from previous analyses is not present. If extraneous peaks from carryover are significant, either re-condition the fiber or run blanks until the number and size of the peaks is reduced. Refer to Chapter 4, Setup and Conditioning for conditioning instructions.

NOTE: While running blanks is always recommended, running blanks on the high temperature methods, SPME_Tri-Bed_Red_HT and SPME_Tri-Bed_Blue_HT, prior to running sample is imperative for accurate results.

CAUTION

Wear appropriate personal protective equipment (PPE) recommended by the compound’s MSDS or the user’s safety authority when sampling compounds using the SPME holder.

NOTE: Screenshots for the red fiber method, SPME_Tri-Bed_Red_Standard, are displayed in the following instruction sequence. However, these instructions can be applied to all SPME default methods.

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9 The screen will display a PREPARING ANALYZE message. See Figure 5-8.

Figure 5-8 Preparing Analyze

10 When the screen prompts, ANALYZE READY, touch RUN ANALYZE. See Figure 5-9.

Figure 5-9 System Ready

11 The SPME Line Purge event will begin.

Figure 5-10 Line Purge

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12 When the Line Purge event is finished, an INSERT SPME FIBER message will appear. See Figure 5-11.

Figure 5-11 Insert SPME

13 Insert the SPME holder and expose the fiber as shown in Chapter 4, Setup and Conditioning.

CAUTION

Do not insert and expose the fiber prior to receiving this message.

CAUTION


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14 Touch Run immediately after the fiber is exposed. See Figure 5-12.

CAUTION

Delaying the initiation of the run may result in a significant loss of sample.

Figure 5-12 Run Button

15 The following message will be displayed after the fiber desorption period is complete. Retract the fiber and remove the fiber holder as shown in Chapter 4, Setup and Conditioning. See Figure 5-13.

Figure 5-13 Retract Fiber

16 The Graph view will be the default display while the method is running. To view the identified compounds in a list format, touch CMPD ID. See Figure 5-14.

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Figure 5-14 GRAPH view for Blank

17 The Compound Identification view will be displayed. To return to the Graph view, touch GRAPH. See Figure 5-15.

Figure 5-15 CMPD ID View for Blank

18 Upon completion of the run, a METHOD FINISHED message will be displayed. See Figure 5-7.


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Chapter 6SPME Sampling

6.1 Introduction

Solid Phase Microextraction (SPME) is a valuable sampling technique because it provides HAPSITE ER operators with the capability of introducing and detecting semivolatile organic compounds (SVOCs) that would otherwise go undetected. The SPME sampling procedure involves exposing a specially designed and manufactured fiber to air, headspace or water. There are many varieties of fibers, most of which are designed to maximize the amount of sample collected for a particular class of compounds. If the HAPSITE ER operator is familiar with the compounds and/or concentrations to be sampled, then the type of fiber used, the sampling time and type of sample preparation can be determined relatively quickly.

However, oftentimes, sample composition and concentrations are unknown. In order to protect the HAPSITE ER from exposure to high concentrations of SVOCs (or VOCs) which can saturate the detector and force the operator to run numerous blanks to clear the system, initial sampling conditions should include short sampling times and large sample dilutions (see section 6.7 on page 6-7).

Since each compound sampled has its own set of unique physical properties that determine how readily it absorbs into, or adsorbs onto, a particular fiber, the proper set of sampling conditions may require the operator to initially run several sample injections. With proper sampling conditions established, the operator can then determine the composition of compounds, as well as roughly estimate their concentration of unknown sample.

6.2 Sampling Techniques

Direct immersion and headspace sampling are methods of collecting analytes with the SPME Sampling System.

In direct immersion sampling, the fiber is placed directly into an aqueous or gaseous sample. If using an aqueous sample, it may be stirred in a consistent manner to improve results, as stirring decreases equilibrium time and reduces variability of results. Direct immersion yields the best results when sampling low volatility compounds that are moderately to highly polar.

When headspace sampling, the fiber is placed in the vapor above the liquid or solid sample. headspace sampling is beneficial for samples with medium to high volatility and low to medium polarity. Samples will also equilibrate faster using headspace sampling than with direct immersion.

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CAUTION

Fibers are extremely fragile. Use extreme caution when handling them.

On average, fibers will last for 50 injections. However, improper sampling may lead to fiber damage. This chapter identifies ways to avoid fiber damage and optimize SPME sample collection.

Extreme care should be taken to avoid bending or breaking the needle that houses the SPME fiber. Tedlar/Teflon Bags and glass vials are two types of sampling containers. When inserting the SPME fiber into a sampling container, first adjust the needle to a depth of one inch beyond the end of the fiber holder. Pierce the septa with the needle and guide it into the vial until fully inserted.

CAUTION

To avoid fiber damage, do not pierce the septa with the fiber exposed.

While holding the black adjustable depth gauge portion of the SPME holder, twist the metal barrel with the other hand to the desired depth.

CAUTION

Over tightening the adjustable depth gauge can damage the threads of the nut.

NOTE: When exposing the fiber, ensure that the fiber does not touch the side or bottom of the sampling container.

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Figure 6-1 Proper Sampling Technique

6.3 Sampling Cautions

CAUTION

Immersing any of the SPME fibers into chlorinated solvents will damage them.

CAUTION

Fibers will swell in certain solvents which may result in the coating becoming stripped off by the needle when the fiber is retracted. The fiber can swell when using both direct immersion and headspace sampling techniques. In some cases, the fiber may actually swell more when sampling in the headspace than when sampling through direct immersion due to the volatility of the analyte being collected.

CAUTION

PDMS (Red) and PDMS/DVB (Blue) fibers should not be used to sample non-polar solvents such as hexane, methylene chloride and diethyl ether as this will cause swelling and stripping of the fiber.

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CAUTION

Do not use the Carboxen/PDMS fibers (Black) to sample organic solvents as they will be strongly retained in the micropores and will require multiple conditioning method runs to remove.

CAUTION

Wear nitrile gloves when handling the SPME holder to avoid contamination of the fiber.

6.4 Sampling Tips

Fiber exposure times will vary. Shorter exposure times can be expected for:

Compounds with a molecular weight of less than 150 amu.

Fibers with thinner, absorbent coatings.

Headspace sampling.

Samples in the high ppb to ppm range.

Factors, such as temperature and stirring, can affect the precision and accuracy of sampling data. To improve the consistency of results, ensure that the sample collection temperatures are constant. Also, consider stirring the sample, which will also reduce the sample equilibration time.

Sample volume can effect the sensitivity. When headspace sampling, sensitivity is increased when the headspace volume is 30% to 50% of the vial. To improve sensitivity when directly immersing the fiber, the sample volume should be approximately 80% of the vial. For both sampling methods, keep the sample volume size and vial size constant for result reproducibility.

Salt (e.g., sodium chloride), which reduces the solubility of some compounds, can be added to the sample to increase the amount of analytes absorbed/adsorbed by the fiber. This improves the sampling response of polar and volatile trace analytes.

Low intensity siloxane contamination peaks may be present in the chromatogram. These are due to thermal degradation of the PDMS phase of the fiber and may not be from compounds in the analyzed sample.

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6.5 Sampling

WARNING

Wear appropriate personal protective equipment (PPE) when handling chemicals as advised by the MSDS or the user’s safety organization.

NOTE: Refer to Chapter 3, Default Methods for additional information on sample selection. In general, an unknown sample should be run with a red fiber

1 If the fiber has never been used or has been stored for an extended period of time, refer to Chapter 4, Setup and Conditioning for instructions on running a long conditioning method.

1a Run a short conditioning method if the fiber has recently been conditioned. Refer to Chapter 4, Setup and Conditioning for instructions on running a short conditioning method.

2 Run a blank before running a sample. Refer to Chapter 5, Operation.

3 If running an air sample, see section 6.6. If running an aqueous sample, see section 6.7. The following screenshots depict Graph, Compound Identification (CMPD ID) and Method Finished views of a sample run with a SPME_Tri-Bed_Red_Standard method. See Figure 6-2, Figure 6-3 and Figure 6-4.Figure 6-2 Graph View

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Figure 6-3 Compound Identification View


6.6 Air Sampling

1 If the composition of the sample is unknown, expose the red fiber for a short period of time (a few seconds to a few minutes).

CAUTION

To avoid contamination, do not expose the fiber unless collecting or desorbing analytes. If transporting the fiber, ensure that the fiber is fully retracted by adjusting the plunger retaining screw to the top of the Z-slot.

2 Run a SPME Survey method. If using the red fiber, choose SPME_Survey_Red.

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3 A response in Survey is indicated by the TIC increasing at least 2-3 times the baseline level. It may be necessary to keep the fiber inserted in the injection port for up to 2 minutes as the response may not be immediate and the TIC may slowly increase for semivolatiles.

4 If no response is seen, expose the fiber for a longer period of time and run another SPME Survey method. Continue to lengthen the exposure time (up to one hour) until a response is seen.

5 If this proves to be unsuccessful, repeat the procedure starting at Step 1 under section 6.5 on page 6-5 with a different fiber.

6 When a response is seen in SPME Survey, run the appropriate Analyze method. For the red fiber, choose SPME_Tri-Bed_Red_HT.mth for semivolatiles and SPME_Tri-Bed_Red_Standard.mth for all other compounds.

6.7 Aqueous Sampling

1 If the composition of the sample is unknown, expose the fiber for a short period of time (a few seconds to a few minutes) in the headspace above the sample. Keep the fiber approximately 1-2 centimeters above the sample source. See Figure 6-5.

Figure 6-5 Headspace Sampling

CAUTION

Do not allow the fiber to come into contact with the liquid when sampling the headspace.

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CAUTION

To avoid contamination, do not expose the fiber unless collecting or desorbing analytes. If transporting the fiber, ensure that the fiber is fully retracted by adjusting the plunger retaining screw to the top of the Z-slot.

2 Run a SPME Survey method. If using the red fiber, choose SPME_Survey_Red.

3 A response in Survey is indicated by the TIC increasing at least 2-3 times the baseline level. It may be necessary to keep the fiber inserted in the injection port for up to 2 minutes as the response may not be immediate and the TIC may slowly increase for semivolatiles.

4 If no response is seen, expose the fiber in the headspace for a longer period of time and run another SPME Survey method. Continue to lengthen the exposure time (up to one hour) until a response is seen.

5 If a response is not seen in Survey when headspace sampling, dilute the sample by a large factor (10-100 fold) and directly immerse the fiber into the aqueous sample. At first, expose the fiber for a short period of time (a few seconds to a few minutes).

Figure 6-6 Diluting Sample

6 If no response is seen, immerse the fiber for a longer period of time and run another SPME Survey method. Continue to lengthen the exposure time (up to one hour) until a response is seen. See Figure 6-7.

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Figure 6-7 Direct Immersion Sampling

7 If no response is seen after maximizing the exposure time, increase the concentration by a factor of ten. At first, expose the fiber for a short period of time (a few seconds to a few minutes) and run another SPME Survey. Lengthen the exposure time (up to one hour) until a response is seen.

8 If no response is seen after maximizing the exposure time, immerse the fiber in undiluted sample. At first, expose the fiber for a short period of time (a few seconds to a few minutes) and run another SPME Survey. Lengthen the exposure time (up to one hour) until a response is seen.

9 If there still is no response, add 25% salt (chloride salts or carbonate salts) and consistently stir the sample while immersing the fiber. Run another SPME Survey method after the fiber has been immersed for a short period of time. Continue to lengthen the exposure time (up to one hour) until a response is seen.

10 If this proves unsuccessful, repeat these steps with a different fiber.

11 When a response is seen in SPME Survey, run the appropriate Analyze method. For the red fiber, choose SPME_Tri-Bed_Red_HT.mth for semivolatiles and SPME_Tri-Bed_Red_Standard.mth for all other compounds.

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6.8 Aqueous Sampling Flow Chart

Figure 6-8 Aqueous Sampling Flow Chart — Page 1 of 2

Unknown Aqueous Sample

Expose fiber into headspace for a short period of time (a few seconds

to a few minutes).

Run SPME_Survey_Red.Response?

Expose fiber in the headspace for a longer

period of time (up to 1 hour).

Dilute the sample by a large factor.

Immerse the fiber into the sample for a short period of time (a few

seconds to a few minutes).

Immerse the fiber into the sample of a longer period of

time (up to an hour).

Change the dilution factor of the sample, so that the

sample is more concentrated.

Immerse the fiber for a short period of time (a few seconds

to a few minutes).

YES-See Aon page 2

NO


YES-See Aon page 2

NO


YES-See Aon page 2

NO


YES-See Aon page 2

NO


YES-See Aon page 2

NO

Continue with Page 2 of 2

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Figure 6-9 Aqueous Sampling Flow Chart — Page 2 of 2



Immerse the fiber in undiluted sample for a short period of time

(a few seconds to a few minutes).



Add 25% salt to the undiluted sample and consistently stir.



Repeat with a different fiber.

If a response was seen in SPME Survey, run the appropriate Analyze method. For the red fiber, choose

SPME_Tri-Bed_Red_HT.mth for semivolatiles and SPME_Tri-Bed_Red_Standard.mth for all other

methods.

A


YES-See A NO


YES-See A NO


YES-See A NO


YES-See A NO

From Page 1 of 2

Immerse the fiber in the undiluted sample for a short period of time (a few seconds to a few minutes).


YES-See A NO

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Chapter 7Maintenance

7.1 Introduction

The thermal desorption chamber inner sleeve will need to be replaced when contamination from sampling is suspected. The persistence of high boiling point compounds in blank runs indicate that contamination has occurred. To verify that the inner sleeve is the source of contamination, run a couple of blanks without a fiber inserted. Afterwards, run a blank without the SPME inserted. If the contamination is only evident on the SPME runs, replace the inner sleeve. See Figure 7-1 for reference.

Figure 7-1 Diagram of Thermal Desorption Chamber Inner Sleeve

CAUTION

Vial contamination can be mistaken for fiber contamination. Ensure that sample vials are clean and contaminant free.

NOTE: Replace the Teflon seal after 200 fiber injections to ensure that the seal is leak tight.

Washer

Thermal DesorptionInner Sleeve

Washer is retained within the Fiber Holder Guide

SPME Fiber Holder Guide

Teflon® Seal

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7.2 Replacing the Thermal Desorption Chamber Inner Sleeve

CAUTION

Wear nitrile gloves throughout the entire procedure.

1 To replace the thermal desorption chamber inner sleeve, the SPME extractor tool, Teflon seal, inner sleeve, washer, wipes and methanol should be available. For part numbers, see Chapter 8, Part Numbers.

Figure 7-2 Materials Needed

Teflon Seal

Washer

Extractor Tool

Inner Sleeve

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2 Uncrew the Universal Bulkhead connector and pull out the LEMO connection to remove the SPME Sampling System. See Figure 7-3.

WARNING

SPME Sampling System and fittings may be hot. Allow system to cool before removing.

Figure 7-3 Removing the SPME Sampling System

3 Unscrew the beige SPME holder guide by turning it counter-clockwise. See Figure 7-4.

Figure 7-4 Unscrewing SPME Holder Guide

SPME

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4 Twist the screw-like end of the SPME Extractor Tool into the white Teflon seal. See Figure 7-5.

Figure 7-5 Removing Teflon Seal

5 When the screw-like end of the tool is engaged into the Teflon seal, pull out the seal and discard. See Figure 7-6.

Figure 7-6 Seal Removed

6 Insert the bent tip side of the tool into the slot. See Figure 7-7.

Figure 7-7 Inserting Inner Sleeve Removal Tool

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7 Hook the tool into the notch in the inner sleeve and pull out to remove the inner sleeve. Discard the inner sleeve. See Figure 7-8.

Figure 7-8 Removing the Inner Sleeve

8 Insert the screw-like portion of the tool into the slot and turn the tool clockwise a couple of times. See Figure 7-9.

Figure 7-9 Removing the Washer

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9 Pull out the tool to remove the washer and discard it. See Figure 7-10.

Figure 7-10 Washer Removed

10 Clean the new washer, inner sleeve and Teflon seal with methanol.

WARNING

Wear appropriate personal protective equipment (PPE) according to the recommendations of the manufacturer when handling methanol.

11 Wipe the washer, inner sleeve and Teflon seal dry with a lint free cloth. See Figure 7-11.

Figure 7-11 Drying Replacement Parts

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NOTE: The SPME Extractor tool is not necessary to replace the Teflon seal, inner sleeve and washer. In the following steps, do not use the SPME Extractor Tool.

12 Insert a new washer into the slot.

13 Insert the new inner sleeve with the smooth side facing the washer and the notched side facing the opening. It is not necessary to use the tool. See Figure 7-12.

Figure 7-12 Direction of Inner Sleeve

14 Manually insert a new white teflon seal into the slot opening. Do not use the tool. See Figure 7-13.

Figure 7-13 Inserting the Teflon Seal

15 Push the Teflon seal into opening. The seal does not have to be fully inserted.

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16 Screw on the beige SPME holder guide. This will also fully insert the Teflon seal. See Figure 7-14.

Figure 7-14 Screwing on SPME Holder Guide

17 Run a conditioning method, without inserting a fiber, to clean the SPME Sampling System.

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Chapter 8Part Numbers

8.1 SPME Kits

IPN 934-707-G2 . . . . . . . . . . . . . . . . SPME Sampling Kit

IPN 059-0621 . . . . . . . . . . . . . . . SPME Manual Sampling Fiber Holder

IPN 059-0622 . . . . . . . . . . . . . . . SPME PDMS Red Fused Silica Fiber

IPN 059-0623 . . . . . . . . . . . . . . . SPME Carboxen/PDMS Black Fused Silica Fiber

IPN 059-0624 . . . . . . . . . . . . . . . SPME PDMS/DVB Blue Fused Silica Fiber

IPN 934-446-P1 . . . . . . . . . . . . . Kit Case

IPN 934-707-G3 . . . . . . . . . . . . . . . . Red Fiber Kit

IPN 059-0622 . . . . . . . . . . . . . . . SPME PDMS Red Fused Silica Fiber

IPN 934-707-G4 . . . . . . . . . . . . . . . . Blue Fiber Kit

IPN 059-0624 . . . . . . . . . . . . . . . SPME PDMS/DVB Blue Fused Silica Fiber

IPN 934-707-G5 . . . . . . . . . . . . . . . . Black Fiber Kit

IPN 059-0623 . . . . . . . . . . . . . . . SPME Carboxen/PDMS Black Fused Silica Fiber

IPN 934-707-G6 . . . . . . . . . . . . . . . . Fiber Holder Kit

IPN 059-0621 . . . . . . . . . . . . . . . SPME Manual Sampling Fiber Holder

8.2 Maintenance

IPN 934-707-G1 . . . . . . . . . . . . . . . . SPME Spare Parts Kit

IPN 934-3170-P1 . . . . . . . . . . . . Teflon Seal

IPN 934-283-G1 . . . . . . . . . . . . . Inner Sleeve Assembly

IPN 934-079-P1 . . . . . . . . . . . . . SPME Extractor Tool

IPN 934-3171-P1 . . . . . . . . . . . . . . . Vespel Washer

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Chapter 9Customer 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.

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

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074-506-P1B SPME Operating Manual

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