1.2 This TAP is applicable to concrete, charcoal, coral, debris, wipes and soil.

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3 March of SCOPE 1.1 This procedure describes the preparation and analysis of solid matrices and wipe samples. 1.2 This TAP is applicable to concrete, charcoal, coral, debris, wipes and soil. 1.3 This procedure uses surrogates as an option for monitoring extraction efficiency. 1.4 From guidelines described in CHP-004, Chemical Hygiene Plan for Category III RDTE Chemical Surety Materiel, this procedure has been assigned a risk index of 19 See Safety procedures Section 7.0 and the Chemical Hygiene Plan (CHP- 004) for additional information. 2.0 PURPOSE This document provides the description for the sample extraction and analysis of agent from solid and wipe samples. 3.0 RESPONSIBILITIES 3.1 It is the responsibility of the Chemical Agent Manager (CAM) to assure that this procedure has been evaluated and is in compliance with operational plans. 3.2 It is the responsibility of all personnel working in the Chemical Surety Laboratory to comply with this procedure. 4.0 REFERENCES 4.1 Agent handling, personal protection equipment (PPE), and safety procedures should be followed as identified in CHP-004, Chemical Hygiene Plan for Category III RDTE Chemical Surety Materiel for agent operations. 4.2 See TAP , Chemical Surety Materiel (CSM) Protective Glove Policy. 4.3 See TAP , Personnel Decontamination Stations.

4 March of PROCEDURE 5.1 Materials Protective equipment including but not limited to protective glasses, nitrile gloves, laboratory coat, etc Dichloromethane (DCM), isopropyl alcohol (IPA), sodium hydroxide, sodium chloride, glacial acetic acid, and deionized water Silver fluoride conversion pads used to convert VX to G-analog Surrogates compounds to monitor extraction efficiency. Suggested compounds include: Diisopropyl fluorophosphate (DIFP) (C 6 H 14 FO 3 P) CAS: ; Supplier Aldrich; surrogate for GB. 2-Chloroethyl ethyl sulfide (CEES) (C 4 H 9 ClS) CAS: ; Supplier Aldrich; surrogate for. O,S-Diethyl ethylthiophosphonate (DEETP) (C 6 H 15 O 2 PS) CAS: unknown; Supplier Chemical Materiel Agency; surrogate for VX. Note that DEETP will also undergo conversion when passed through an AgF pad to form ethyl ethylphosphonofluoridate (C 4 H 10 O 2 FP) (referred as DEETP analog) Pipettes, micro-spatulas, test tubes or 3 dram vials with Teflon -lined caps, autosampler vials, 10 ml syringes, nylon syringe filters, glass wool, ph paper, etc. (see procedure) Vortex mixer and/or centrifuge Vacuum pump Gas chromatograph equipped with a flame photometric detector (GC/FPD), and a mass spectrometer (GC/MS) with autosampler mm DAAMS and 8-mm DAAMS Chromosorb-106 and Tenax TA tubes

5 March of EXTRACTION OF SOLID SAMPLES FOR GB, VX, AND Sample preparation may be different from matrix to matrix. Some matrices are reactive and will cause the agents to decompose. When applicable, the analyst must take precautions to minimize agent decomposition When necessary buffered solutions may be required to be added to the various matrix in order to minimize decomposition. For GB and samples will need to be buffered between a ph of 4-7 and VX samples will need to be buffered at a ph of Sample ph has a significant impact on VX recovery. Since ph cannot be measured in organic solvent systems, the ph of the sample must be measured in a separate sample aliquot. This can be done by weighing approximately 1 gram of sample, adding 2 ml of a buffer at approximately ph 10, mixing vigorously for 30 seconds, and measuring the ph of the aqueous solution. If the ph is below 8, then a ph 10 buffer with a higher buffer capacity or a buffer with a higher ph must be used. Continue to test buffer solutions until the ph range is between 9.5 and GB and will decompose on matrices that have a ph greater than 8, e.g., concrete. In matrices where the ph is above 8, ph 4 buffers or glacial acetic acid should be used to adjust the ph of the extract. The volume of buffer used should not exceed 2.0 ml and should be added before extraction solvent Sample must be extracted within 7 days. Extraction must be analyzed within 14 days of extraction Weigh g of solid into a 3-dram vial with Teflon-lined screw cap. Record weight into a controlled notebook. Sample weight measured can vary provided that the extraction solvent amount is adjusted accordingly (2 ml of solvent to each gram of sample) For blank and laboratory control sample (LCS) soil samples, use sand verified to not contain agent above the reporting limit. For blank and LCS concrete samples use concrete provided by Umatilla Chemical Agent Disposal Facility (UMCDF) for blank

6 March of 17 and LCS use For blank and LCS wipe samples, place one wipe in a vial and wet with 400 µl of IPA For GB and ph basic samples, add 100 µl of glacial acetic acid. Allow 5 minutes for the acetic acid to dry on the matrix Spike all the samples with the appropriate surrogates: Suggested DEETP spike is 12 ng for VX Suggested DIFP spike is 50 ng for GB Suggested CEES spike is 50 ng for Spike the matrix spike (MS), matrix spike duplicate (MSD) or blank spike sample with agent. Record spike amounts into controlled notebook. Spike amounts should be reflective of instrument and matrix dependent detection limits Suggested GB spike is 20 ng Suggested VX spike is 12 ng Suggested spike is 20 ng Extraction solvent addition Add 2.0 ml of buffer solution, if necessary for particular matrix. In cases where acetic acid was added, add 2 ml of DI water For GB/ - Add 2.0 ml of 10% 2-propanol in DCM or 2.0 ml of DCM to all samples. Note that some matrices will absorb the solvent system such that sufficient quantities of solvent cannot be collected. In these instances, additional solvent may be added; that is, wipe samples may require 4 ml of 10% IPA/DCM. In the event that more than 1.0 grams of sample was weighed, adjust amount of solvent added accordingly.

7 March of For VX - Add 2.7 ml DCM and 2.0 ml of ph 10 buffer to all VX solid samples. Verify that the ph is greater than Put the lid on the vial Mix on a vortex mixer for 1 minute. GB concrete samples may require further mixing to reduce viscosity if the sample gels up Centrifuge the sample if necessary Filter the solvent extract into a 1-dram vial, using a 0.45 µm syringe filter For VX samples, remove 900 µl of the DCM layer (bottom) and place into another vial with 100 µl of 2-propanol (final effective volume = 3 ml). 5.3 EXTRACTION OF WATER SAMPLES FOR GB, VX, AND Sample preparation may be different based on ph of the aqueous sample. Extreme ph levels (high or low) are reactive and will cause the agents to decompose. When applicable, the analyst must take precautions to minimize agent decomposition Sample must be extracted within 7 days. Extraction must be analyzed within 14 days of extraction Measure 1.0 ml of water into a 3-dram vial with Teflon-lined screw cap. Record measured amount into a controlled notebook. Sample amount measured can vary provided that the extraction solvent amount is adjusted accordingly (2 ml of solvent to each 1 ml of sample) For blank and LCS samples use deionized water Spike all samples with the appropriate surrogates: Suggested DEETP spike is 12 ng for VX Suggested DIFP spike is 50 ng for GB

8 March of Suggested CEES spike is 50 ng for Spike the MS, MSD or LCS sample with agent. Record spike amounts into controlled notebook. Spike amounts should be reflective of instrument and matrix dependent detection limits Suggested GB spike is 20 ng Suggested VX spike is 12 ng Suggested spike is 20 ng Extraction solvent addition When necessary ph will be adjusted using buffered solutions or glacial acetic acid to minimize decomposition. For GB and samples will need to be buffered between a ph of 4-7 and VX samples will need to be buffered at a ph of The volume of buffer used should not exceed 2.0 ml and should be added before extraction solvent For GB/ - Add 2.0 ml of dichloromethane to all samples. In the event that more than 1.0 ml of sample was measured, adjust amount of solvent added accordingly For VX - Add 2.7 ml DCM and 2.0 ml of ph buffer to all VX samples. Verify that the ph is greater than Put the lid on the vial Mix on a vortex mixer for 1 minute Centrifuge the sample if necessary Filter the solvent extract into a 1-dram vial, using glass wool or a 0.45 µm syringe filter, if necessary For VX samples, remove 900 µl of the DCM layer (bottom) and place into another vial with 100 µl of 2-propanol (final effective volume =

9 March of 17 3 ml). 5.4 ANALYTICAL PROCEDURES The analytical analysis can be performed by any one of the following methods: GC/MS or GC/FPD. Note that VX direct detection limits do not meet the waste control limits (WCL) of 20 ppb. Therefore, VX will need to be converted via silver fluoride to G-analog which requires DAAMS analysis DAAMS (GC/FPD) Method An initial calibration curve will be run and evaluated before samples can be injected. All standards will be spiked onto the short end (end filled with glass wool) of 8-mm DAAMS tubes on a vacuum manifold with a vacuum of ml/min. The VX standard will be prepared in isopropyl alcohol. Note that VX must be spiked through an AgF Pad Connect long side of an 8-mm DAAMS tube to a vacuum manifold with a suction of about ml/min. Use Chromosorb 106 for VX analysis Spike 25 µl of the organic layer from the extract, into the glass wool inside the DAAMS tube or onto the AgF conversion pad connected to the short end side of the DAAMS tube. Continue airflow for 5 minutes after the DAAMS tube has been spiked The 8-mm DAAMS tube is removed from the assembly and connected by Swagelok union to a 3-mm DAAMS tube The contents of the 8-mm DAAMS tube is transferred to the 3- mm tube by putting the 8-mm DAAMS tube through an aluminum heating block set at o C and connecting the 8-mm DAAMS tube to a helium purge line set at ~ ml/min continuous flow for 3 minutes The 3-mm tube is removed from the transfer assembly For DAAMS injection, the 3-mm tube will be connected to the

10 March of 17 carrier gas line on the GC. The 3-mm tube is then inserted into a modified injection port and the start button is pressed on the GC Suggested configurations. Any configuration change is valid provided that all calibration standards and samples are assayed using the same configuration and method parameters. Configuration changes may include different column/s, different inlet systems, heartcutting, and cryo-focusing. Suggested configuration: Use a DB meter column and set the injector to 220 C. Oven Program: DIFP and DEETP: 90 C 2 min 10 C/min 100 C 50 C/min 240 C 3 min Calibration Standards: VX and DEETP: 30, 60, 100, 200 and 400 pg FPD Detector: VX use a phosphorus filter Liquid Injection (GC/MS) Analysis of GB and will involve liquid injection on the GC/MS Withdraw 400 µl of extract for each sample or standard and place in an appropriately labeled autosampler vial with insert Spike internal standard into each vial at the same concentration. Suggest using naphthalene-d8 at a concentration of 0.1 ng/µl in all standards and samples Cap the autosampler vial and place, in sequence, on the autosampler tray Set up the sequence in the software according to the samples and

11 March of 17 standards on the tray. Injection volume must be the same for samples and calibration standards Press start on the autosampler Suggested configurations. Any configuration change is valid provided that all calibration standards and samples are assayed using the same configuration and method parameters. Configuration changes may include different column/s, different inlet systems, heartcutting, and cryo-focusing. Suggested configuration: Use a RTX-VGC 30 meter column and set the injector to 200 C Oven Program: GB and 60 C 2 min 15 C/min 240 C 5 min Calibration Standards: and GB: 2.5, 5.0, 10, 15, 20, and 30 pg/µl CEES and DIFP: 5, 10, 20, 30, 40 and 60 pg/µl MS (SIM) Detector: GB ions: Primary ion 99 m/z, Secondary ion 125 m/z, 81 CEES ions: Primary ion 124 m/z, Secondary ion 126 m/z ions: Primary ion 109 m/z, Secondary ion 158 m/z DIFP ions: Primary ion 101 m/z, Secondary ion 127 m/z Naphthalene-d4: Primary ion 136 m/z, Secondary ion 108 m/z 5.5 ACCEPTANCE CRITERIA A summary of calibration and QC acceptance criteria is presented in appendix Table A One of several calibration types may be used; however, it must be employed throughout the whole sample set for that particular agent. Regardless of calibration type, a minimum of five calibration points at different concentrations must be used. In the event that the calibration criteria is not met, and a single point is causing the failure, the single point may be reanalyzed provided it is performed within 6 h of the other points

12 March of 17 and provided it is before samples are analyzed. If reanalysis of a single point under these conditions corrects the problem, then the new point is used in the curve. This occurrence must be clearly documented with the curve using the original point and the new point, time and date run and the analyst performing the calibration. If a low concentration point of the curve is removed, then the reporting limit is increased. If the highest concentration point is removed, dilutions of samples must be within range. A full explanation must be included in the data package. If the new calibration point does not correct the problem, corrective action will be conducted and the entire calibration curve will be reanalyzed Linear Regression The calibration curve is deemed valid if the calculated concentration from the regression curve for all target compounds are <25% difference across the working range of the method, with the exception of <35% difference at the lowest point on the calibration and the R2 for the regression is > Also, target ions from the lowest calibration point must meet a 10 1 S N Response Factors Sample concentrations are calculated from the mean response factor. The calibration curve is deemed valid if the calculated % relative standard deviation (%RSD) is less than or equal to 20% and the calculated concentration for all target compounds are <25% difference across the working range of the method, with the exception of <35% difference for the lowest calibration point. Also, target ions from the lowest calibration point must meet a 10 1 S N Continuing calibration standards must be run at the beginning and end of each sample sequence to verify initial calibration values. Only 10 samples can be run between continuing calibration standards. The continuing spike level should be approximately the same as that of the second highest spike level for the initial calibration A continuing calibration standard is deemed valid if the calculated concentration value for each agent is within ±20 % difference of the spiked amount and the relative retention agrees within +5% the retention time window established from initial calibration. Note: if a response factor calibration is employed, the continuing calibration standard is deemed valid if the continuing response factor is within ±20 % difference

13 March of 17 of the mean response factor from the calibration curve and the relative retention agrees within +5% the retention time window established from the initial calibration All blanks must be free of agent All blank spikes, matrix spikes, and matrix spike duplicate recoveries must be within QC limits of %. Recoveries for MS and MSD outside these limits are acceptable provided the LCS passes and it is shown that the recoveries outside tolerance are the result of the matrix. The relative percent difference (RPD) between matrix spike and matrix spike duplicate should be within the QC limit of 35% Suggested surrogate recoveries should be within % Recoveries outside these limits need to be documented in the narrative with an explanation Agent peak criteria Potential agent peak All peaks within agent retention time window will be considered as a potential relative hit. The agent retention time window is ±5% of the average agent retention time found from the two continuing calibration standards (CCS) that bracket the sample in question All potential agent peaks must be above the MDL for that method Confirmation of agent peaks Analysis by GC/MS provides confirmation using ion traces. Reanalysis using an alternate column is not required. Confirmation considerations include: All ions should be present

14 March of CALCULATIONS The ion traces must line up within +2 scan units, The ratios of two ions in the sample must match the ratio found in the continuing calibration standards (CCS) + 30%, Ion masking must be considered; therefore secondary ions may be used for confirmation Given high probability of interferences, the analyst must evaluate confirmation considerations on a sample-to-sample basis Initial Calibration Calculations (Concentration is in terms of on column amounts) Linear Equation Response = B (Conc.) + A, where Conc. is the calculated concentration and B and A are coefficients calculated by the processing software. For regression output, B is the X coefficient, and A is the constant, where concentration is the Independent variable and Response is the dependent variable. Note: Response is equal to area if no internal standard is used, otherwise it is Target Area * IS Conc. / IS Area. When solved in terms of concentration, the equation is: Conc. = (Response A) / B Calibration by Response Factors (RF) RF = (Target Area * IS Conc) / (IS Area * Target Conc) Mean RF is the average of all Initial Calibration Standard Response Factors. To calculate the percent relative standard deviation (%RSD) find the sample standard deviation for the initial calibration standard response factors and divide by the mean response factor.

15 March of Sample Concentration Calculations (µg/l or µg/kg) 5.7 REPORTING 6.0 MAINTENANCE Sample Concentration in Solid µg/kg = ( A * B ) / ( C * D ) Where: A = ng or ng/µl on column amount of target compound B = Extract volume in µl C = DAAMS injection Volume in µl: for liquid injection enter (1) D = Amount of sample in grams Data packages will be prepared in accordance with TAP Preparation of Data Packages for WDC SwRI FRM-274, Method Detection Limit Studies for Organics: A FRM-274 will be submitted for all method detection limit studies. The form will present all seven replicates and calculations of the MDL, recovery, and RPD. All instruments used in this procedure will be maintained. Any instrument maintenance performed will be recorded by the analyst or service engineer in the maintenance logbook. 7.0 SAFETY 7.1 Requirements indicated in the CHP-004, Chemical Hygiene Plan for Category III RDTE Chemical Surety Materiel for agent operations must be met. 7.2 PPE requirement is safety glasses, laboratory coat, nitrile gloves, and a mask within arm s reach. The availability of response equipment and support personnel should be as indicated in CHP-004, Chemical Hygiene Plan for Category III RDTE Chemical Surety Materiel for agent operations.

16 March of Secondary containment is required for all transfer of agent out of engineering control. 7.4 Response team must be available during agent operation. Monitoring system must be operational for specific agent in use or most volatile agent in storage. 7.5 All self-aid and first-aid materials must be available. 7.6 Exposure to chemical agent material is possible from contact. Respiratory exposure can result from spills or improper use of ventilation control Risk is primarily associated with compromise of protective gloves. Compromise is most likely to occur as agent vials are opened Dichloromethane has been reported to cause cancer in laboratory animals, avoid contact with eyes, skin, and clothing. Avoid breathing vapors Sodium hydroxide is corrosive. Causes burns to any area of contact. Reacts with water, acids, and other materials. 7.7 Emergency Response Procedures should be followed as identified in CHP-004, Chemical Hygiene Plan for Category III RDTE Chemical Surety Materiel for agent operations. 8.0 RECORDS 8.1 All records will be maintained and reported in accordance with client/contract requirements. 8.2 Extraction notebooks and instrument injection logbooks will be filled out and controlled according SwRI ISO SOP Raw data, Quickforms file, or spreadsheet containing the Forms (1-8) data will be archived.

17 March of 17 Table A-1 Summary of Calibration and Quality Control Criteria for Agent Analysis Table A-1 Summary of Calibration and Quality Control Criteria for Agent Analysis QC Check Minimum Frequency Acceptance Criteria Corrective Action MS Tune Check- Tune Evaluation (MS only) At the beginning of a 24- hour period of analysis Meet manufactures specifications- Agilent Tune Evaluation Conduct maintenance to address the problem- Clean the source, check for air leaks, etc. Initial Multipoint Calibration (ICAL) for all analytes (minimum of five standards) ICV-Second source calibration verification CCV Internal Standards (IS) (MS Only) ICAL prior to sample analysis Option 1: Response Factors (RF or RRF) - %RSD 20% for each analyte and concentration 100 ± 25% of actual concentration across working standards, except for the low concentration 100 ± 35%. Correct problem then repeat ICAL Option 2: Linear Regression - r for each analyte and concentration 100 ± 25% of actual concentration across working standards, except for the low concentration 100 ± 35%. Once per ICAL All analytes within 100 ± 25% of expected value. Correct problem and verify second source standard. Rerun second source verification. If that fails, correct problem and repeat ICAL 1) Must bracket sample analysis 2) No more than 10 samples can be assayed between CCVs Each sample All analytes within ±20% D of expected value from ICAL Note: D = difference when using RF or RRFs or drift when using linear regression. IS area within -50% to +100% of area from IS in preceding CCV standard Correct problem then rerun CCV. If that fails, repeat ICAL. Determine whether failure was from instrument malfunction or sample matrix. Correct any malfunctions. Reanalyze samples.

18 March of 17 Table A-1 Summary of Calibration and Quality Control Criteria for Agent Analysis QC Check Minimum Frequency Acceptance Criteria Corrective Action Method Blank One per analytical batch No analytes detected > the lowest standard concentration Assess data, correct the problem, and reanalyze. If the blank is contaminated, all samples and QC associated with the contaminated blank need to be re-extracted. For wipe samples, contact the client to determine corrective action. LCS for all target One per analytical batch Target recoveries % Correct problem then reanalyze. If still out, all samples and QC associated with the failing LCS need to be re-extracted. For wipe samples, contact the client to determine corrective action. MS/MSD Surrogate Spike One per analytical batch. (Not required for water samples such as trip blanks, equipment rinseates, etc.) Every sample, spiked sample, standard, and method blank Target recoveries % and 35% RPD Surrogate recoveries % Assess data to determine whether there is a matrix effect or analytical error. Correct problem then reanalyze. If the MS/MSD still fail, consult the client. Correct problem then re-prepare and reanalyze the affected samples. If matrix effect is verified, discuss in case narrative.

19 March of 17 Revision 8 Revised to identify instrument maintenance in response to 2012-CAR-0013 and Document corrective actions in response to 2012-PAR Revision 7 Updated TAP to identify corrective action for calibration curves section 5.5 and Added section 5.3 water extraction procedures. Revision 6 Major revisions throughout document to reflect current procedures and updated TAP number from 0500 to 0605 Revision 5 Update risk form and adjust risk Revision 4 TAP revised to reflect updated laboratory operations for this method.

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