Attachment 24B Air Monitoring SOPs.pdf

CDP COBRATF Training Operations and Support Services

Attachment 24 - B

Air Monitoring SOPs

UNCONTROLLED

i

STANDARD OPERATING PROCEDURE

Organization: Center for Domestic Preparedness Date: October 7, 2019 Title: Dilute CASARM, Stock, Working Standard and PT Solution Procedures

CDP-COBRATF-AMP SOP 006.2

I. Purpose To ensure air monitoring personnel perform appropriate procedures for receipt, accountability, preparation, and destruction of dilute standards used in the Air Monitoring Program.

II. Supersession This SOP supersedes AMP SOP 006.1, Dilute CASARM, Stock, Working Standard and PT

Solution Procedure, effective date April 4, 2017

III. Authority CDP COBRATF Air Monitoring Program Quality Control Plan

IV. References A. CDP COBRATF Air Monitoring Plan B. Current revision of the Proficiency Testing Plan of the CASARM Quality Assurance

Program C. CDP COBRATF Chemical Hygiene Plan D. CDP COBRATF AMP SOP 003, Type 1 GC/FPD Methods E. Chemical Laboratory Stability Study (available in Chemical Laboratory) F. CQATFM QC-11, Shipment Status Report G. Department of Defense (DD) Form 1911, Materiel Courier Receipt

V. Acronyms and Definitions A. 2MUC – Maximum Use Concentration: maximum use concentration (MUC) means the maximum atmospheric concentration of a hazardous substance from which an employee can be exposed to be protected when wearing a respirator, and is determined by the assigned protection factor of the respirator or class of respirators and the exposure limit of the hazardous substance. The MUC monitoring method in use at the CDP COBRATF will be established at two times the maximum use concentration designated (2MUC), and will be operated at chemical agent concentrations equivalent to 100 times the STEL AEL concentration values for the chemical agents VX and GB.

B. AgF – Silver Fluoride; converts VX into G-analog

C. AMP – Air Monitoring Program D. Analyst – A person performing some type of laboratory process; interchangeable with term technician, but does not imply that job title is technician file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/Air%20Monitoring%20Plans/AMP%20QC%20Plan%20Rev%202%20%20%209-9-2019.pdf file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/Air%20Monitoring%20Plans/Air%20Monitoring%20Plan/Air%20Monitoring%20Plan%20%20Rev%2011%20%20%205-14-19.pdf file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/CDP%20Safety%20Plan%20Annexes/Annex%20L%20Chemical%20Hygine%20Plan.pdf file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/COBRATF%20SOPs/AMP%20SOP,%20WIs/AMP%20SOP%20003.1%20Type%202%20GC%20FPD%20Methods/AMP%20SOP%20003.1%20Type%202%20GC%20FPD%20Methods.pdf ii

E. CAL – Calibrate/calibration F. CASARM – Chemical Agent Standard Analytical Reference Material G. CBC – Chemical Biological Center H. cm – centimeter; a metric unit of measure I. CQAT – CASARM Quality Assurance Team J. DD – Department of Defense K. G – gram; a metric base unit of measure L. GB – Sarin; isopropyl methylphosphonofluoridate; a non-persistent nerve agent M. GC – Gas Chromatograph; an analytical instrument used for measuring chemical components N. GPL – General Population Limit O. Hot Trash – All refuse accumulated during dilute standard preparation P. IAW – In Accordance With Q. IDLH – Immediately Dangerous to Life and Health R. IPA – Isopropyl Alcohol S. ISO – International Organization for Standardization T. Method – A process that begins with the collection of a sample and is followed by the analysis of the sample by an appropriate analytical technique; method requirements specify the type of sampling media, air flow rates, collection time, the details of the sample preparation, and the type and set points of the instrument used to analyze the sample; examples of methods include type 1 and type 2 U. mL – milliliter; a metric unit of volume V. NFPA – National Fire Protection Agency W. NIST – National Institute of Standards and Technology X. ng – Nanogram Y. ng/uL – Nanograms per microliter

Z. PPE – Personal Protective Equipment

AA. PT – Proficiency Test(ing)

AB. QC – Quality Control

AC. QP – Quality Process

AD. RDTE – Research, Development, Testing, and Evaluation; used in reference to drinking water level standards

AE. Reagent – A substance that, because of the reactions it causes, is used in chemical analysis and /or synthesis

AF. SSR – Dilute Shipment Status Reports iii

AG. STEL – Short Term Exposure Limit; the maximum concentration to which unprotected chemical workers may be continuously exposed for up to 15 minutes

AH. uL – Microliter; a metric unit of measure; 1/1,000,000 liters

AI. VSL – Vapor Screening Level; a CDP COBRATF value used to clear areas, items, or waste; the value is derived from the STEL concentration, but the sampling time is greater than 15 minutes

AJ. VX – Ethyl ({2-[bis(propan-2-yl)amino]ethyl}sulfanyl)(methyl)phosphinate; a persistent nerve agent

AK. WPL – Worker Protection Limit

AL. Z – The generic designation for the applicable monitoring standard (STEL, ASC, etc.)

VI. Responsible Office All Air Monitoring Laboratories

Intentionally left blank.

iv

Table of Contents

I. Purpose ........................................................................................................................................ i II. Supersession ................................................................................................................................. i III. Authority ...................................................................................................................................... i IV. References .................................................................................................................................... i V. Acronyms and Definitions ............................................................................................................ i VI. Responsible Office ..................................................................................................................... iii VII. Standard Operating Procedures

A. Receipt of CASARM Solutions B. Accountability...……………………………………………………………………...……..3

C. Preparation D. Disbursement and Storage of Standards E. Testing F. Destruction VIII. Forms Prescribed

VII. Standard Operating Procedures NOTE: See attached hazard assessment (Appendix A) A. Receipt of CASARM Solutions.

1. CASARM solutions are sent to us through the CASARM Quality Assurance Team, Aberdeen Proving Ground, MD and coordinated by the Laboratory Chemist.

2. Movement to CDP COBRATF Chemical Laboratory:

a. Chemical laboratory personnel pick up CASARMS Standards at the airport designated by the transportation team and transports the standards from the airport to the COBRATF in a government vehicle.

b. Take decon spill kit with the following items to pick up area:

(1) Bleach spray/squirt bottle

(2) Paper towels

(3) Nitrile gloves

(4) Heavy-duty trash bags (3)

(5) Vermiculite

NOTE: If there is any leak on the floor/outside the shipping container, it is decontaminated immediately. The item is double bagged along with the contaminated waste.

c. Inspect the shipping container for obvious signs of leakage.

d. Personnel transport boxes to the laboratory.

3. Inside Chemical Laboratory:

a. Wearing gloves and lab coat, unpack the shipping container and place secondary containers inside the hood. Observe the container(s) for leakage.

b. While under the hood, open the secondary container, inspect for leaks, and inventory all ampoules.

c. If an ampoule is cracked and/or leaking, segregate the ampoule. Decontaminate remaining ampoules and all packing material and containers that have been contaminated. Dispose of contaminated waste by double bagging it, moving it into the agent laboratory and placing it in the vault hood pass through chute.

d. Once that has been done notify Safety Control.

e. Place remanining ampoules in labeled containers and store in the refrigerator.

4. Label each container with:

a. Lot number, concentration of solution, source, receipt date, expiration date, ampoule volume, and individual ampoule numbers in the container.

b. NFPA label with the following information: Health 4, Flammability 1, Reactivity

1, Specific Hazard 0.

c. Check each shipment for the following:

(1) Certificate of analysis for CASARM grade solutions or a memorandum for record stating concentration of solutions – one for each agent solution shipped.

(2) DD Form 1911

(3) CQATFM QC-11

d. An Accountable Officer for chemical agents indicates acceptance of custody on the DD Form 1911.

e. Return all accountability documents to the CDP COBRATF Accountable Officer.

5. Store all dilute solutions, to include CASARMS ampoules, at or below 4oC.

B. Accountability.

1. CASARM (RDTE) Solutions: The typical concentration of CASARM solutions for

VX and GB supplied by CBC is approximately 0.25 mg/mL for GB and approximately 0.10 mg/mL for VX.

2. An Accountable Officer periodically checks records to verify completeness of all documents. Discrepancies are corrected immediately.

3. Make an entry on AMPF 021 upon receipt of CASARM solutions and when an ampoule is used.

4. Preparation of working standards is the primary use of CASARM solutions and accountability ends upon using the vial. After the vial of standards has been used or loses its effectiveness, decontaminate.

5. Each time a vial of working standards is issued, AMPF 026 is signed. Chemical laboratory personnel initial the return/destruction of unused solution.

6. In the event a working standard is declared ineffective, decontaminate and log entry on the preparation form to adjust the balance.

7. Expired CASARM solution is destroyed by chemical laboratory personnel.

8. Conduct inventories of CASARM solutions semiannually and upon receipt.

9. E-mail a copy of the SSR to the personnel identified on the SSR.

10. See Chart 1 and Chart 2 for dilute process flows.

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C. Preparation

1. General Information

a. Two sets of solutions are prepared: CAL and QC.

(1) CASARM solutions of GB and VX are received from CBC in glass ampoules.

(2) The CAL solutions are prepared from the CASARM ampoules with a “C” at the end of the lot number.

(3) QC solutions are prepared from the ampoules with a “Q” at the end of the lot number.

(4) One analyst prepares the “C” solution while a different analyst prepares the “Q”.

b. Assigning Lot Numbers:

(1) The Julian date (a combination of the last two digits of the year and the three digit number of the day of the year. EXAMPLE: 1/1/2011 = 11001) determines the first five digits of the lot number.

(2) The next digit is determined by the order in which the dilution is made.

(3) Those numbers are followed by the type of agent (GB, VX, GX).

(4) Proficiency Test solutions have a “PT” associated with the lot number.

(5) The expiration date for the Stocks, Working Standard and PT solutions is one month from the date of preparation, unless the laboratory demonstrates otherwise (see Chemical Laboratory Stability Study).

c. Labels: Every dilute solution container should have a bordered label (red border for “C” solutions and blue border for “Q” solutions) which includes the following information:

(1) Agent Name (VX, GB, GX)

(2) Solution Concentration

(3) Solvent Name

(4) Preparation Date

(5) Expiration Date

(6) CDP COBRATF Assigned Lot Number

d. Solvent:

(1) Ensure the quantity of solvent from a given lot is sufficient to prepare all dilutions planned for the task at hand.

(2) The solvent used should be, at a minimum, listed as reagent grade.

(3) Record solvent name, manufacturer, grade and lot number on AMPF 029 /

AMPF 023.

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2. Glassware/Syringes:

a. Use only calibrated volumetric flasks to make each dilution. Because syringes do not always reach down to the bottom of a volumetric flask, solutions prepared in volumetric flasks that are needed for further dilutions can be transferred to another labeled container to facilitate draw and measurement.

b. Use the following procedure to clean glassware to be used for standard preparation (including vials) and dry before use, even if it is new, excluding silanized glassware purchased for one-time use:

(1) Rinse three (3) times with isopropyl alcohol.

(2) Return to rack to dry.

NOTE: Never put glassware on rack unless it has been cleaned.

(3) Record cleaning on AMPF 028 or AMPF 030 as applicable.

(4) Allow vials to dry completely before use.

(5) Decon and discard used vials in the hot trash. Do not reuse.

c. Volumetric glassware calibration:

(1) Select the volumetric glassware to be calibrated. Inspect each piece for physical defects. Record the serial number of each piece of glassware and any observed physical defects on form AMPF 027.

(2) If a number of pieces are to be calibrated, add the volumes of the various pieces to obtain a total volume. Select a beaker with a volume greater than the total volume of the glassware to be calibrated. Fill the container with distilled or deionized water. Allow the water to equilibrate to room temperature.

(3) Weigh the glassware to be calibrated on an analytical balance to obtain a tare weight. Record the tare weight on AMPF 027.

(4) Carefully fill the glassware to the mark with water such that the meniscus sits on top of the mark. Weigh the glassware on an analytical balance to obtain the combined weight of the flask and the water. Record the weight on AMPF 027.

(5) Subtract the tare weight from the combined weight; record the value obtained on AMPF 027. The difference in weight should approximate the listed volume for the container (i.e., ‘a 10 mL volumetric flask should contain 10 g of water when filled to the mark’).

(6) Repeat for each piece of glassware.

(7) If a NIST traceable and/or ISO Quality System Certified Certificate of Graduation Accuracy is issued with a new piece of glassware, the glassware need not be calibrated before use.

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d. Use only dry glassware and syringes. When a syringe is being used with the same source solution it should not be rinsed with the solvent between dilutions. Rinse syringes three (3) times with solvent before putting away.

e. Other appropriate measuring instruments may be used instead of syringes.

f. Make only one (1) dilution at a time. Stay behind the 20 cm line when preparing dilutions, except when making final adjustments.

3. Calculations:

a. The following equation can be used to determine volume of source solution to use or concentration of new solution.

V1C1 = V2C2 or C2 = V1C1 V2

V1 = Volume of Source Solution V2 = Volume of New Solution C1 = Concentration of Source Solution C2 = Concentration of New Solution

Example: 50 mL (V2) of new solution is needed. The concentration needs to be

4.0 ng/uL GB (C2). The source solution, which is to be used, has a concentration of 100.80 ng/uL GB (C1). How much of the source solution needs to be used (V1).

V1 = V2C2 = 50 mL x 4.0 ng/uL GB = 1.98 mL 2.00 mL of source C1 100.80 ng/uL GB

b. Dilute Solution Preparation Note of Explanation: Using the formula equation above, Preparation Notes are calculated to give directions on which source solution should be used, how much of the source solution should be used, the volume of the new solution and syringes to draw the source solution. These notes for dilute solutions may be hand written or typed, are stored in the appropriate dilute solution book and can be modified to address the specific types of standard solutions requested with Laboratory Chemist (or designee) approval.

c. Chemical laboratory staff assist in the preparation of the calculations and initials/dates the final draft. The Laboratory Chemist, or designee, validates and approves the calculations and signs/dates the final draft. Once this requirement is complete, these calculations become Preparation Notes. The notes are then released for solution preparation.

4. Target Concentration Requirements:

a. Lab Daily Standard (VSL)

GB = 4ng/4uL = 1ng/uL + 5% = 0.95-1.05ng/uL

VX = 0.4ng/4uL = 0.1ng/uL + 5% = 0.095-0.105ng/uL

b. M/C STEL

GB = 0.36ng/4uL = 0.09ng/uL + 5% = 0.0855-0.0945ng/uL

VX = 0.036ng/4uL = 0.009ng/uL + 5% = 0.00855-0.00945ng/uL

c. Wastewater Standard

GB = 1ng + 5% = 0.95-1.05ng/uL

VX = 1ng + 5% = 0.95-1.05ng/uL

d. AgF Test Standard

GB = 1.89ng/1uL + 5% = 1.7955-1.9845ng/uL

VX = 3.6ng/1uL + 5% = 3.42-3.78ng/uL

e. M/C 2MUC

GB = 15ng/4uL = 3.75ng/uL + 5% = 3.56 – 3.93ng/uL

VX = 1.5ng/4uL = 0.375ng/uL + 5% = 0.356 – 0.393ng/uL

f. Lab WPL

GB = 7.2ng/4uL = 1.8ng/uL + 5% = 1.71-1.89ng/uL

VX = 0.24ng/4uL = 0.06ng/uL + 5% = 0.057-0.063ng/uL

g. Lab GPL

GB = 0.72ng/4uL = 0.18ng/uL + 5% = 0.171-0.189ng/uL

VX = 0.432ng/4uL = 0.108ng/uL + 5% = 0.1026-0.1134ng/uL

h. M/C IDLH

GB = 50ng/4uL = 12.5ng/uL + 5% = 11.875-13.125ng/uL

VX = 1.5ng/4uL = 0.375ng/uL + 5% = 0.356-0.393ng/uL

i. Lab STEL

GB = 3ng/4uL = 0.75ng/uL + 5% = 0.7125-0.7875ng/uL

VX = 0.3ng/4uL = 0.075ng/uL + 5% = 0.07125-0.07875ng/uL

5. Materials/Equipment:

a. Assorted volumetric flasks and vials, cleaned

b. Disposable pipettes/bulbs

c. Syringes or other appropriate measuring device

d. Dilute CASARM ampoules, warmed to room temperature

e. Solvent (IPA- Reagent Grade at a minimum)

f. Bleach

g. Labels

6. PPE:

a. Lab coat

b. Nitrile gloves

7. Preparing Dilutions:

a. Assemble required equipment/supplies.

b. Obtain AMPF 029 / AMPF 023 / AMPF 024. Due to the importance of agent solution traceability, all items of these blank forms must be filled out completely.

c. Ampoules:

(1) Allow ampoules to equilibrate to room temperature before use. This helps prevent contamination from the condensation of atmospheric moisture, which can hasten agent degradation.

(2) Open ampoule and transfer proper volume of solution to a volumetric flask using a calibrated syringe.

(3) Record ampoule used on AMPF 021.

(4) Record dilution information on AMPF 029.

(5) Decontaminate any unused portion of dilute CASARM ampoules and place in hot trash container.

(6) If second agent ampoule is needed, repeat steps above.

d. Stock and Working Standard Solutions:

(1) Using Preparation Notes, determine and assemble the appropriate syringe, volumetric flask with stopper, source standard and other containers needed to make the dilution.

(2) Use syringe listed on Preparation Notes to pull calculated quantity of source standard.

(3) Add the calculated quantity of the source standard (from Preparation Notes) to the volumetric flask with the selected syringe.

(4) Add solvent to the volumetric flask until the bottom of the meniscus lies on the line found on the neck of the flask.

(a) Use a pipette to add solvent when close to line.

(b) To obtain proper dilution of the desired concentration, the meniscus must lie exactly on the line, if the line is passed in filling, the flask must be emptied and the entire process repeated.

(c) Stopper the flask and mix by carefully swirling or very carefully inverting the flask several times.

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(d) The stopper must be held in place with one finger while inverting.

(5) Label volumetric flask and container.

(6) Record dilution information on AMPF 029 / AMPF 023 / AMPF 024.

(7) Set containers aside. Decontaminate any glass pipettes that may have been used and discard them in the broken glass container under the hood.

(8) If any volumetric flask(s) is emptied, clean per section VII.C.2.b. Glassware must be cleaned before next use.

(9) Repeat this process for each concentration of standard necessary.

(10) Cap vials and wrap volumetric flask stoppers with parafilm.

(11) Place all solutions in the refrigerator.

e. PT Standard Solutions

(1) When requested by CASARM, the chemical laboratory staff dilute the PT standard (GB and VX), based on the reported range, to the appropriate concentration for each of the type 1 methods in use.

(2) Use AMPF 023 and/or AMPF 024 to track the dilutions.

(3) Preliminary calculations (high, low, and mid range) may be performed based on the reported range to assist in determining appropriate dilution of the CASARM PT vials.

(4) Perform a 5 point calibration on a GC using the standard for the Type 1 method being tested, ensuring the correlation coefficient is 0.99 minimum for each agent.

(5) Determine which syringes will be used and formulate Preparation Notes for the preliminary PT dilutions.

(6) Prepare PT labels (usually a green border).

(7) Make dilutions IAW sectionVII.C.7.d of this procedure based on the preliminary PT Preparation Notes. Record all dilution information on AMPF 023 and AMPF 024.

(8) Spike a minimum of 3 tubes with the prepared standards and analyze IAW

AMP SOP 003.

(9) Back calculate the concentration of the PT vial using the average of the 3 tubes.

(10) Based on the calculated concentration of the PT vial, formulate a final set of Preparation Notes for the PT dilutions that will be tested by all participating Air Monitoring Program laboratories.

(11) Prepare PT labels (usually a green border).

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(12) Make dilutions IAW sectionVII.C.7.d of this procedure based on the final PT Preparation Notes. Record all dilution information on AMPF 023 and

AMPF 024.

(13) Disburse standards IAW section VII.D of this procedure.

(14) Reporting results: see section VII.G.

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D. Disbursement and Storage of Standards.

1. Disbursement:

a. Pipette approximately 0.3-2 mL of required standard into a labeled vial.

b. Seal the vial.

c. Record data on AMPF 029 or AMPF 023 / AMPF 024 as applicable.

d. Place vials in refrigerator.

2. Storage:

a. Store all standards at or below 4oC.

b. Log refrigerator temperatures each day of operation on AMPF 001 / AMPF 043 as applicable.

c. Thermometers used for measuring refrigerator temperatures are calibrated IAW

QMP 001. Thermometer calibrations are verified prior to change-out by comparing values from the old thermometer to values from new thermometer prior to the calibration expiration and recorded on AMPF 042. Thermometers are changed out immediately after verification is complete.

3. Issue:

a. Standard vials issued out must be signed for on AMPF 026.

b. Any vial of standard solution issued and used in the toxic agent area must be returned by placing it in the pass through chute.

c. Upon return, destroy any vials issued out by pouring bleach into the vial, then place it into the hot trash container.

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E. Testing:

1. Calibrate/challenge instrument using appropriate operating method

(e.g. AMP SOP 002, AMP SOP 003, etc.) for standard(s) being tested.

2. Perform a minimum of three (3) shots on the instrument for the standard(s) being tested of both the C and Q standard vials.

3. Average the 3 shots and ensure that C vs. Q concentration is less than 10% for each standard tested using the following calculation: Average Q – Average C / Average C.

4. Report values to Laboratory Chemist (or designee).

5. Laboratory Chemist (or designee) will validate data and approve solutions for use.

6. A Standard(s) that does not meet the 10% minimum pass criteria is discarded and a new standard(s) prepared and tested.

file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/COBRATF%20SOPs/AMP%20SOP,%20WIs/AMP%20SOP%20002.3%20MINICAMS%20Methods%20Procedures/AMP%20SOP%20002.3%20MINICAMS%20Procedures.pdf file://///amcd12f01/forms/UNCONTROLLED%20SOPs,%20QMPs,%20Manuals%20and%20Plans/COBRATF%20SOPs/AMP%20SOP,%20WIs/AMP%20SOP%20003.1%20Type%202%20GC%20FPD%20Methods/AMP%20SOP%20003.1%20Type%202%20GC%20FPD%20Methods.pdf

F. Destruction

1. Use commercial bleach for decontamination of dilute VX and GB.

2. Transfer all flasks, vials, ampoules or other containers of CASARM solutions or working standards to be decontaminated to the hood.

3. Transfer the CASARM solutions or working standards to an appropriately sized container. Add bleach using the ratio of 5:1 (solution to contaminated material).

4. Allow to stand overnight.

5. Clean Up:

a. Wipe up any spilled liquid and place used paper towels in a hot trash container.

b. Double bag all the hot trash and transfer to pass through chute.

c. Record destruction on AMPF 021 / AMPF 029 / AMPF 023 / AMPF 024 as appropriate.

file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20021.0%20Dilute%20Ampoule%20Accountability.doc file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20029.1%20Dilute%20Sds%20Solutions%20Worksheet%20and%20Disbursement%20(002)%20Draft.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20023.0%20Special%20Dilute%20Solution%20Worksheet%20&%20Disbursement.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20024.0%20Special%20Dilute%20Solution%20Worksheet%20Continuation.pdf

G. Semi-Annual/PT Evaluations

1. Each prepared PT solution is analyzed by a member of air monitoring personnel participating in the PT. A result from each QP challenge performed with each type 1 method is reported to CASARM to fulfill the requirements of the proficiency test.

2. Each analyst participating in the PT is issued a vial of PT standard for analysis IAW section VII.D.

3. Standard concentrations are unknown to analysts participating in PT or semi-annual evaluations.

4. Each analyst calibrates an instrument and challenges it three times with the unknown standard for the assigned method.

5. The calibration must be performed on the same day as the analysis.

6. The analyst, date, unknown sample ID, instrument ID, method, calibration standard lot number and its concentration range are recorded on AMPF 025.

7. The analyst then determines the agent level of the unknown solution by challenging the instrument with a 4 µL injection.

8. The Z values for each of the three challenges are recorded on AMPF 025. These values are then reported to the Laboratory Chemist.

9. The Laboratory Chemist enters the found concentrations and the dilutions used to prepare the solutions into a PT/semi-annual workbook to calculate the concentration for the PT solutions.

10. These values are reported to CASARM as the proficiency test results.

11. The known concentrations are used to evaluate the semi-annual proficiency of the analyst and reported back to air monitoring personnel as acceptable or unacceptable.

12. Written notification of any analyst having unacceptable results are reported to the supervisor within 5 working days.

13. Each analyst shall be evaluated at least yearly on all type 1 methods for which they are certified.

14. In the event that a certified analyst’s PT and/or semi-annual results are judged to be unacceptable, the technician who generated the failing results is temporarily restricted from operating (calibrating or challenging) that method.

15. Any individual PT/semi-annual shots that do not meet the pass criteria are evaluated on a case-by-case basis by the Laboratory Chemist, who determines and documents course of action. If necessary, unknown evaluations are repeated.

16. PT/Semi-annual results are recorded on AMPF 022.

17. Original data is filed with the PT solutions paperwork by the chemical laboratory.

file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20025.1%20PTSemi-Annual%20Test%20Data%20Reporting%20Form%201.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20025.1%20PTSemi-Annual%20Test%20Data%20Reporting%20Form%201.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20022.1%20PT%20Semi-Annual%20Evaluation%20Form.xlsx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20022.1%20PT%20Semi-Annual%20Evaluation%20Form.xlsx

VIII. Forms Prescribed A. CDP COBRATF AMPF 001, Refrigerator Temperature/Working Standard Solutions Log

B. CDP COBRATF AMPF 021, Dilute Ampoule Accountability

C. CDP COBRATF AMPF 022, PT/Semi-Annual Evaluation Form

D. CDP COBRATF AMPF 023, Special Dilute Solutions Worksheet and Disbursement

E. CDP COBRATF AMPF 024, Special Dilute Solutions Worksheet and Disbursement (Continuation)

F. CDP COBRATF AMPF 025, PT/Semi-Annual Test Data Reporting Form

G. CDP COBRATF AMPF 026, Chain of Custody: Receipt of Dilute Solutions

H. CDP COBRATF AMPF 027, Glassware Calibration

I. CDP COBRATF AMPF 028, Glassware Use/Cleaning

J. CDP COBRATF AMPF 029, Dilute Standards Solutions Worksheet and Disbursement

K. CDP COBRATF AMPF 030, Vial Cleaning Log

L. CDP COBRATF AMPF 042, Thermometer Verification Log

M. CDP COBRATF AMPF 043, Refrigerator Temperature Record

N. PT/Semi-Annual Calculation Workbook

O. Dilute Solution Preparation Notes file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20001%201%20Refrigerator%20Temp%20%20Working%20Standards%20Solutions%20Log%201.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20021.0%20Dilute%20Ampoule%20Accountability.doc file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20022.1%20PT%20Semi-Annual%20Evaluation%20Form.xlsx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20023.0%20Special%20Dilute%20Solution%20Worksheet%20&%20Disbursement.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20024.0%20Special%20Dilute%20Solution%20Worksheet%20Continuation.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20025.1%20PTSemi-Annual%20Test%20Data%20Reporting%20Form%201.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20026.1%20Receipt%20of%20Dilute%20Solutions.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20027.0%20Glassware%20Calibration.doc file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20028.0%20Glassware%20Use%20Cleaning.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20029.1%20Dilute%20Sds%20Solutions%20Worksheet%20and%20Disbursement%20(002)%20Draft.pdf file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20030.0%20Vial%20Cleaning%20Log.docx file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20042.0%20Thermometer%20Verification%20Log.doc file://///amcd12f01/forms/CDP%20COBRATF%20FORMS/AMP%20Forms/AMPF%20043.1%20Refrigerator%20Temperature%20Record%20Draft.doc

Chart 1

Dilute Request Procedures

Chart 2

Administration/Laboratory – CDP COBRATF

Determine (Projection):

Consumption of CASARMS (RDTE Dilute Solution) Air Monitoring Program

Request:

Authorized e-mail and/or paper memo

Phone Call – as needed

Requestor:

Name, Address and Phone Agent Type(s) Agent Quantity Primary Vial Size Preferred Delivery Date COORDINATE WITH

CASARM (Dilute Agent) CDP Budget Analyst Supplier

Dilute Agent – Accountability Procedures

(1) Request:

(2) Receipt:

(3) Record Book/Log:

(4) Storage:

(5) Issued:

(6) Use:

(7) Transfer:

(8) Destruction:

(9) Inventory:

(10) Inventory Report:

START

Request

Dilute (RDTE) Agent

(a) Coordinate with CASARM

(b) Arrival Notification (Date/Time)

(c) Custodian/Buddy to Guard House with heavy duty cart (if necessary)

(d) Lab Shipment Container

(e) Check for leaks

(f) After Duty Hours: Keep in guard house storage room then check next working day for accountability

(g) Sign DD Form 1911

(h) Fax DD Form 1911 to CBC Acct Officer

Prepare for New Arrival COBRATF System – LOG IN

Refrigerator

Prepared solutions for instruments

Instrument challenges and wet chemistry

When applicable, other primary custodians

When applicable

Semiannual or as applicable

Deconned/Record on paperwork

END

FOR OFFICIAL USE ONLY

WORK INSTRUCTION

Organization: Center for Domestic Preparedness Date: July 2, 2018

Title: Construction, Testing and Conditioning of MINICAMS Preconcentrator Tubes

CDP-COBRATF-AMP WI 004.2

I. Purpose

To document instructions for construction, testing, and conditioning of preconcentrator tubes

II. Supersession

CDP COBRATF AMP WI 004.1, Construction, Testing and Conditioning of MINICAMS Preconcentrator Tubes, effective date April 5, 2017

III. Authority

Air Monitoring Program Quality Control Plan

IV. References

A. CDP COBRATF AMP SOP 002, MINICAMS Method Procedures

B. CDP COBRATF AMP SOP 007, Procedures for Air Monitoring Products

V. Acronyms and Definitions

A. CAL – Calibrate

B. HayeSep D (40/60 mesh) – sorbent material used in preconcentrator tubes to capture and release chemical agents

C. ID – Inside Diameter

D. LMFC – Linear Mass Flow Controller

E. mL – Milliliter; a metric unit of measure

F. mm – Millimeter; a metric unit of measure

G. OD – Outside Diameter

H. PCT – Preconcentrator Tube

I. Pyrex Glass Tubing – glass tubing used to construct preconcentrator tubes

J. Silane Glass Wool – material used to hold sorbent material in preconcentrator tubes between the spacers

K. Spacer – Pyrex tubing that fits inside a larger piece of Pyrex tubing that holds the silane glass wool in place around the HayeSep D (40/60 mesh)

L. uL – Microliter; a metric unit of measure; 1/1,000,000 liters

VI. Responsible Office

MINICAMS Laboratory

FOR OFFICIAL USE ONLY 2

VII. Instructions

NOTE: See hazard assessment in Appendix B of AMP SOP 002.

A. Tools Required (Quantity)

1. Torch capable of fire polishing the end of glass tubing (1)

2. Impact-resistant safety goggles (1)

3. Ultraviolet safety goggles (1)

4. Calibrated flow controller (1)

5. Calibrated magnahelic gauge (1)

6. Ruler graduated in mm (1)

7. Miscellaneous small tools and fittings used to manipulate glass wool and sorbent material, and test the finished PCTs

B. PCT Purchasing

1. When purchasing PCT’s ensure that all specifications are listed on purchase request.

2. When PCT’s are received ensure certification of construction specifications match what is listed on the purchase request and manufacture certificate of compliance.

C. PCT Construction

NOTE: If Preconcentrator Tubes are purchased and not constructed in house proceed to Section D for testing

1. Cut a piece of 3.0 mm-OD x 2.4 mm-ID glass tubing to a length of 100 ± 2 mm. This will be the “PCT” outer tube.

2. Cut a piece of 1.65 mm-OD x 1.18 mm-ID glass tubing to a length of 33 ± 3 mm.

This is the “short spacer”.

3. Use the torch to fire polish one end of the 100 ± 2 mm PCT so it will capture the short spacer when it is placed into the tube. Make sure the end of the PCT is not closed off when it is fire polished.

4. Push 3 ± 1 mm layer of the silane treated glass wool into the PCT until it touches the spacer.

5. Use a vacuum to pull 15 ± 1 mm of the sorbent (HayeSep D) into the PCT.

6. Push a 3 ± 1 mm layer of the silane treated glass wool into the PCT until it touches the sorbent.

NOTE: Use magnehelic to test PCTs before inserting long spacer to check pressure drop, and ensure pressure falls between 90-140 in. of water.

7. Cut a second piece of the 1.65 mm-OD x 1.18 mm-ID glass tubing to a length of 48 ± 3 mm to fill the space between the second glass wool plug and the end of the tube.

This is the “long spacer”.

8. Insert the long spacer into the PCT.

FOR OFFICIAL USE ONLY 3

9. Use the torch to fire polish the other end of the 100 ± 2 PCT so the long spacer does not fall out when the PCT is inverted. Ensure the end of the PCT is not closed off when it is fire polished.

10. Repeat steps B.1- B.9 above until a batch of tubes has been completed.

D. PCT Testing

NOTE: Any PCT that has defects or that falls outside the allowable length (100 ± 2 mm) fails the inspection and must be discarded immediately.

1. Inspect each PCT to ensure it was constructed properly and that there are no obvious defects (length of the PCT out of tolerance, spacers or sorbent material falling out, etc).

2. Assign a unique batch number to identify the tubes. This number should appear on AMPF 012 and the label for the container in which the finished tubes are placed (after testing).

3. Adjust flow to 950 mL/min on LMFC.

4. Connect each finished PCT to pressure drop testing apparatus for pressure drop testing.

5. Record the pressure drop “as measured on the magnehelic gauge” on AMPF 012.

6. A PCT is acceptable if the pressure drop measured at 950 mL/min is in the range of 90-140 in. of water and it passes the physical inspection stated in C.1 above). Mark whether a PCT passes or fails on AMPF 012.

E. PCT Heat Conditioning

1. The HayeSep D used in PCT tubes is pre conditioned by the vendor as specified before purchase.

F. PCT Agent Conditioning

NOTE: PCTs must be conditioned with agent after installation, prior to first use.

1. Install MINCAMS PCT.

2. Place MINICAMS in service mode.

3. Obtain appropriate agent standard.

4. Spike PCT with 5uL of the appropriate standard.

5. Allow MINICAMS cycle to run.

6. Repeat steps D.2 – D.5 above two more times.

7. Record in instrument logbook.

VIII. Forms Prescribed

CDP COBRATF AMPF 012, MINICAMS PCT Test Data

FOR OFFICIAL USE ONLY

WORK INSTRUCTION

Organization: Center for Domestic Preparedness Date: July 19, 2019

Title: Manually Punching Silver Fluoride (AgF) Conversion Pads

CDP-COBRATF-AMP WI 009.2

I. Purpose

To provide instructions for manually punching AgF pads

II. Supersession

This supercedes: AMP WI 009.1, Punching Silver Flujoride (AgF) Conversion Pads, Effective Date: April 30, 2018

III. Authority

CDP COBRATF AMP SOP 007, Air Monitoring Program Products and Supporting Functions

IV. References

None noted

V. Acronyms and Definitions

A. AgF – Silver Fluoride

B. NIOSH – National Institute of Occupational Safety and Health

C. PPE – Personal Protective Equipment

VI. Responsible Office

Training Operations Support Services

VII. Instructions

A. Tools Required (Quantity)

1. Cleaning Solution (Liquid soap and water) in spray bottle

2. Paper towels

3. Hearing protection

4. Nitrile or butyl rubber gloves

5. Punch (1) 3/8” diameter

6. Teflon Block

7. Hammer

8. Tweezers or Medium Screw Driver

9. Labled haz waste container

10. Bagged AgF sheets (signed out from Laboratory personnel)

11. Labeled AgF containers/laboratory (2)

FOR OFFICIAL USE ONLY 2

12. AMPF 038

13. Shop vacuum

14. Eye protection

15. Lab coat

NOTE 1: A new punch may be obtained from the O&M Safety Manager

B. Preparation of Work Station

1. Pour one cap full of liquid soap into spray bottle and fill with water to make cleaning solution..

2. Place Teflon block on the work station.

3. Gather all tools and equipment used for the process.

4. Place the labled haz waste container near the work station.

5. Turn on shop vacuum.

NOTE 2: Work station is a table located in the O&M building.

NOTE 3: Do not expose AgF material to moisture or prolonged light as it can alter the integrity of the material.

6. Don PPE used during the process (hearing protection, eye protection, nitrile or butyl rubber gloves and lab coat).

7. Unwrap the AgF sheets and place one (1) sheet onto the Teflon Block.

8. Using the punch and hammer, punch AgF pads and put into labeled container.

9. For quality control, place one random AgF pad per sheet into the appropriately marked sample container provided by the laboratory.

10. Retrieve any scrap AgF material and place it in the labled haz waste container.

NOTE 4: When removing scrap material, be sure to check for loose AgF pads or pads that may be stuck in the punch.

NOTE 5: Damaged pads can be placed inside the labled haz waste container.

11. Once complete, repeat steps C.2 – C.5 above for remaining AgF sheets.

12. Place both containers back into the bag supplied by the laboratory and sign AMPF 038.

13. Return the bag and AMPF 038 to laboratory personnel.

C. Work Station Clean-Up

1. Thoroughly wipe down the work station and all tools used with cleaning solution.

2. Place lab coat and all paper towels and gloves used to clean the workstation inside the labled haz waste container.

3. Return the punch, hammer, and Teflon Block to the chemical laboratory.

FOR OFFICIAL USE ONLY 3

4. The labled haz waste container shall be given to the O&M Safety Manager for storage in the AgF satellite accumulation drum.

VIII. Forms Prescribed

CDP COBRATF AMPF 038, Certificate of Compliance / Silver Fluoride (AgF) Conversion Sheets