Attachment_14_Laboratory_Operations.pdf

Training Operations and Support

Services – COBRATF

Attachment 14

COBRATF Laboratory Operations

Standard Operating Procedures CDP COBRA Training Facility Title: Safety In The Laboratory SOP Number: CDP COBRATF 6.1.5 Prepared by: Chemical Agent Laboratory Quality Review: Chemical Hygiene Review:

CDP COBRATF Assistant Director Approval: Approval Date: 2/23/11

Revision: 5 6.1 Page 1 of 10 Effective Date: 2/28/11

1.0 Objective

Provide instruction to personnel on safety measures that are essential

2.0 Scope

Operations & Maintenance (O&M) Personnel, Air Monitoring Personnel, Laboratory Personnel and any other employee assigned to do work at the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) Chemical Agent Laboratory

3.0 References

3.1 CDP COBRATF Standards Document

3.2 CDP COBRATF SOP 1.18, Disposition of Expendable and Non-Expendable Materials in Toxic Agent Training Area

3.3 CDP COBRATF SOP 3.1, Respiratory Protection for Visitors

3.4 CDP COBRATF SOP 6.2, QA/QC – QLs, QPs, GC Performance for Type 2

Method & Confirmation of Agent

3.5 CDP COBRATF SOP 7.1, Chemical Agent Material Accountability and RDTE Solution Accountability

3.6 CDP COBRATF SOP 16.1, ERP for Lab Neat Agent Operations

3.7 CDP COBRATF Form 4.18.V, Lab Entry Log

3.8 CDP COBRATF Form 4.18.X, Laboratory Pre/Post Operational Checks

4.0 Procedures

4.1 Laboratory Entrance

A sign is posted on the laboratory door that warns personnel of the presence of VX and GB and lists the entrance requirements.

4.2 Containment of Agent

4.2.1 Containment of agent liquid and vapors is required at all times within the laboratory. When agent must be removed from the containment provided by the laboratory ventilation hood, the following restrictions apply:

a. Neat agent is doubly contained. Personnel must wear a protective mask.

Standard Operating Procedure CDP COBRA Training Facility

Revision: 5 6.1 Page 2 of 10 Effective Date: 2/28/11

b. Whenever possible, quantities of agents that are above the levels defined as Research, Development, Test and Evaluation (RDT&E) dilute solutions material are not brought out of the hood into the laboratory.

c. Aliquots of stock solution that are greater than the levels defined as surety material (concentrations greater than RDT&E solutions) will be treated the same as neat agent, in terms of containment.

4.2.2 A single containment system must totally contain agent liquid and vapor.

Examples include glass bottles with screw caps, syringes, vials with septums, and sealed ampoules.

4.2.3 A double containment system must provide total primary containment as above and, in the event of leakage or breakage of the primary containment, must totally contain agent liquid and substantially contain agent vapors. Examples of secondary containment include, but are not limited to, metal cans with friction fit lids containing absorbent material and sealed syringe carriers.

4.3 Ventilation/Hood System

NOTE: When surveyed by the Industrial Hygiene Technician, all three hoods must maintain an inward airflow as verified by smoke tests or other visual means per the CDP COBRATF Standards Document.

4.3.1 An Industrial Hygiene Technician/Officer performs face velocity surveys on a quarterly basis and when the system has undergone major repairs.

A Lab Technician checks and records (on CDP COBRATF Form 4.18.X) the average face velocity at the beginning of each operational day, using a Thermo-Anemometer or similar instrument. The average daily reading is 100 + 10 lfpm. Notify Safety Control if the average face velocity is not within range and do not work under the hood.

4.3.2 Leave the ventilation hood open only while working with agent and/or other toxic materials. Close the hood at the end of the operation.

4.3.3 No agent or agent-contaminated equipment located inside a ventilation hood should be allowed within twenty (20) centimeters of the face of the hood. This is designated by taped line on the hood floor.

4.3.4 The hood is provided with both visible and audible alarm devices that are activated when the magnehelic reading is outside the set range. The visible alarm is located so that personnel, while working at the hood, can readily see it. Each day personnel enter the laboratory, hood alarms are checked. The audible alarm is checked by turning the power "off" and

Revision: 5 6.1 Page 3 of 10 Effective Date: 2/28/11 then “on”, which should activate the alarm. The visible alarm is checked to see if the red light is on. If the alarms are not functioning properly, O&M Personnel will be notified.

4.3.5 The filtration/ventilation/hood system in the laboratory remains on at all times.

4.3.6 In Case of Ventilation Failure:

a. Stop work, hold breath, and mask immediately.

b. Properly secure any surety material that is out.

c. Evacuate the laboratory.

4.4 Agent Monitoring

4.4.1 Monitoring of laboratory air is accomplished on a continuous basis by the Miniature Chemical Agent Monitoring System (MINICAMS) at the Short Term Exposure Limit (STEL) level and during hot operations at the COBRATF Maximum Concentration Limit (CMCL) level.

4.4.2 The following conditions require first entry monitoring, protective clothing, and possible decontamination:

a. Agent spill outside of containment.

b. Major spill within the hood, containing any agent.

c. Ventilation failure of a hood with uncontained agent.

d. Ventilation failure of hood with contained agent and lasting longer than 24 hours.

4.4.3 Designated personnel do first entry monitoring of the laboratory. A protective mask is worn as a minimum, until negative results are obtained from MINICAMS and Depot Area Air Monitoring System (DAAMS) samples as needed, and the ventilation has been restored for at least 30 minutes.

4.4.4 A secondary power failure indication is considered as a ventilation failure.

If security personnel/Safety Control indicate a power failure has occurred, determine the date, time, and duration of the power failure (indication light on lab control panel should be on). If the power failure has been less than 24 hours, and security/Safety Control personnel indicated power has been restored for at least 30 minutes, and the hood blower is operating, Revision: 5 6.1 Page 4 of 10 Effective Date: 2/28/11 personnel may enter the laboratory in street clothes. If the power failure was longer than 24 hours, then first entry monitoring is required.

4.4.5 For the following conditions, entry in street clothes with visual observation for tampering, leakage, or ventilation failure is acceptable:

a. Normal entry with no apparent problems.

b. Following restoration of ventilation for at least 30 minutes in a hood used for storage of agent (not to include agent in decontamination solutions) provided the ventilation loss did not exceed 24 hours.

4.5 Protective Clothing & Equipment

NOTE: When wearing butyl rubber impermeable protective clothing, wearers must avoid contact with open flame or objects, which ignite the clothing. The material burns and does not possess self-extinguishing properties.

4.5.1 Appropriate CDP COBRATF personnel are issued a properly fitted protective mask. If visitors to the lab do not have a protective mask refer to the CDP COBRATF Standard Operating Procedure (SOP) 3.1.

4.5.2 Approved gloves are worn when working with agent at or above surety levels, or with samples of unknown concentration. Extreme caution must be taken not to remove gloves, possibly contaminated equipment or sample containers that may have been contaminated, from the safe confines of the fume hood until a safe level of decontamination has been reached.

4.5.3 Goggles and rubber apron (or lab coat) are worn when using volatile solvents, bases, or acids.

4.5.4 Personal protective clothing, Level C, is kept readily available for use in cases of emergency or for operations requiring Level C protective clothing. The protective clothing is kept available for emergency operations or worn where contamination is encountered. All protective clothing is inspected and tested by PC&E.

4.5.5 If a splash hazard exists, a face shield and chemical goggles must be worn or the sash must be lowered enough to protect the face.

4.6 Personnel must remove all jewelry from hands and arms before the start of an operation involving agent.

Revision: 5 6.1 Page 5 of 10 Effective Date: 2/28/11

4.7 VX/GB Contamination

See CDP COBRATF SOP 16.1.

4.8 Emergency Shower & Eye-Wash

The personnel deluge-shower and eyewash are accessible to all workstations within the laboratory. The laboratory personnel, to ensure working conditions, do a check of the deluge-shower and eyewash. See CDP COBRATF Form 4.18.X.

4.9 Access to Exits

Equipment is installed in a position that ensures free access to exits. Means of exit are maintained free of all obstructions or impediments to allow full instant use in case of a fire, agent release, or other emergency.

4.10 Fire Extinguishers

Fire extinguishers are mounted in readily accessible locations in the laboratory.

The fire extinguishers are checked monthly by the O&M personnel.

4.11 Entry to the Lab

Entry to the laboratory is restricted to authorized personnel. During normal operations, a maximum of 6 and a minimum of 2 personnel are allowed inside the laboratory. In addition, the laboratory is locked when unoccupied. All visitors entering the laboratory must sign into the laboratory on the appropriate form.

4.12 Training of personnel

Personnel who work with agents are trained in the use and handling of toxic agents prior to assignment; how to don, wear, and remove protective clothing; the use of decontaminating materials; and the procedures to be followed in the event of a spill or exposure. Personnel receive training, and then are tested yearly on the signs and symptoms of agent poisoning on a continuing basis.

4.13 Decontaminating Material

A supply of decontaminating material adequate for the quantity of agent present is immediately available in the laboratory. The sodium hypochlorite solutions (bleach) used as decontaminating material are tested annually for available chlorine. The containers of sodium hypochlorite solutions (bleach) are labeled with the available chlorine content and date tested.

4.14 Removing Agent

Butyl gloves over surgical gloves are used for removing vials/ampoules of agent from carrying containers, and for handling ampoules containing agents. Use right hand while removing the syringes and agent containers from the glove box pass-through chute to avoid possible dropping of the agent outside the hood.

4.15 Equipment Used in Agent Analysis

All equipment used, to include but not limited to glassware, tongs, forceps and syringes, are decontaminated immediately upon completion of analysis.

Revision: 5 6.1 Page 6 of 10 Effective Date: 2/28/11

4.16 In Case of Emergency

In the event of a chemical accident/incident or fire, the appropriate alarms are located so that they may be activated while in duress.

4.17 Eating, Drinking, Chewing, Smoking

No eating, drinking, chewing or smoking is permitted in the toxic laboratory.

4.18 Potentially Hot Samples

All incoming samples to the laboratory from the hot area are considered potentially hot and treated as such by monitoring and laboratory personnel. These samples are placed under the hood, deconned, and analyzed to verify the presence of agent.

4.19 Confirmation of an Agent Present by DAAMS:

See CDP COBRATF SOP 6.2.

4.20 Labeling Containers Containing VX & GB: See CDP COBRATF SOP 7.1.

4.21 Covering of Open Sores or Wounds

The Supervisor refers personnel working in the laboratory with open sores or wounds to the CDP COBRATF Medical Staff for appropriate medical action prior to being issued permission to enter the laboratory.

4.22 Inspection for Symptoms of Agent Exposure

Personnel are checked for symptoms by Safety Control personnel before leaving the training building.

4.23 Reporting of Abnormal Situations

Any agent exposure, suspected exposure, agent spill or release, or other abnormal situation that may result in personnel injury must be reported to supervisory personnel immediately after taking the necessary emergency actions.

Personnel with possible agent exposure report for medical evaluation as soon as possible. Immediately halt any operation when abnormal or hazardous conditions occur.

4.24 Use of Suction Bulbs or Mechanical Pipettes

Do not use mouth for pipetting any liquid. Use a suction bulb or mechanical pipette to avoid possible contact of the mouth with a contaminated pipette.

4.25 Handling Concentrated Acids and Bases

4.25.1 Particular care is required when handling concentrated acids and bases.

Concentrated acids and bases should be added carefully to water and never water to acid or base. When a person is splashed with an acid or base, large volumes of water are required immediately to prevent serious burns.

Revision: 5 6.1 Page 7 of 10 Effective Date: 2/28/11

4.25.2 When using volatile solvents, bases or acids, the work is performed under a ventilation hood. For example, nitric acid, in addition to being injurious to the skin and eyes, is a strong oxidizer of organic materials.

The oxidation of some organic materials may produce products such as TNT, and Nitroglycerine, with the possibility of fire or explosion. To assure safety, use the hood and wear gloves and goggles.

4.26 Working Areas Should be Free of Obstacles

Make sure that the working surface where agent is to be handled is clear and free of obstruction. The work area is maintained and left in a neat and orderly manner at all times.

4.27 Glassware (Please see Appendix A for common laboratory equipment).

4.27.1 Disposing of Bad Glassware - All chipped, cracked, or broken glassware is placed in a special container, after decontamination, for disposal. Do not pick up broken pieces of glass with bare hands. Use tongs for large pieces and paper towels for small pieces. This special container is marked “For Broken Glass Only”. When filled, pour approximately 2-3 inches of bleach inside container and put in the pass-through chute.

4.27.2 Never put excessive pressure on glassware with bare hands.

4.27.3 Use care in making rubber-to-glass connections. Lengths of glass tubing should be supported while they are being inserted into rubber. The ends of the glass should be fire polished and a lubricant, water or a water-soluble lubricating jelly should be applied when making such connections.

The tubing should be as close to the end being inserted as possible to prevent bending or breaking.

4.27.4 Never try to force rubber tubing or stoppers from glassware. Cut the rubber or material off.

4.28 Flushing Chemicals Down Drain

Check the MSDS for proper disposal of chemicals. If the chemical can be flushed into the underground hold tank, use plenty of water.

4.29 Handling Chemicals

All neutralized liquid wastes are disposed of through the lab drain system to the sump. When the lab sump is full, it automatically empties itself into the CDP COBRATF waste holding tank. All possibly contaminated solid waste is placed in double plastic bags, put in the pass-through-chute by lab personnel and then handled as per CDP COBRATF SOP 1.18.

Revision: 5 6.1 Page 8 of 10 Effective Date: 2/28/11

4.30 Decontamination of Waste Equipment and Spills

4.30.1 Decontaminating agents that are acceptable for decontaminating waste, equipment, and spills of gross neat agent contamination include:

a. High Test Calcium Hypochlorite or Calcium Hypochlorite Dry (HTH) (nominal 10%), Super Tropical Bleach (STB) slurry or sodium hypochlorite (bleach) with approximately 5% total available chlorine for VX.

b. Ten percent Sodium Hydroxide (10% NaOH), caustic soda, or sodium hypochlorite (bleach) with approximately 5% total available chlorine for GB.

4.30.2 For dilute GB and VX, commercial bleach (Sodium Hypochlorite solution) is sufficient.

4.31 CDP COBRATF Form 4.18.X

Laboratory personnel prior to beginning operations and before closing the lab each day perform daily checks following CDP COBRATF Form 4.18.X.

4.32 Visitors to the Lab

4.32.1 All personnel entering the toxic lab in the training building of the CDP

COBRATF are familiar with the requirements listed in this SOP or are accompanied by a certified lab person.

4.32.2 Visitors to the laboratory are given a briefing on laboratory safety procedures.

4.33 In Case of Severe Weather

4.33.1 If a tornado or other severe weather warning is in effect, stop all agent operations.

4.33.2 Secure agent in the vaults and secure the vault hood.

4.33.3 Move to appropriate safe location under Safety Control directions.

4.34 In Case of Fire in the Lab

4.34.1 Determine the type fire (electrical, oil/solvent, or other).

4.34.2 Use the appropriate fire extinguisher to extinguish the fire while co-worker notifies Safety Control. If Halon is used in this operation, the fire extinguisher should be used as personnel exit the lab.

Revision: 5 6.1 Page 9 of 10 Effective Date: 2/28/11

4.34.3 If unable to extinguish the fire and/or smoke begins to cause irritation, evacuate the laboratory immediately.

4.34.4 If the situation permits, secure all agent vaults and vault hood.

4.34.5 Evacuate the laboratory.

4.35 Equipment and Supplies

ITEM QUANTITY

Signs As Required Ventilation/Filtration Systems 1

Deluge – Shower & Eye - Wash 1 Fire Extinguishers 2 Decon Material As Required Alarm To Safety Control & Guard Post 1 Ampoules As Required Parafilm As Required Thermo Anemometer 1

LEVEL C REQUIREMENTS

Mask 1/person Toxicological Agent Protective (TAP) Apron 1/person Butyl Rubber Gloves With Inserts 1/person TAP Boots 1/person

Revision: 5 6.1 Page 10 of 10 Effective Date: 2/28/11

APPENDIX A: COMMON LABORATORY EQUIPMENT

Title: QA/QC – QLs, QPs, GC Performance for SOP Number: CDP COBRATF 6.2.9 Type 2 Method & Confirmation of Agent Prepared by: Chemical Agent Lab Quality Review: Chemical Hygiene Review:

Revision: 9 6.2 Page 1 of 5 Effective Date: 2/28/11

To prepare Quality Laboratory (QL) and Quality Process (QP) Samples and determine the control status of gas chromatographs

2.0 Scope

All personnel assigned to the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) Chemical Agent Laboratory

3.1 Quality Control Plan for the Chemical Agent Laboratory at the CDP COBRATF

3.2 CDP COBRATF Form 4.18.FA, DAAMS Tube Status Sheet

3.3 CDP COBRATF Form 4.18.FB, DAAMS Tube Status Sheet Continuation

3.4 CDP COBRATF Form 4.18.FC, DAAMS Tube Preparation and Acceptance

3.5 CDP COBRATF Form 4.18.IL, QL/QP Quality Data Sheet

3.6 CDP COBRATF SOP 6.15, V-to-G Conversion Filters (AgF Pads)

3.7 CDP COBRATF SOP 6.25, Preparation and Analysis of DAAMS Samples

3.8 CDP COBRATF SOP 6.30, Procedures for DAAMS Tubes

3.9 Chemical Agent Standard Analytical Reference Material (CASARM) Quality

Assurance (QA) Plan for Chemical Agent Air Monitoring At Training Facilities

4.1 Major Equipment & Supplies:

4.1.1 6mm Depot Area Air Monitoring System (DAAMS) tubes

4.1.2 V-to-G Conversion Filter

4.1.3 Vacuum pump

4.1.4 Sampling manifolds

Title: Receipt of CASARMS Solutions SOP Number: CDP COBRATF 6.3.4 Prepared By: Chemical Agent Lab Quality Review: Chemical Hygiene Review:

CDP COBRATF Assistant Director Approval: Approval Date: 12/27/10

Revision: 4 6.3 Page 1 of 3 Effective Date: 1/3/11

Establish procedures to receive, unpack, inventory and record Chemical Agent Standard Analytical Reference Material (CASARM) solutions.

The provisions of this Standard Operating Procedure (SOP) are applicable to all personnel assigned to the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) Chemical Agent Laboratory and the Supply Technician.

3.0 Reference

3.1 Army Regulation 50-6

3.2 SOP CDP COBRATF 7.1, Chemical Agent Material Accountability and RDTE

3.3 DD Form 1911

3.4 CQATFM SR-11, Shipment Status Report

4.0 Procedures

4.1 Coordinate Shipment

CASARM solutions are prepared by U.S. Army Edgewood Research, Development and Engineering Center, CASARM Quality Assurance Branch, Aberdeen Proving Ground, MD. The Laboratory Director coordinates shipment of the CASARMS dilute solutions to CDP COBRATF.

4.2 Movement to CDP COBRATF Laboratory

NOTE 1: The Laboratory personnel are notified when the CASARM solutions have arrived and are ready for pick-up.

NOTE 2: If the solution is received after duty hours, it is placed in the storage area.

Laboratory personnel are notified so inventory can be performed the next working day.

4.2.1 Inspect the shipping container for obvious signs of leakage.

NOTE 3: 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.

Title: Laboratory Gloves SOP Number: CDP COBRATF 6.5.3 Prepared By: Chemical Agent Lab Quality Review: Chemical Hygiene Review:

Revision: 3 6.5 Page 1 of 3 Effective Date: 1/3/11

Provide personnel protection for the Center for Domestic Preparedness’ (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) laboratory.

This Standard Operating Procedure (SOP) is applicable to all personnel assigned to the CDP COBRATF Chemical Agent Laboratory and PC&E (Protective Clothing and Equipment) personnel.

3.1 Army Regulation 50-6

3.2 CDP COBRATF Standards Document

3.3 CDP COBRATF Chemical Hygiene Plan

3.4 CDP COBRATF Form 4.18.AM, Glove/Filter Changing Schedule

4.1 Types of Gloves Used

4.1.1 Chemical protective butyl rubber gloves (Standard) are used when handling agent contaminated or potentially contaminated items and for emergency situations in the handling of agent and/ or to clean up spills outside the hood or glove box. These gloves are also used as covers over glove box gloves.

4.1.2 Glove box gloves are used for all glove box operations. These gloves are

15 mil butyl rubber gloves (Non Standard).

4.1.3 Exam gloves are used in handling all non-agent containing reagents, and research development testing and evaluation (RDTE) solutions.

4.2 Changing Chemical Protective Gloves

4.2.1 A pair of gloves is left in the front of each hood.

4.2.2 At least once a month these gloves are replaced. Old gloves are consolidated, bagged, and placed in the pass through chute for PC&E cleaning and re-certification. Gloves contaminated with liquid neat agent are deconned and discarded with the hot trash and destroyed.

Title: Laboratory Gloves SOP Number: CDP COBRATF 6.5.3

Revision: 3 6.5 Page 2 of 3 Effective Date: 1/3/11

4.3 Changing Surgical Gloves:

4.3.1 These gloves are changed when torn, contaminated, or as necessary.

4.3.2 The gloves are removed and placed in the regular trash. If the gloves were worn during hot operations, the gloves are placed in the hot trash container in the vault hood. The hot trash is bagged at the completion of agent operations and transferred through the pass through chute for destruction.

4.4 Changing Glove Box Gloves

NOTE 1: This is a two-person operation. IT IS NOT to be done alone.

4.4.1 Person 1: First, loosen the clamp on one glove with a screwdriver or nut driver.

4.4.2 Remove the clamp and felt strip.

4.4.3 Remove the O-ring and roll the edge of the glove into the grove where the

O-ring was located.

4.4.4 Person 2: Place the new glove on your arm and roll the top of the glove down a few inches.

4.4.5 Place your arm with the new glove inside the old glove.

4.4.6 Person 1: Place the end of the new glove over the glove box adapter, smoothing the glove out to the seal.

4.4.7 Persons 1 & 2: Hold the new glove in place while person 2 removes the old glove.

4.4.8 Person 2: Remove arm from new glove.

4.4.9 Person 1: Replace the O-Ring, felt strip, and clamp.

4.4.10 Repeat 4.4.1 to 4.4.9 for the other glove.

4.4.11 Bag the old gloves and place in the pass through chute for cleaning and recertification by laundry.

4.4.12 Glove box gloves and butyl rubber gloves in the hoods are changed out with a clean, certified pair of gloves immediately following neat agent operations. The change dates are recorded on CDP COBRATF form

4.18.AM.

Title: Laboratory Gloves SOP Number: CDP COBRATF 6.5.3

Revision: 3 6.5 Page 3 of 3 Effective Date: 1/3/11

NOTE 2: Gloves contaminated with liquid neat agent are deconned and discarded with the hot trash and destroyed. If used in emergency operations, they are discarded after use for destruction and replacements obtained.

4.5 Safety Consideration

4.5.1 When wearing butyl rubber impermeable protective clothing avoid contact with open flames or objects that ignite clothing. This material burns and does not posses self-extinguishing properties.

4.5.2 The Emergency Shower is located in the laboratory next to the agent vault hood.

4.5.3 The Emergency Eye-Wash station is located in the sink next to the agent vault hood.

4.5.4 Fire Extinguishers are mounted on the walls of the laboratory. One is located next to the agent vault hood and one is located next to the front door of the laboratory.

Revision: 4 6.3 Page 2 of 3 Effective Date: 1/3/11

4.2.2 Laboratory personnel transport boxes to the laboratory.

4.3 Inside Laboratory:

NOTE: This operation is performed using the two-person rule.

4.3.1 Notify Safety Control of intent to unpack boxes.

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

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

4.3.4 If the ampoules are cracked and/or leaking, decontaminate the ampoule and the solution. Decontaminate the other unbroken ampoules, as well as, all packing material and containers that are contaminated. Dispose of contaminated waste by double bagging and placing in the vault hood pass through chute.

4.3.5 Place unbroken ampoules in labeled containers (as instructed in section

4.4) and store in the refrigerator.

4.4 Label each container with:

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

4.4.2 National Fire Protection Association (NFPA) Label

4.5 Accountability: Complete all paperwork per CDP COBRATF SOP 7.1.

4.5.1 Check each shipment for the following:

a. Certificate of Analysis for CASARM grade solutions or a memorandum for record stating concentration of solutions– one for each agent solution shipped.

b. DD Form 1911

c. CQATFM SR-1, Shipment Status Report

Revision: 4 6.3 Page 3 of 3 Effective Date: 1/3/11

4.5.2 An agent accountability officer indicates acceptance of custody on the DD

Form 1911.

4.5.3 All accountability documents are returned to the CDP COBRATF accountability officer.

4.6 Safety Considerations

4.6.1 For containment purposes, treat aliquots of stock solution with concentrations greater than RDT&E solutions the same as neat agent, in terms of containment.

4.6.2 A single containment system must totally contain agent liquid and vapor.

Examples include glass bottles with screw caps, syringes, vials with septums, and sealed ampoules.

4.6.3 The laboratory hoods must be certified and within range (100+/- 10 linear feet/ minute) through the working opening when agent operations are conducted.

4.6.4 Do not place agent or agent-contaminated substance within twenty centimeters of the face of the hood.

4.6.5 In case of ventilation failure stop breathing, stop work, and mask immediately.

Properly secure any surety material that is out and evacuate the laboratory.

4.6.6 If chemical containment occurs, use the Emergency Shower located in the laboratory next to the agent vault hood.

4.6.7 In case of a chemical splash in the eyes use the Emergency Eye-Wash station located in the sink next to the agent vault hood.

4.6.8 In the event of a fire use Fire Extinguishers mounted on the walls of the laboratory. One is located next to the agent vault hood and one is located next to the front door of the laboratory.

Type 2 Method and Confirmation of Agent

Revision: 9 6.2 Page 2 of 5 Effective Date: 2/28/11

4.1.5 Calibrated flowmeter

4.1.6 Syringes

4.1.7 Timer

4.1.8 Daily standard solutions

4.2 Assemble necessary equipment.

4.3 Obtain chromatographically clean 6mm DAAMS tubes (See CDP COBRATF SOP

6.30).

4.4 Assemble V-to-G conversion filters and 6mm tubes in-accordance-with (IAW) CDP

COBRATF SOP 6.15.

4.5 Obtain appropriate Daily Standard Solutions and syringe.

4.6 QL Preparation: QLs are used to check the performance of analytical systems used by the laboratory for the determination of agent.

4.6.1 QL samples are prepared in the laboratory.

4.6.2 Using appropriate fittings, assemble the vacuum pump and sampling manifold in the laboratory, if needed.

4.6.3 Place the 6mm tubes with V-to-G conversion filter units in the manifold and turn on the vacuum pump. Adjust the flow rate to 1 L/min. Spike an appropriate quantity of the “Q” daily standard solution onto the center of the outer surface of the V-to-G conversion filter. Aspirate for 5 minutes to remove solvent residue from the sorbent.

4.6.4 Record data on CDP COBRATF Form 4.18.IL.

4.6.5 Analyze QL sample IAW CDP COBRATF SOP 6.25.

4.7 QP Preparation:

When QPs are going to be aspirated along with real samples, obtain two chromatographically clean 6mm tubes with V-to-G conversion filters attached.

4.7.1 Using appropriate fittings, assemble the pump and sampling manifold in the laboratory, if needed.

Revision: 9 6.2 Page 3 of 5 Effective Date: 2/28/11

4.7.2 Place the tubes in the manifold and turn on the pump. Adjust the flow rate to 1 L/min. Spike a 1Z equivalent quantity of the “Q” Daily Standard solution onto the center of the V-to-G conversion filter. Aspirate for 5 minutes. Check final flow. Include QPs with 6mm tubes needed for sampling in the field.

4.7.3 Record data on CDP COBRATF Form 4.18.IL.

4.7.4 Analyze QP sample IAW CDP COBRATF SOP 6.25.

4.8 Establish GC Performance Data (if needed): Record all QL/QP results on CDP

COBRATF Form 4.18.IL.

4.8.1 Use the Calibration Daily Standard solution to prepare the QLs set to establish the 0.5 – 1.5Z QL range and for the 1.0Z QL used to initially check the range. Use the ”Q” Daily Standard solution for all other QLs and QPs.

4.8.2 Note that a 1.0Z QL sample will be run each day before determining the area responses for QPs or real samples.

a. Any day an instrument is used to analyze unknown samples by the DAAMS technique, the gas chromograph (GC) is challenged with a 1.0Z QL. Each sample consists of a real sample and a 1.0Z QP.

The real sample is analyzed and a QP is analyzed. The 1.0Z QP area responses for each agent must show at least a 3:1 signal to noise ratio for the respective responses obtained for the 1.0Z QL sample run on the same day. If necessary a second real sample and QP can be analyzed. If the 1st QP fails and the 2nd QP passes and an assignable cause can be attributed to the failure of the 1st QP, the analysis is valid.

b. If the second QP fails, a 1.0Z QL is analyzed. If the QL passes, the instrument is considered in control. If the QL fails, the instrument is considered out of control. The problem must be assessed and the range re-established before the instrument can be used for analysis again. In either case the analysis is not valid.

c. The area response for any real sample (i.e., unknown sample) collected must be three times greater than the noise to show the presence of an agent to be confirmed by DAAMS.

d. In the event that DAAMS are used as the primary method of analysis

(for example, screening the site perimeter or other site locations), 1

Revision: 9 6.2 Page 4 of 5 Effective Date: 2/28/11

QP is required at the beginning (or change of agent), with an additional QP every 4-5 hours, and 1 QP at the end of operations.

4.8.3 Any day an instrument is used for other analysis (test Silver Fluoride (AgF) pads, check cleaning process on DAAMS tubes, etc.), the GC is challenged with a 1.0Z QL. To pass, the QL area responses for each agent must be between the 0.5Z QL and 1.5Z QL established earlier in the week. If the QL passes, the instrument is in control and the analysis is valid.

NOTE: If a QL fails, the operator is allowed to analyze a second QL. If the second QL passes, the analysis is valid. If the second QL fails, the instrument is considered out of control and the analysis is considered invalid and must be repeated on an instrument considered in control. The operator then investigates the out of control situation to determine a possible cause and then must re-establish the range. A 1.0Z QL must pass before the instrument is considered in control. The QLs required to re-establish the range are prepared from the Calibration Standard series of dilutions.

4.9 Continuing Checks of DAAMS Tubes

4.9.1 Complete the top portion of a new CDP COBRATF Form 4.18.FA. If any tube was discarded during the testing phase, comment on CDP COBRATF Form 4.18.FA. When any tube is discarded for any reason, a comment is written on CDP COBRATF Form 4.18.FA.

4.9.2 After a lot of tubes are used, they must be chromatographically cleaned before the lot can be re-used. Chromatographs are filed with the cleaning information.

a. 6mm Tubes: To clean - desorb tube in the heating block set at 200 +

10°C for approximately 3 minutes manually or desorb in the automatic thermal desorption (ATD). Accountability of the 6mm tubes must be maintained at all times so when the tube’s pen clip is removed, care must be taken to ensure the correct pen clip is returned to the correct 6mm tube. When the ATD is used to clean the tubes, all tubes are cleaned and have a clean chromatograph prior to being used again.

b. To test the cleaning process, refer to the CASARM QA Plan, Table

12-1, to determine the number of tubes to be sampled on the GCs manually. Write results on CDP COBRATF Form 4.18.FB.

c. If the Area Response for VX or GB > a 3:1 signal to noise ratio, the entire lot is cleaned again and retested or the lot is discarded unless a chromatogram is produced for each tube within the lot that is

Revision: 9 6.2 Page 5 of 5 Effective Date: 2/28/11 being cleaned, then only the tube that is in question needs cleaning again.

4.9.3 1Z QLs will be used to monitor the tube’s continuing ability to recover agent. The tube passes if the Area Response for VX and GB > 75% of the previous 1.0Z QL’s Area Response when the range was last determined.

If the tube fails and low recovery cannot be attributed to another problem, the tube is removed from service. Write comment on CDP COBRATF Form 4.18.FA.

4.9.4 Each time a DAAMS tube is used for analysis or challenging the GC number must be recorded (ex. When a QL is prepared, the tube numbers are recorded on the QL/QP Quality Data Sheet. CDP COBRATF Form 4.18.FA/FB can be used to record tube numbers).

4.9.5 When a lot is discarded, write the date on CDP COBRATF Form 4.18.FA and CDP COBRATF Form 4.18.FB and file chromatograms

Title: Preparation of Laboratory Standards SOP Number: CDP COBRATF 6.7.7 Prepared By: Chemical Agent Lab Quality Review: Chemical Hygiene Review:

CDP COBRATF Assistant Director Approval: Approval Date: 2/22/11

Revision: 7 6.7 Page 1 of 6 Effective Date: 2/23/11

To prepare working standards with concentrations made for calibration and Quality Check (QC) challenges, or as necessary

Personnel assigned to the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) Chemical Agent Laboratory and Air Monitoring section

3.1 Chemical Agent Standard Analytical Reference Material (CASARM) Quality

3.2 Quality Control (QC) Plan for the Chemical Agent Laboratory at the CDP COBRATF

3.3 Dilute Solution Book

3.4 CDP COBRATF SOP 6.26, Cleaning of Laboratory Glassware

3.5 CDP COBRATF Form 4.18.CV, Chain of Custody-Receipt of Dilute Solution

3.6 CDP COBRATF Form 4.18.EX, Glassware Use/Cleaning

3.7 CDP COBRATF Form 4.18.FD, Dilute Standards Solutions Worksheet

3.8 CDP COBRATF Form 4.18.FE, Special Dilute Solutions Worksheet

3.9 CDP COBRATF Form 4.18.FG, Special Dilute Solutions Worksheet Continuation

3.10 CDP COBRATF Form 4.18.FY, Dilute Ampoule Accountability by Lot

3.11 CDP COBRATF Form 4.E.3, CASARM Dilute Chemical Agent Ampoule Record

4.1 Materials/Equipment:

4.1.1 Assorted volumetric flasks and vials

4.1.2 Disposable pipettes

4.1.3 Syringes or other appropriate measuring device

Revision: 7 6.7 Page 2 of 6 Effective Date: 2/23/11

4.1.4 Dilute CASARM ampoules

4.1.5 Solvent (isopropyl alcohol – IPA Reagent Grade at a minimum)

4.1.6 Bleach

4.1.7 Deionized water

4.1.8 Labels

4.2 General Information

NOTE: Lab Technician(s) prepares calculations and provides them to the Lab Director. The Lab Director validates and approves the calculations. Once this requirement is complete, these calculations become Director’s Notes. The notes are then released to the Lab Techs for solution preparation.

4.2.1 Laboratory Director’s Note of Explanation: These notes give directions on which source solution should be used, how much of the source solution should be used and the volume of the new solution. The notes for dilute solutions are stored in the Dilute Solution Book in the laboratory and can be modified to address the specific types of standard solutions requested.

4.2.2 Two sets of solutions are prepared, calibration solutions and QC solutions.

The calibration solutions are prepared from the ampoules sent by U.S.

Army Edgewood Chemical Biological Center (ECBC) with a “-C” at the end of the lot number and QC solutions are prepared from the ampoules with a “-Q” at the end of the lot number. Each set of solutions is prepared by two separate lab personnel.

4.2.3 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:

a. Agent Name (VX, GB, GX)

b. Solution Concentration

c. Solvent Name

d. Preparation Date

e. Expiration Date

f. CDP COBRATF Assigned Lot Number

Revision: 7 6.7 Page 3 of 6 Effective Date: 2/23/11

4.2.4 Lot Numbers

a. 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. The next digit is determined by the order in which the dilution is made.

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

c. At the end of the lot number for the Calibration Standards, a “-C” is placed to signify that it is a calibration standard, and the “QC” standards are followed by a “-Q”.

d. Proficiency Test solutions have a “PT” associated with the lot number.

4.2.5 Dilute CASARM Ampoules, Stock Standard Solutions and Working

Standard Solutions:

a. CASARM solutions of GB and VX are received from ECBC in glass ampoules.

b. All solutions stored at or below 4oC and removed from cold storage for use must be allowed to equilibrate to room temperature before being opened. This helps prevent contamination from the condensation of atmospheric moisture, which can hasten agent degradation.

c. When refrigerating, vial should be capped and stoppers for volumetric flasks should be wrapped with parafilm.

d. When an ampoule is used, there must be an entry on CDP COBRATF

Form 4.E.3 and CDP COBRATF Form 4.18.FY.

e. Stock Standard Solutions are made from Dilute CASARM Ampoules.

f. The expiration date for the Stock Standard Solutions and the Working

Standard Solutions is one month from the date of preparation, unless the laboratory demonstrates otherwise.

4.2.6 Ensure that the quantity of solvent from a given lot is sufficient to prepare all dilutions planned for the task at hand. The solvent used should be, at a minimum, listed as reagent grade. Record solvent name, manufacturer, grade and lot number on CDP COBRATF Form 4.18.FD.

Revision: 7 6.7 Page 4 of 6 Effective Date: 2/23/11

4.2.7 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. All glassware used for a dilution shall be cleaned per CDP COBRATF

SOP 6.26, and recorded on CDP COBRATF Form 4.18.EX.

c. 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. When finished with the syringe, rinse three (3) times with solvent before putting away.

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

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

4.2.9 Calculations: 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 solution C1 100.80 ng/uL GB

4.3 Preparation of Dilutions:

4.3.1 Assemble required equipment/supplies.

Revision: 7 6.7 Page 5 of 6 Effective Date: 2/23/11

4.3.2 Obtain CDP COBRATF Form 4.18.FD for dilute solutions, or CDP

COBRATF Form 4.18.FE/FG for special dilute solutions or other dilute solutions. Due to the importance of agent solution traceability, all items of these blank forms must be filled out completely.

4.3.3 Ampoules:

a. Open ampoule and transfer correct amount of solution to a volumetric flask using a calibrated syringe.

b. Record data.

c. Decontaminate empty ampoule and place in Hot Trash container.

d. If second vial is needed, repeat steps a-c in paragraph 4.3.3 (e.g., If a solution is being prepared that will contain both GB and VX, an ampoule of GB CASARM solution and an ampoule of VX CASARM solution will be needed).

4.3.4 Stock Standard Solutions and Working Standard Solutions

a. By using the Director’s Notes of Explanation, determine and assemble the appropriate syringe, volumetric flask with stopper, source solution and other containers needed to make the dilution.

b. Add the calculated quantity of the source standard to the volumetric flask with the selected syringe. See Director’s Notes of Explanation for the calculated quantity and source standard for each dilution.

c. Add solvent to fill the volumetric flask until the bottom of the meniscus lies on the line found on the neck of the volumetric flask. Use a pipette to add solvent when close to this line. 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.

d. Stopper the flask and mix by carefully swirling or very carefully inverting the flask several times. The stopper must be held in place with one finger while inverting.

e. Label volumetric flask and container.

f. Record data.

Revision: 7 6.7 Page 6 of 6 Effective Date: 2/23/11

g. Set containers aside. Decontaminate any glass pipettes that may have been used and discard them in the broken glass container under the hood. If any volumetric flask(s) is emptied, clean per CDP COBRATF SOP 6.26. Glassware may be cleaned at any time after a process is completed, but must be cleaned before next use. Record glassware data on CDP COBRATF Form 4.18.EX.

h. Repeat this process for each concentration of standard desired.

i. Decontaminate any unused portion of dilute CASARM ampoules (VX and GB) and record data.

j. Place all solutions in the refrigerator.

4.4 Disbursement of Standards:

4.4.1 Pipette approximately 0.5-2 mL of required standard into a labeled vial.

Seal the vial.

4.4.2 Record data on CDP COBRATF Form 4.18.FD or CDP COBRATF Form

4.18.FE/FG.

4.4.3 Standards for the Air Monitoring Section must be signed for by Air

Monitoring personnel on CDP COBRATF Form 4.18.CV.

4.4.4 Any unused portion of the vial is decontaminated.

4.4.5 Whenever an Air Monitoring Technician needs a standard solution vial to use in the hot area, provide the vial in a plastic bag or other suitable, sealable container. The Air Monitoring Technician must return the standard solution vial by placing it in the pass through chute.

4.4.6 Once returned to laboratory personnel, the standards may be destroyed by pouring bleach into the container, letting sit for at least five (5) minutes and emptying contents into the Hot Trash container.

Title: Calibration and Use of pH Meter SOP Number: CDP COBRATF 6.12.4 Prepared By: Chemical Agent Laboratory

Revision: 4 6.12 Page 1 of 2 Effective Date: 2/28/11

To establish a procedure for the calibration and use of a pH meter and insure that this instrument performs properly and gives accurate measurements.

Applicable to all personnel assigned to the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, Radiological Training Facility (COBRATF) Chemical Agent Laboratory.

3.1 PerpHect Meter Models 310, 320, 330 Instruction Manual, Thermo Orion.

3.2 PerpHect Ag/AgCl pH Electrodes Instruction Manual, Thermo Orion.

4.1 Prepare Electrode

4.1.1 Clean any salt deposits from the exterior of the electrode by rinsing with deionized water.

4.1.2 Remove plastic sleeve from over fill hole. Check the level of the filling solution (4M KCl w/AgCl) in the pH electrode. To maintain an adequate flow rate, the level of filling solution must always be above the reference junction and at least one inch above the sample level when immersed.

Fill as necessary with filling solution.

4.2 Autocalibration with Two Buffers

NOTE 1: The buffers used for calibration and the samples must be approximately the same. Stir all buffers and samples during pH measurement (swirl the container by hand or by magnetic stirrer).

NOTE 2: To rinse, place electrode in distilled/deionized water and then into an extra container filled with the solution to be measured (either the buffer or sample).

4.2.1 Calibrate by using pH 7.00 and pH 10.01 buffers.

4.2.2 Press CAL key to initiate calibration sequence. CAL is displayed for two seconds. Press the YES key to accept the last calibration range (7-10) or select one of these calibration ranges using the SCROLL ( ▲ , ▼) keys.

Title: Calibration and Use of pH Meter SOP Number: CDP COBRATF 6.12.4

Revision: 4 6.12 Page 2 of 2 Effective Date: 2/28/11

Press the YES key to accept. pH 7 will be displayed for two seconds.

Rinse electrode (see note 2) and place electrode in pH 7.00 buffer.

Reading will be displayed and updated as calibration continues. When the READY light come on, indicating electrode stability, press the YES key to accept.

4.2.3 pH 10 will then be displayed for two seconds. Remove electrode from pH

7.00 buffer. Rinse electrode (see note 2) and place in pH 10.01 buffer.

When the READY light comes on, press the YES key to accept buffer value. SLP will be displayed for two seconds, and then the calculated slope will be displayed.

4.2.4 Slope should be 92% to 102%. If slope is outside this range, see troubleshooting section in the Instruction Manual.

4.2.5 Meter will automatically go into the MEASURE mode. The READY light will come on to indicate electrode stability.

4.2.6 Rinse electrode.

4.3 Measure the pH of the Unknown Sample

4.3.1 Immerse electrode in sample. Record pH directly from the main meter display when the READY light is displayed, or when the electrode signal is stable.

4.3.2 Replace cap filled with electrode storage solution onto the electrode.

4.3.3 Replace plastic sleeve over fill hole on the electrode.

4.4 For information about the electrode or for troubleshooting directions, see the

Instruction Manual.

Title: V-to-G Conversion Filters (AgF Pads) SOP Number: CDP COBRATF 6.15.6 Prepared By: Chemical Agent Lab Quality Review: Chemical Hygiene Review:

Revision: 6 6.15 Page 1 of 6 Effective Date: 2/28/11

To prepare, test, and assemble V-to-G Conversion Filters and record required data in the Chemical Agent Laboratory of the Center for Domestic Preparedness (CDP) Chemical, Ordnance, Biological, and Radiological Training Facility (COBRATF).

Chemical Agent Laboratory Personnel, Air Monitoring Personnel, Hot Trash/Hot Laundry Personnel

3.1 Chemical Systems Laboratory Contractor Report ARC5L-CR-82052, Depot Area Air Monitoring System (DAAMS) and VX Study, Southern Research Institute, Nov. 1982

3.2 CDP COBRATF Form 4.18.EY, Silver Fluoride Conversion Sheet, Preparation and

Acceptance Test Data Form

3.3 CDP COBRATF Form 4.18.ET, Certificate of Compliance

4.1 Assemble required equipment/supplies needed for preparation.

4.2 Major Equipment and Supplies:

4.2.1 Preparation:

a. Desiccating Material

b. Ethanol, absolute

c. Potassium Fluoride

d. Silver Nitrate

e. Polyester Material

f. Analytical Balance

g. Oven

h. Magnetic Stirrer and 2 magnetic stirring bars

i. Disposable Beaker

j. Aspirating Flask or Filtration Flask

k. Filter paper #2, if needed

l. Tray, polypropylene

m. Forceps or Tweezers

n. Deionized/Distilled Water

Revision: 6 6.15 Page 2 of 6 Effective Date: 2/28/11

4.2.2 Assembly/Sampling:

a. Punching block

b. Polyester material with AgF

c. Mallet

d. Polypropylene or teflon union

e. Punch (appropriate size)

NOTE 1: CAUTION, the silver salts used in this procedure will stain skin and clothing. Avoid direct skin contact with these substances. Use gloves.

NOTE 2: The quantities of silver nitrate solution, potassium fluoride solution, and resulting silver fluoride solution may be adjusted to the number of pads to be treated.

NOTE 3: Be sure to always wear gloves during the preparation and handling of silver fluoride pads to protect the skin from irritation due to chemical contact.

4.3 Complete CDP COBRATF Form 4.18.EY while preparing, sampling and testing Silver Fluoride (AgF) Pads.

4.3.1 Preheat the oven to approximately 50ºC.

4.4 Prepare Silver Nitrate (AgNO₃) Solution

4.4.1 Use the balance to weigh 37.50g +/-0.05 of AgNO₃.

4.4.2 Place the weighed amount of AgNO₃ in a labeled beaker and add 80 mL of distilled or deionized water.

4.4.3 Place a magnetic bar in the beaker, place the beaker on a magnetic stirrer, and stir until all salt is dissolved.

4.4.4 Record data.

4.5 Prepare Potassium Fluoride

4.5.1 Use the balance to weigh 12.50g +/-0.05g of KF 2H₂O.

4.5.2 Place…