MIL-STD-282.pdf

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MIL---STD---282B

22 December 2015

SUPERSEDING

(See 6.5)

DEPARTMENT OF DEFENSE

TEST METHOD STANDARD

FILTER UNITS, PROTECTIVE CLOTHING, GAS---MASK

COMPONENTS AND RELATED PRODUCTS:

PERFORMANCE TEST METHODS

AMSC N/A FSC 4240

DISTRIBUTION STATEMENT C. Distribution authorized to U.S. Government Agencies and their contractors; ExportControlled andCritical Technology; 18Dec2015.Other requests should be referred to: U.S. Army Edgewood Chemical Biological Center, ATTN: RDCB--- DEL---S, 5183 Blackhawk Road, Aberdeen Proving Ground, MD 21010---5424.

MIL---STD---282B

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FOREWORD

1. This standard is approved for use by all Departments and Agencies of the Department of Defense (DoD) within the distribution limitations noted at the bottom of the cover.

2. This standard covers methods used in the routine testing and inspection of filter units, protective clothing, gas mask components and related products.

3. Comments, suggestions, or questions on this document should be addressed to: U.S.

Army Edgewood Chemical Biological Center, ATTN: RDCB---DEL---S, 5183 Blackhawk Road, Aberdeen Proving Ground, MD 21010---5424 or emailed to USArmy.APG.ECBC.List.Specs-Team@mail.mil. Since contact information can change, you may want to verify the currency of this address information using the ASSIST Online database at https://assist.dla.mil.

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SUMMARY OF MODIFICATIONS

1. Updated the identification of changes paragraph of the standard to identify that the presence of vertical lines indicate where changes have been made throughout the standard.

2. For consistency throughout the Test Methods, chemical warfare agents were first introduced as Mustard (HD), Sarin (GB), Soman (GD) and Thickened Soman (TGD), then HD, GB, GD and TGD were used thereafter throughout the test methods, respectively.

3. The following modifications to MIL---STD---282 revision A with change 1 have been made:

Paragraph Modification Distribution statement Changed Warning statement Changed

2.2.1 Changed

6.5 Added

3.1 of Method 204.1.3 Changed

4.1.1 of Method 204.1.3 Changed

4.1.3 of Method 204.1.3 Changed

4.2 of Method 204.1.3 Changed

4.3.2 of Method 204.1.3 Changed

5.1 of Method 204.1.3 Changed

5.2 of Method 204.1.3 Changed

6.1.1 of Method 204.1.3 Renumbered

6.1.2 of Method 204.1.3 Deleted

3.1 of Method 209.1.2 Changed

3.1.1 of Method 209.1.2 Changed

3.2 of Method 209.1.2 Changed

4.1 of Method 209.1.2 Changed

4.2 of Method 209.1.2 Changed

4.2.1 of Method 209.1.2 Changed

4.2.2 of Method 209.1.2 Changed

4.2.3 of Method 209.1.2 Changed

5.1 of Method 209.1.2 Changed

5.2.1 of Method 209.1.2 Changed

5.2.2 of Method 209.1.2 Changed

5.3.1 of Method 209.1.2 Changed, renumbered

5.3.2 of Method 209.1.2 Deleted

3.1 of Method 205.1.1 Changed

4.2 of Method 205.1.1 Changed

4.3.2 of Method 205.1.1 Changed

5.1 of Method 205.1.1 Changed iv

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5.2 of Method 205.1.1 Changed

6.1.1 of Method 205.1.1 Changed, renumbered

6.1.2 of Method 205.1.1 Deleted

4.3 of Method 206.1.5 Changed

5.3 of Method 206.1.5 Changed

5.4 of Method 206.1.5 Changed

3.1 of Method 208.1.2 Changed

3.1.1 of Method 208.1.2 Changed

3.2 of Method 208.1.2 Changed

4.1 of Method 208.1.2 Changed

4.2 of Method 208.1.2 Changed

4.2.1 of Method 208.1.2 Changed

4.2.2 of Method 208.1.2 Changed

4.2.3 of Method 208.1.2 Changed

5.2.1 of Method 208.1.2 Changed

5.3.1 of Method 208.1.2 Changed, renumbered

5.3.2 of Method 208.1.2 Deleted v

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CONTENTS

PARAGRAPH PAGE

FOREWORD ii

1. SCOPE 1

1.1 Purpose 1

1.2 Numbering system 1

1.2.1 Decimal point significance 1

1.2.2 Group numbers assignment 1

2. APPLICABLE DOCUMENTS 1

2.1 General 1

2.2 Government documents 2

2.2.1 Specifications, standards, and handbooks 2

2.2.2 Other Government documents, drawings, and publications 2

2.3 Order of precedence 2

3. DEFINITIONS 2

4. GENERAL REQUIREMENTS 2

4.1 Test requirements 2

5. DETAILED REQUIREMENTS 2

6. NOTES 3

6.1 Intended use 3

6.2 Acquisition requirements 3

6.3 Subject term (key word) listing 3

6.4 Change notations 3

6.5 Supersession Data 3

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TEST METHODS

METHOD PAGE

105.11.1 Rough handling of particulate filters, adsorbent units, collective protectors, and similar items 4

204.1.3 Mustard (HD) resistance of impermeable materials

(static---diffusion method) 7

209.1.2 Mustard (HD) resistance of impermeable materials

(static---diffusion method) 13

205.1.1 VX resistance of impermeable materials

(static---diffusion method) 17

206.1.5 Sarin (GB), Soman (GD) and Thickened Soman (TGD) resistance of impermeable materials (static---diffusion method) 21

208.1.2 Sarin (GB) resistance of impermeable materials

(static---diffusion method) 26

FIGURES

FIGURE PAGE

1. Rough handling apparatus 6

2. Static---diffusion apparatus 11

3. Specimen arrangement, static---diffusion test 12

4. Arrangement for static---diffusion test 25

FOR OFFICIAL USE ONLY

1. SCOPE

1.1 Purpose. This standard covers methods used in the routine testing and inspection of filter units, protective clothing, gas mask components and related products.

1.2 Numbering system. Test methods covered by this standard are numbered in accordance with the following systems:

1.2.1 Decimal point significance. Test methods are assigned consecutive numbers within the ap-propriate group. Group numbers are assigned as shown in 1.2.2. The numbers 1 to 99 in each group are assigned to the different types of tests.When the same type of test is used in a different group, the numbers in the 1 to 99 group remain the same. The numbers to the right of the first decimal point designate the different items or units being tested within the test group. Numbers to the right of the second decimal point designate the number of revisions.

:---Group : :---Type of test : : :---Item of unit tested : : : :---Revision 0 0 0. 0. 0

1.2.2 Group numbers assignment. Group numbers are assigned as follows:

Group 1 --- Test Methods 100 to 199 are assigned to filter units and related products’ test pro-cedures.

Group 2 --- TestMethods 200 to 299 are assigned to impermeable protective clothing test pro-cedures.

Group 3 --- Test Methods 300 to 399 are assigned to permeable clothing test procedures.

Group 4 --- Test Methods 400 to 499 are assigned to gas---mask facepieces.

Group 5 --- Test Methods 500 to 599 are assigned to gas---mask canisters.

Group 6 --- Test Methods 600 to 699 are assigned to general test methods and other miscella-neous methods.

2. APPLICABLE DOCUMENTS

2.1 General. The documents listed in this section are specified in sections 3, 4, or 5 of this standard. This section does not include documents cited in other sections of this standard or recom-mended for additional information or as examples. While every effort has been made to ensure the completeness of this list, document users are cautioned that they must meet all specified require-ments of documents cited in sections 3, 4, or 5 of this standard, whether or not they are listed.

FOR OFFICIAL USE ONLY

2.2 Government documents.

2.2.1 Specifications, standards, and handbooks. The following specifications, standards, and handbooks form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those cited in the solicitation or contract.

DEPARTMENT OF DEFENSE SPECIFICATIONS

MIL---DTL---51408 --- Paper, Chemical Agent Detector, VGH, ABC---M8 MIL---DTL---51518 --- Paper, Chemical Agent Detector: M9 (SR119 Dye)

(Copies of these documents are available online at http://quicksearch.dla.mil)

2.2.2 Other Government documents, drawings, and publications. The following other Govern-ment documents, drawings, and publications form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are those cited in the solicitation or contract.

DEPARTMENT OF THE ARMY PAMPHLETS (DA PAM)

385---61 --- Toxic Chemical Agent Safety Standards

(Copies of this document are available online at http://www.apd.army.mil/AdminPubs/ Pubs_home.asp.)

2.3 Order of precedence. Unless otherwise noted herein or in the contract, in the event of a con-flict between the text of this document and the references cited herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained.

3. DEFINITIONS

This section is not applicable to this standard.

4. GENERAL REQUIREMENTS

4.1 Test requirements. The requirements that must be met by the items subjected to the test methods described herein are specified in the individual specifications. Whenever this standard con-flicts with the individual specification, the latter shall govern.

5. DETAILED REQUIREMENTS

This section is not applicable to this standard.

6. NOTES

(This section contains information of a general or explanatory nature that may be helpful, but is not mandatory.)

FOR OFFICIAL USE ONLY

6.1 Intended use. The test methods covered by this standard are intended for routine testing and inspection of filter units, protective clothing, gas mask components and related products.

6.2 Acquisition requirements. Acquisition documents should specify the following:

(a) Title, number, and date of this standard.

6.3 Subject term (key word) listing.

GB

GD

HD

TGD

VX

6.4 Change notations. The margins of this standard are marked with vertical lines to indicate modifications generated by this change. This was done as a convenience only and the Government assumes no liability whatsoever for any inaccuracies in these notations. Bidders and contractors are cautioned to evaluate the requirements of this document based on the entire content irrespective of the marginal notations.

6.5 Supersession data. This document supersedes MIL---STD---282 revision A with change 1 dated 24 September 2012.

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METHOD 105.11.1

ROUGH HANDLING OF PARTICULATE FILTERS, ADSORBENT UNITS, COLLECTIVE

PROTECTORS, AND SIMILAR ITEMS

The application of this test method will not be restricted to one particular apparatus.

1. SCOPE

1.1 This test method is intended for use in subjecting particulate filters, gas filters and similar items to the rough handling required by applicable specifications.

2. APPARATUS

2.1 The apparatus shall consist of a platen assembly which is capable of imparting mechanical shocks to items which are securely anchored directly to it. This platen shall be fitted withmechanical restraining devices to ensure that the mounted items are securely anchored and will not shift (in a lateral sense) from their original mounting location during the conduct of the rough handling event.

The restraining devices shall be robust enough to ensure that the mounted test articles remain in direct contact with the top surface of the platen throughout the duration of the rough handling event.

This platen shall measure 30 by 30 inches and have a total weight of 240 ± 20 pounds including the restraining devices and associated hardware.

2.2 The platen described in 2.1 shall be a component of the apparatus, and shall be ruggedized to withstand severe mechanical shocks. The filter contact surface may be constructed of aluminum or magnesium to preclude filter damage and to ensure the platen assembly remains within the weight requirements of 2.1. Any wear surface (i.e. cam followers and strike plate contact areas) shall be constructed of steel. The rough handling apparatus shall be anchored to a concrete floor suitable to absorb the necessary impacts of the vertically directed mechanical shocks.

3. PROCEDURE

3.1 Position and clamp the filter on the platen in accordance with the applicable end item specifi-cation and or test procedure so that there shall be no distortion to the frame or body of the filter when it is securely clamped in place.

3.2 The platen and filter shall be raised and let fall (free) by gravity 3/4+--- 1/8 inch, unless other-wise directed in the specification on the filter under test, onto the steel base---plate at the rate of 200 +--- 20 drops per minute for 15+--- 0.1 minutes.

3.3 The test shall be performed at a room temperature of 70_+--- 25_F.

4. NOTES

4.1 Approved safety procedures shall be observed while performing tests.

4.2 Throughout the test the filter shall remain in a firm position.

METHOD 105.11.1

FOR OFFICIAL USE ONLY

4.3 Filters may be padded or blocked where clamps press against the side or top of the frame, but not the bottom, to prevent distortion of the filters.

4.4 The platenmust be parallel to the base---plate at all times (thereby eliminating any horizontal movement and or force).

4.5 A rough handling apparatus capable of meeting these requirements is located at Edgewood Chemical Biological Center (see Figure 1). For more information on this rough handling apparatus contact: U.S. Army Edgewood Chemical Biological Center, ATTN: RDCB---DET---T, 5183 Black-hawk Road, Aberdeen Proving Ground, MD 21010---5424.

FOR OFFICIAL USE ONLY

FIGURE 1. Rough handling apparatus.

FOR OFFICIAL USE ONLY

METHOD 204.1.3

MUSTARD (HD) RESISTANCE OF IMPERMEABLE MATERIALS

(STATIC---DIFFUSION METHOD)

1. SCOPE

1.1 This method describes a static diffusionmethod for determining the mustard (HD) resistance of impermeable materials. HD resistance, when measured by this method, is the time for sufficient HD to pass through the material, vaporize, and cause a “vapor break” as indicated on the indicator paper. It is not measuring the time for the liquid film to pass through the material.

2. OUTLINE OF METHOD

2.1 The test is conducted by placing a specified quantity of liquid HD on the top surface of the material, which rests on standard Congo red indicator paper. WhenHD permeates the test material, it evaporates and the vapors react with S---328 (tetrachloro---7, 8---diphenylglycoluril) that has been spotted on the paper, producing hydrogen chloride (HCl) that reacts with the impregnant Congo red, changing it to a blue color. The time required for sufficient HD to pass through the test material and effect the color change in the indicator paper is the HD resistance of the material.

3. APPARATUS

3.1 The apparatus, Q170 (see Figure 2), used is an oven thermostatted at 37_+--- 0.5_C, containing a heater, circulating fan or fans, charcoal filter bed, drawers to hold glass trays of test specimens, and mirrors to view the undersides of the specimen trays. The specimen trays are made of glass plates that permit seeing the detector paper under the mounted specimens when viewed through the mir-ror, which is mounted at an appropriate angle underneath the trays. A clear window in the front wall of the oven allows the mirror to be seen. The drawers can be pulled part way out or completely re-moved to allow the trays of specimens to be placed on the drawers. The bottoms of the drawers are open so that the specimens can be seen through the glass trays. If the drawers are to be removed, dummy fronts can be inserted into the openings to maintain the internal temperature. The dimen-sions of the oven and the number of drawers can be tailored to fit the available hood space. The heat-er and thermostat are designed tomaintain the internal temperature at 37_+--- 0.5_C, with a relatively fast rise without overshooting the required temperature. The fan, or fans, circulate the air under the trays, through an opening at the end of the trays, across the top of the trays, and through a charcoal filter to the underside. The air circulation is required to maintain a uniform temperature, but the velocity is low enough not to disturb the specimens on the trays. The charcoal filter serves to adsorb any HD vapor that might escape from the specimens. The filter is made of loose charcoal spread in a tray whose bottom is made of wire screen; a cloth scrimmay be laid in the tray to prevent fines from passing through. The walls of the apparatus should be insulated to prevent heat loss.

4. PREPARATION FOR TEST

4.1 Indicator paper (see 7.3).

METHOD 204.1.3

FOR OFFICIAL USE ONLY

4.1.1 S---328 solution. Mix 0.5+--- 0.075 gm of S---328 (tetrachloro---7, 8---diphenylglycoluril) and 0.1+0.015 gm/---0 gm of anhydrous sodium or potassium carbonate with 10 mL of 1,1,2,2---tetrachlo-roethane. Shake the mixture thoroughly and filter through aWhatman No. 42 filter paper or equiva-lent. Pour the clear filtrate into a small actinic glass bottle. The bottle should be kept closed at all times when not in use. A fresh solution should be prepared weekly.

4.1.2 Impregnating. Dip 4.25---cm circles of qualitative filter paper, intended for coarse and ge-latinous or for medium precipitates, into approximately 0.1 percent solution of Congo red in distilled water. When the paper is thoroughly impregnated, allow to air dry. The treated paper may be kept indefinitely but must be prepared and stored in an acid---free and HD---free atmosphere.

4.1.3 Spotting. Spot the impregnated paper with the S---328 solution as follows: Dip a cotton swab or similar tool into the S---328 solution and then touch the swab to the Congo red impregnated paper.

Make one spot at the center of the paper and four others about it at a distance of approximately 1/4---inch. Let the spots dry. The spotted paper is defective after 24 hours and should be used prefer-ably before 12 hours have elapsed. If the test specimen runs more than 24 hours, the indicator paper should be changed at the end of the 24---hour period. Examine the dried spots before use; if a discol-oration, even a faint one, appears, it is likely the S---328 solution is defective and should be re---made before continuing with the test.

4.2 Apparatus. Turn on the fan and temperature controller. The temperature must be main-tained at 37_+--- 0.5_C, measured with a calibrated thermometer/thermocouple on the glass plate on which the specimens are placed. To simulate total mass that must be maintained at this temperature during the test, lay two glass plates in each tray, one to represent the cover glasses, and adjust the controller settings until the temperature can be maintained. These settings should be adequate for the duration of the test, but the temperature must be verified and recorded at the end of the test. If the apparatus is used on a daily basis, it is best to leave the power on at all times to maintain the temperature. If a temperature other than 37_+--- 0.5_C is indicated bring to the correct temperature by adjusting the controller. If a variable temperature is found in the apparatus check the temperature regulating system for defects.

4.3 Test specimens.

4.3.1 Cutting specimens. Cut the required number of disks or swatches from the material to be tested. The specimens should be slightly larger than the rings used to mount them (see 4.3.2).

4.3.2 Mounting specimens. Place the specimens on a smooth, flat surface. Attach a ring that is impervious to HD, has an inside diameter of 3/4 to 1 inch and is approximately 1/4 inch high to the specimen and press firmly until it is securely set, providing an airtight seal between specimen and ring. A suitablemethod is as follows:Melt equal parts beeswax and crystalline paraffin wax. Immerse felt rings into the melt until the rings are saturated with wax. Remove a ring from themelt with tongs, allow excess liquid wax to drain, and place the ring on the specimen. Place a weight on the ring to hold it in place until the wax cools and the ring is firmly attached to the specimen. Do not allow any wax to coat the specimen inside the ring.

FOR OFFICIAL USE ONLY

5. PROCEDURE

5.1 Preconditioning of specimens. Place disks of indicator paper on a glass plate. Place the mounted specimens on the indicator---paper disks, with the specimen contacting the paper. Place the glass plate, with specimens and indicator paper into a clean oven at 37_+--- 0.5_C for enough time to allow them to attain 37_+--- 0.5_C. Also place glass cover plates into the oven for preconditioning at 37_+--- 0.5_C.

5.2 Testing. Set the preconditioned glass plate and specimens on a platform heated to 37_+---0.5_C in front of the testing apparatus. Using a suitable dropper, place 0.150+---0.0225 gm of liquid HD of at least 95 percent purity on each specimen, inside the attached ring. The purity of agent shall be determined within one year of the test date. Cover each specimenwith a glass cover plate (see Figure 3). Open the drawer, place the glass plate on the drawer support and push in the drawer. Observe the indicator paper by means of the mirror inside the apparatus; a portable light may be used to illumi-nate the indicator paper. The end of the test occurs when the first visible blue color appears where the paper was spotted or at the end of the time period specified by the customer or material specifica-tion, whichever occurs first. If the blue color first appears at the outer edge of the spots and moves inward, suspect a false break (see 6.2) from vapors inside the apparatus instead of from agent per-meation through the specimen. Record the time interval between the instant the HD is placed on the specimen and the first visible appearance of blue on the spotted portion of the indicator paper. This time interval is termed the HD resistance of the material.

5.3 Decontamination. After the test is completed, clean the equipment for reuse by following standing operating procedures that are in effect at the facility performing the testing. It is necessary that all reusable items, such as glass plates and cover slips, be decontaminated and cleaned to the extent that there is no residual HD that might affect personnel or the indicator paper used in subse-quent testing.

6. QUALITY CONTROL

6.1 Standard reference material (SRM). For each type of material test using this method, an SRM should be made available for the laboratory to use as a means of quality control for within day and between day variation. The SRM should simulate the sample material to be tested as closely as possible with respect to formulation and ideally break after the sample material. Each lot of an SRM should have a volume that is large enough to allow all of the following: the laboratory to test SRM samples on successive days to establish a data base; the development of a statistical quality control chart with control limits; and, thereafter, to test the SRM during each test of sample materials. A minimum of two SRM samples should be tested each time and the results plotted on control charts with established quality control limits. If these limits are breached, sample data should be considered invalid and the test repeated after the cause of excess variation is identified, corrected and docu-mented; a contingency plan for such situations should be documented andmade available for labora-tory personnel conducting the test. These procedures apply only to thosematerials for which an SRM is available.

6.2 Negative control samples. In addition to the SRM, run the following negative control samples concurrently with each set of determinations. One negative control shall be S---328 impregnated

METHOD 204.1.3METHOD 204.1.3

FOR OFFICIAL USE ONLY

Congo red indicator paper exposed to the test system atmosphere, without HD being added. The purpose of this negative control is to determine if any vapor contamination exists within the test sys-tem atmosphere. The second negative control to run (if material for it is available) shall be a mounted sample with S---328 impregnated Congo red indicator paper carried through the entire test, without HD being added. The purpose of this negative control is to determine if any chemicals ema-nate from the samplematerial during the test, causing a positive reactionwith the S---328 and turning the indicator paper blue, thus, resulting in a false positive.

7. NOTES

7.1 HD produces severe blister action in both the liquid and vapor phases. All HD containers should be kept in a well ventilated hood when not in use. Great care should be exercised to prevent either the liquid HD or its vapor from coming in contact with the body.

7.2 Personnel should wear butyl rubber gloves in all operations involving the handling of HD. The glove protocol in effect for the standing operating procedures being used should be strictly observed.

7.3 If the material tested contains a compound that reacts with S---328, a false end point is ob-tained. Protective dubbing is an example of such a material. Thus, leather impregnites, such as dub-bing, cannot be tested for HD resistance using S---328---spotted Congo red paper and watching for the blue spots to appear. The HD resistance of materials such as dubbing impregnated leather may be measured by using DB---3 indicator paper (see MIL---D---50028) in place of the S---328---spotted Congo red paper.

7.4 If the services of a contracted commercial laboratory are to be procured for performance of this testmethod, certification of such laboratory must be initiated andmaintained by the government during the contractual period. As a source of technical expertise regarding this test method, the gov-ernment certifying body is to utilize the services of the government laboratory responsible for the routine performance of this test method for production acceptance testing purposes. The govern-ment laboratory is to provide the contract laboratory the current standing operating procedures for conduct of this test method, necessary apparatus, SRM, if available, and supplies of necessary re-agent solutions andmaterials. If SRMs are available, the government laboratory is to test and evalu-ate the proficiency of the contract laboratory to conduct this test method before contract work starts and periodically during the contract. Contract work is not to be performed unless the contractor can demonstrate quality control in the laboratory using SRMs and proficiency in the performance of this test method.

FOR OFFICIAL USE ONLY

A. Heating element

B. Fans

C. Bed of Charcoal

D. Thermoregulator

E. Mirror

F. Drawers (each holds 20 samples)

G. Window

FIGURE 2. Static---diffusion apparatus.

FOR OFFICIAL USE ONLY

FIGURE 3. Specimen arrangement, static---diffusion test.

FOR OFFICIAL USE ONLY

METHOD 209.1.2

MUSTARD (HD) RESISTANCE OF IMPERMEABLE MATERIALS

(STATIC---DIFFUSION METHOD)

This test method is in addition to Test Method 204.1 MUSTARD (HD) RESISTANCE OF

IMPERMEABLE MATERIALS (STATIC---DIFFUSION METHOD).

The application of this test method will not be restricted to one particular apparatus.

1. SCOPE

1.1 This method describes a static diffusion method for determining the HD resistance of im-permeable materials as required by applicable specifications.

2. PRECAUTIONS

2.1 Since HD is extremely toxic in both the liquid and vapor phases, tests using this agent shall be conducted only in testing facilities meeting safety requirements for the handling of HD as presented in DA PAM 385---61.

3. APPARATUS

3.1 The apparatus shall consist of a suitable container that provides an air chamber above and below a horizontal sample. The upper chamber shall be small enough to preclude significant evapo-ration. Ports shall be provided that allow room air to be drawn across the underside of the sample.

To analyze the effluent for chemical agents, the apparatus shall contain one of the effluent sampling systems in 3.1.1. The analyzer shall be capable of measuring a permeation ratio of at least 0.5 micro-grams per centimeter squared per minute.

3.1.1 Effluent sampling systems to quantify agent in the microgram to milligram range consist of:

3.1.1.1 Bubbler Method. This method uses a glass bubbler containing a known amount of solvent as the cumulative sampler. To determine the amount of HD collected in the bubbler a gas chromato-graph (GC) or autoanalyzer is used.

3.1.2 Effluent sampling systems to quantify agent in the nanogram to microgram range consist of:

3.1.2.1 Solid Sorbent Tube Method. This method uses solid sorbent tubes as the cumulative sam-pler. These tubes are either metal (stainless steel preferred) or glass that contain a small quantity of a solid sorbent (see 6.1). A GC is used to determine the amount of HD collected in the solid sorbent tubes.

3.1.2.2 Stream Selection System. This method pulls a sample directly into the detection device by the use of a stream selection system as a continuous sampler. The stream selection system is a series of heat trace lines constructed of flexible tubing connected to a sampling port. The sampling port is

METHOD 209.1.2

FOR OFFICIAL USE ONLY

connected to a vacuum manifold through a mass flow controller or critical orifice which feeds into a GC that has beenmodified to provide a continuous stream of the test atmosphere (see 6.2). The GC contains a solid sorbent pre---concentrator tube (PCT) (see 6.3).

3.2 Calibration/standardization of apparatus. The laboratory must demonstrate that the instru-ment used to determine the effluent agent concentration is reliable over a dynamic range. This must be achieved by calibrating/standardizing the instrument with a series of calibration standards pre-pared over this range using a Chemical Agent Standard Analytical Reference Material (CASARM) sample of HDwith a purity value of 95 percent or greater. If a CASARM is not available, the highest available purity of HD shall be used at a verified concentration of 95% or higher established within one year of the test date. For information on obtaining a CASARMsample ofHD contact: U.S.Army Edgewood Chemical Biological Center, ATTN: RDCB---DPC---RS, 5183 Blackhawk Road, Aber-deen Proving Ground, MD 21010---5424. The laboratory shall construct at least a five---point stan-dard calibration curve of the concentration of agent versus the detector response. The linear response shall be 0.995 or better for HD. In instances HD does not provide a linear response for calibration, a calibration curve with six levels is required when a non---linear regression is used. The frequency of calibration/standardization shall be weekly while in operation unless the laboratory can demonstrate otherwise.

4. PROCEDURE

4.1 Place the test sample horizontally in the air chamber container. Without contacting the sam-ple, use a dropper to apply enough agent (0.5+---0.075 mLs) to cover a known area of at least 10 cm2 of the top surface of the sample with liquid HD of 95 percent or greater purity. The purity of agent shall be determined within one year of the test date. If testing multiple samples, ensure that the amount of HD applied is consistent for each of the samples. Draw air across the bottom of the sam-ple and continuously analyze the effluent for agent using the appropriate method in 4.2. Record the time at the moment agent is placed upon the sample and the time a cumulative amount of 4 micro-grams per centimeter squared is measured in the effluent or amount of agent present after the time specified in the military specification. The test shall be carried out at 22_+--- 2_C.

4.2 One of the following methods can be used to analyze the effluent agent concentration. As technology advances, the laboratory may develop an alternate method of detection. However, in these instances, this new methodology must be validated by the laboratory and approved for use by the customer.

4.2.1 Bubbler method. The bubbler contains a known volume of a collection solvent having good solubility in HD. During testing, air is drawn through the bubbler at a known flow rate. HD vapor in the air dissolves in the collection solvent, therefore, the collection efficiency of the bubbler solu-tion at the air flow rate and temperature used must be known to eliminate saturation of the bubbler solution. An aliquot of the collection solvent from the used bubbler is analyzed on the same day of collection to determine the amount of HD collected. Bubblers are sampled at prescribed periods throughout the test. At the completion of each prescribed sampling period, each bubbler must be replaced with a fresh bubbler.

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4.2.2 Solid sorbent tube method. This sampler is aspirated for a prescribed period of time at a known flow rate measured by a calibrated flow meter. The flow rate must be 0.5 L/min or less due to the low air permeability of the packed tube. Following the prescribed sampling period, the solid sorbent tube is replaced with a fresh tube and the sampled tube analyzed to determine the amount of the HD collected. The analysis is done by thermally desorbing into a GC or extracting the chemi-cal from the tube with an appropriate solvent and then injecting the extracted solution into a GC calibrated to measure HD.

4.2.3 Stream selection method. The air stream is sampled for a selected compound (HD) and a selected interval of time (typically 4 minutes) with the solid sorbent tube. The stream selection sys-tem cycles through a set number of ports taking approximately one sample per hour on any given swatch. Any chemical absorbed by the solid sorbent tube is then thermally desorbed into the GC for measurement of the amount of HD collected. The solid sorbent tube is automatically cycled between the collection and the thermal desorption.

5. QUALITY CONTROL

5.1 Stream selection system line verification. Laboratories using the stream selection method must demonstrate the integrity of the heat---traced lines on a weekly basis while in operation. This is accomplished by challenging each line with a challenge equivalent to the mid---point calibration standard, but made, preferably, from a solution prepared independent of the calibration standard.

The percent recovery is then calculated. Lines are acceptable for use if the recovery value is within 25 percent of the target value or within performance based control limits.

5.2 Continuing calibration verification (CCV).

5.2.1 Bubblers and solid sorbent tubes. Analyze a mid---point calibration standard (preferably prepared from a solution independent of the calibration standard) at the beginning, after every 20 samples and at the end of every run. Calculate the percent recovery for these standards. The percent recovery shall be 100 ± 20 percent or within performance based control limits. Samples that were analyzed between an acceptable and unacceptable CCV are considered invalid, and the test shall be repeated after the cause of the excess variation is identified, corrected, and documented.

5.2.2 Stream selection systems. Analyze a mid---point calibration standard (preferably from a second source) prior to, and at the end of operations, each day of testing. Calculate the percent re-covery for these standards. The percent recovery shall be 100 ± 20 percent or within performance based control limits. If the end of the day CCV standard falls outside the acceptance limits, re---chal-lenge the instrument. If this re---challenge falls outside the acceptance limits, the test is considered invalid and shall be repeated after the cause of the excess variation is identified, corrected, and docu-mented.

5.3 Standard reference material (SRM). For each type of material test using this method, an SRM should be made available for the laboratory to use as a means of quality control for within day and between day variations. The SRM should simulate the sample material to be tested as closely as possible with respect to formulation and ideally break after the sample materials. Each lot of an SRM should have a volume that is large enough to allow all the following: the laboratory to test SRM

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samples on successive days to establish a data base; the development of a statistical quality control chart with control limits; and, thereafter, the ability to test the SRMduring each test of samplemate-rials . Aminimumof two SRM samples should be tested each time and the results plotted on control charts with established quality control limits. If these limits are breached, sample data should be considered invalid and the test repeated after the cause of excess variation is identified, corrected and documented; a contingency plan for such situations should be documented and made available for laboratory personnel conducting the test. These procedures apply only to those materials for which an SRM is available. If an SRM is not available, the laboratory shall control chart the results for the CCV and take appropriate action as specified above.

5.4 Blank. Ablankmust be testedwith each sample batch, if additional material is available. The blank shall be a sample carried through the entire test without HD being added. The purpose of the blank is to determine if any chemicals emanate from the sample material during the test and cause a false positive.

6. NOTES

6.1 Tenax GC is a commercially available, proven solid sorbent, and has been shown to be ac-ceptable for use in the solid sorbent tube method.

6.2 AMiniature Chemical Agent Air Monitoring System (MINICAMS) is commercially avail-able, and has been shown to be an acceptable system for use in the stream selection method.

6.3 Tenax TA is a commercially available, proven solid PCT sorbent tube, and has been shown to be acceptable for use in the stream selection method.

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METHOD 205.1.1

VX RESISTANCE OF IMPERMEABLE MATERIALS

(STATIC---DIFFUSION METHOD)

1. SCOPE

1.1 This method describes a static diffusion method for determining the liquid VX resistance of impermeable materials. VX resistance, when measured by this method, is the time for sufficient liq-uid VX to pass through the material and cause a color change on the indicator paper.

2. OUTLINE OF METHOD

2.1 The test is conducted by placing a specified quantity of VX on the top surface of the material, which rests on standard ABC---M8 indicator paper in accordance with MIL---DTL---51408, or M9 indicator paper in accordance with MIL---DTL---51518. When VX permeates the test material, the liquid reacts with the dyes in the indicator paper changing it to a green (M8) or red (M9) color. The time required for sufficient VX to pass through the test material and effect the color change in the indicator paper is the VX resistance of the material.

3. APPARATUS

3.1 The apparatus, Q170 (see Figure 2), used is an oven thermostatted at 37_+--- 0.5_C, containing a heater, circulating fan or fans, charcoal filter bed, drawers to hold glass trays of test specimens, and mirrors to view the undersides of the specimen trays. The specimen trays are made of glass plates that permit viewing of the detector paper under the mounted specimens when viewed through the mirror, which is mounted at an appropriate angle underneath the trays. A clear window in the front wall of the oven allows the mirror to be seen. The drawers can be pulled part way out or completely removed to allow the trays of specimens to be placed on the drawers. The bottoms of the drawers are open so that the specimens can be seen through the glass trays. If the drawers are to be removed, dummy fronts can be inserted into the openings to maintain the internal temperature. The dimen-sions of the oven and the number of drawers can be tailored to fit the available hood space. The heat-er and thermostat are designed tomaintain the internal temperature at 37_+--- 0.5_C, with a relatively fast rise without overshooting the required temperature. The fan, or fans, circulate the air under the trays, through an opening at the end of the trays, across the top of the trays, and through a charcoal filter to the underside. The air circulation is required to maintain a uniform temperature, but the velocity is low enough not to disturb the specimens on the trays. The charcoal filter serves to adsorb any vapor that might escape from the specimens. The filter is made of loose charcoal spread in a tray whose bottom is made of wire screen; a cloth scrimmay be laid in the tray to prevent fines from pass-ing through. The walls of the apparatus should be insulated to prevent heat loss.

4. PREPARATION FOR TEST

4.1 Indicator paper. Cut M8 or M9 indicator paper to size for placement under the specimens to be tested.

METHOD 205.1.1

FOR OFFICIAL USE ONLY

4.2 Apparatus. Turn on the fan and temperature controller. The temperature must be main-tained at 37_+--- 0.5_C, measured using a calibrated thermometer/thermocouple on the glass plate on which the specimens are placed. To simulate total mass that must be maintained at this temperature during the test, lay two glass plates in each tray, one to represent the cover glasses, and adjust the controller settings until the temperature can be maintained. These settings should be adequate for the duration of the test, but the temperature must be verified and recorded at the end of the test. If the apparatus is used on a daily basis, it is best to leave the power on at all times to maintain the temperature. If a temperature other than 37_+--- 0.5_C is indicated bring to the correct temperature by adjusting the controller. If a variable temperature is found in the apparatus check the temperature regulating system for defects.

4.3 Test specimens.

4.3.1 Cutting specimens. Cut the required number of disks or swatches from the material to be tested. The specimens should be slightly larger than the rings used to mount them (see 4.3.2).

4.3.2 Mounting specimens. Place the specimens on a smooth, flat surface. Attach a ring that is impervious to VX, has an inside diameter of 3/4 to 1 inch and is approximately 1/4 inch high to the specimen and press firmly until it is securely set, providing an airtight seal between specimen and ring. A suitablemethod is as follows:Melt equal parts beeswax and crystalline paraffin wax. Immerse felt rings into the melt until the rings are saturated with wax. Remove a ring from themelt with tongs, allow excess liquid wax to drain, and place the ring on the specimen. Place a weight on the ring to hold it in place until the wax cools and the ring is firmly attached to the specimen. Do not allow any wax to coat the specimen inside the ring.

5. PROCEDURE

5.1 Preconditioning of specimens. Place disks of the indicator paper on a glass plate. Place the mounted specimens on the indicator---paper disks, with the specimen contacting the paper. Place the glass plate, with specimens and indicator paper into a clean oven at 37_+--- 0.5_C for enough time to allow them to attain 37_+--- 0.5_C. Also place glass cover plates into the oven for preconditioning at 37_+--- 0.5_C.

5.2 Testing. Set the preconditioned glass plate and specimens on a platform heated to 37_+--- 0.5_C in front of the testing apparatus. Using a suitable dropper, place 0.150+--- 0.0225 gm of liquid VX of at least 95 percent purity on each specimen, inside the attached ring. The purity of agent shall be determined within one year of the test date. Cover each specimenwith a glass cover plate (see Figure 3). Open the drawer, place the glass plate on the drawer support and push in the drawer. Observe the indicator paper by means of the mirror inside the apparatus; a portable light may be used to illumi-nate the indicator paper. The end of the test occurs when the first visible color appears where the paper was spotted or at the end of the time period specified by the customer or material specifica-tion, whichever occurs first. Note: VX causes a green color on M8 paper and a red color on M9 pa-per. Record the time interval between the instant the VX is placed on the specimen and the first visible appearance of green or red on the indicator paper. This time interval is termed the VX resis-tance of the material.

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5.3 Decontamination. After the test is completed, clean the equipment for reuse by following standing operating procedures that are in effect at the facility performing the testing. It is necessary that all reusable items, such as glass plates and cover slips, be decontaminated and cleaned to the extent that there is no residual VX that might affect personnel or the indicator paper used in subse-quent testing.

6. QUALITY CONTROL

6.1 Standard reference material (SRM). For each type of material test using this method, an SRM should be made available for the laboratory to use as a means of quality control for within day and between day variation. The SRM should simulate the sample material to be tested as closely as possible with respect to formulation and ideally break after the sample material. Each lot of an SRM should have a volume that is large enough to allow all of the following: the laboratory to test SRM samples on successive days to establish a data base; the development of a statistical quality control chart with control limits; and, thereafter, the ability to test the SRMduring each test of samplemate-rials. A minimum of two SRM samples should be tested each time and the results plotted on control charts with established quality control limits. If these limits are breached, sample data should be con-sidered invalid and the test repeated after the cause of excess variation is identified, corrected, and documented; a contingency plan for such situations should be documented and made available for laboratory personnel conducting the test. These procedures apply only to those materials for which an SRM is available.

6.2 Negative control samples. In addition to the SRM, run the following negative control sam-ples concurrently with each set of determinations. One negative control shall beM8 orM9 (indicator paper) exposed to the test system atmosphere, without VXbeing added. The purpose of this negative control is to determine if any vapor contamination exists within the test system atmosphere. The sec-ond negative control to run (if material for it is available) shall be a mounted sample with M8 or M9 indicator paper carried through the entire test, without VX being added. The purpose of this nega-tive control is to determine if any chemicals emanate from the sample material during the test, caus-ing a positive reaction with the M8 or M9 and turning the indicator paper green (M8) or red (M9), thus, resulting in a false positive.

7. NOTES

7.1 VX is a nerve agent of extremely low vapor pressure. All containers should be kept closed in a well ventilated hood when not in use. Great care must be exercised to prevent liquidVX from com-ing in contact with the body.

7.2 Personnel should wear butyl rubber gloves in all operations involving the handling of VX. The glove protocol in effect for the standing operating procedures being used should be strictly observed.

7.3 If the services of a contracted commercial laboratory are to be procured for performance of this testmethod, certification of such laboratory must be initiated andmaintained by the government during the contractual period. As a source of technical expertise regarding this test method, the gov-ernment certifying body is to utilize the services of the government laboratory responsible for the routine performance of this test method for production acceptance testing purposes. The govern-

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ment laboratory is to provide the contract laboratory the current standing operating procedures for conduct of this test method, necessary apparatus, SRM, if available, and supplies of necessary re-agent solutions andmaterials. If SRMs are available, the government laboratory is to test and evalu-ate the proficiency of the contract laboratory to conduct this test method before contract work starts and periodically during the contract. Contract work is not to be performed unless the contractor can demonstrate quality control in the laboratory using SRMs and proficiency in the performance of this test method.

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METHOD 206.1.5

SARIN (GB), SOMAN (GD) and THICKENED SOMAN (TGD) RESISTANCE OF

IMPERMEABLE MATERIALS

(STATIC---DIFFUSION METHOD)

1. SCOPE

1.1 This method describes a static diffusionmethod for determining the GB, GD and TGD vapor resistance of impermeable materials.

2. PRECAUTIONS

2.1 Since GB, GD and TGD are extremely toxic in both the liquid and vapor phases, tests using these agents shall be conducted only in testing facilities governed by safety regulations for the han-dling of GB, GD and TGD and the treatment of casualties produced by these substances.

3. OUTLINE OF METHOD

3.1 The test is conducted by placing approximately 0.1 gm of liquid agent (either GB, GD or TGD) on the top surface of the material to be tested. The disk is sealed between two glass cups and the bottom cup contains approximately 20 fruit flies (see 7.1). The time, in minutes, required for the agent to permeate the test material and cause paralysis or death of one---half of the flies is the agent vapor resistance of the material.

4. APPARATUS

4.1 Assembly. The assembly of the apparatus is shown in Figure 4.

4.2 Glass cups. The glass cups have ground---glass---faced flanges approximately 2---1/8 inches in diameter.

4.3 Test temperature. The test shall be conducted at 25_+--- 2_C, measured with a calibrated ther-mometer. Since the test apparatus is mounted in a fume hood, the room temperature must be main-tained at the specified test temperature. If the temperature cannot be controlled, a constant temperature box must be provided.

5. PROCEDURE

5.1 Preparation of test specimens. Die or cut the required number of disks from the sample, approximately 2---1/4 inches in diameter.

5.2 Mounting test specimens. Mount each test specimen between two glass cups as follows: Pre-heat required number of glass cups on a temperature controlled hot plate (100_ --- 105_C). Lay the specimen on a clean, hard, flat surface. Touch the heated ground---glass---face of a cup flange to the surface of a wax application tray consisting of equal parts of beeswax and crystalline paraffin wax, so that the ground---glass---face is covered with wax. Press cup to specimen surface and allow wax to

METHOD 206.1.5

FOR OFFICIAL USE ONLY

harden. Invert cup; repeat the waxing procedure with the…