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National Institute for Occupational Safety and Health

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National Personal Protective Technology Laboratory

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P.O. Box 18070

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Pittsburgh, PA 15236

r o o p y Revision: 1.1 Date: 21 December 2005

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Procedure No. CET-APRS-STP-CBRN-0403

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DETERMINATION OF CBRN ACID GASES (HYDROGEN CYANIDE)

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SERVICE-LIFE TEST, AIR-PURIFYING ESCAPE RESPIRATORS

o STANDARD TEST PROCEDURE (STP)

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1. PURPOSE

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This test establishes the procedure for ensuring that the level of protection provided by

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the CBRN Acid Gases (Hydrogen cyanide) Service Life Test, Air Purifying Escape

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Respirators Standard Test Procedure submitted for Approval, Extension of Approval, or

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examined during Certified Product Audits, meet the minimum certification standards set

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forth in 42 CFR Part 84, Subpart G, 84.63(a)(c)(d); Volume 60, Number 110, June 8,

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1995 and the Statement of Standard for Chemical, Biological, Radiological, and Nuclear

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(CBRN) Air Purifying Escape Respirator, Dated September 30, 2003.

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2.
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GENERAL

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This STP describes the Determination of CBRN Acid Gases (Hydrogen Cyanide) Service

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Life Test, Air-Purifying Escape Respirators Standard Test Procedure test in sufficient

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detail that a person knowledgeable in the appropriate technical field can select equipment

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with the necessary resolution, conduct the test, and determine whether or not the product

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passes the test.

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3.
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EQUIPMENT/MATERIAL

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The list of necessary test equipment and materials follows:

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3.1.1. Miller Nelson Research Model 401 Flow-Temperature-Humidity Control

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System or equivalent. This system is an automated system to control the

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airflow, temperature, and humidity of an air supply for an operating

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system. Laboratory air and distilled water are supplied to the unit. The unit

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output is air of the variable volume/flow dependant on the size of unit

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(10% of max flow to max flow in liters per minute (Lpm) ± 2%), and

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relative humidity (10%–98% ± 3%) and temperature (20ºC–30º 0C ±

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0.3%).

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Approvals: 1st Level 2nd Level 3rd Level

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Procedure No. CET-APRS-STP-CBRN-0403
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3.1.2. EdgeTech Dew Prime II Hygrometer, Model 2000 or equivalent. A

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micro- processor based programmable dew point instrument. The
hygrometer uses the dew point and ambient temperature to calculate the

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relative humidity. Dew point and ambient temperature range is: -50 to 130

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C ± 0.2 o C; relative humidity is 1 to 95 %± 0.5%.

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3.1.3. Labview software developed for NIOSH Service Life Testing.

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3.1.4. California Analytical Instruments, Model 1314 Photoacoustic Multigas

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Monitor with UA0980 optical filter or equivalent.

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3.1.5. Gas Chromatograph, Shimadzu, Model 14A with Flame Ionization
Detectors or equivalent.

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3.1.6. Mass Flow Controller, Brooks Instruments, Variable flow rate depending

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on use.

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3.1.7. Read out and Control Electronics, Brooks Instruments, Model 0154,

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Power supply and controller for the Brooks Mass Flow Controller.

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3.1.8. Dry Test Meter, American Meter Company, Model and size depending on

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air flow to be measured.

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3.1.9. Certified cylinders of 10 ppm, 500 ppm and 1000 ppm hydrogen cyanide,

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balance gas Nitrogen.

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3.1.10. Hydrogen cyanide permeation tube.

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3.1.11. Cyanogen permeation tube.

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3.1.12. Hydrogen Cyanide cylinders, 2% hydrogen cyanide, balance gas of

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c o helium.
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3.1
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Test fixture for mounting canisters.

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3.3
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The test chamber consisting of a 12" x 11½" x 7" air tight metal box with door

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opening lined with gasket material. Two ½" bulkhead Swaglok® fitting located

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on the backside of the test chamber for the introduction of the test concentration

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and for the exit of the test fixture. This fixture is not commercially available.

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3.4
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Resistance tester consisting of a vacuum source capable of delivering 85 Lpm, a

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6-inch water column slant manometer or electronic manometer and connections

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appropriate for items being tested. See description in RCT-APR-003 and RCT-
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APR-007.
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4.
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TESTING REQUIREMENTS AND CONDITIONS

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4.1. This test procedure is only valid if the respirator system has first completed

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NIOSH Standard Test Procedure entitled Determination Of Durability Test For

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Environmental And Transportation Conditions And Rough Handling Drop Test

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On Chemical Biological Radiological Nuclear (CBRN) Air-Purifying Escape
Respirators Standard Test Procedure (STP).

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c o 4.2. Prior to beginning any testing, all measuring equipment to be used must have

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been calibrated in accordance with the manufacturer's calibration procedure and

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schedule. At a minimum, all measuring equipment utilized for this testing must

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have been calibrated within the preceding 12 months using a method traceable to

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the National Institute of Standards and Technology (NIST).

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Any laboratory using this procedure to supply certification test data to NIOSH

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will be subject to the provisions of the NIOSH Supplier Qualification Program

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(SQP). This program is based on the tenets of ISO/IEC 17025, the NIOSH Manual

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of Analytical Methods and other NIOSH guidelines. An initial complete quality

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system audit and follow on audits are requirements of the program. Additional

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details of the Program and its requirements can be obtained directly from the

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institute.

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4.4 Precision and accuracy (P&A) must be determined for each instrument in

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accordance with laboratory procedures and NIOSH/NPPTL guidance. Sound

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practice requires, under NIOSH Manual of Analytical Methods, demonstrating a

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tolerance range of expected data performance of a plus or minus 25% of a 95%

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confidence interval of the stated standard requirement. NIOSH/NPPTL P&A

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tolerance can be higher but not lower.

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4.5
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Compressed gas cylinders must meet all applicable Department of Transportation

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requirements for cylinder approval as well as retesting / requalification.

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4.6
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Normal laboratory safety practices must be observed. This includes safety

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precautions described in the current NIOSH Pittsburgh Health and Safety

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Program.

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Safety glasses, lab coats, and hard-toe shoes must be worn at all times.

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4.6.2. Work benches must be maintained free of clutter and non-essential test

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equipment.

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4.6.3 When handling any broken glass laboratory equipment, lab technicians
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and personnel must wear special gloves, which protect against lacerations
Procedure No. CET-APRS-STP-CBRN-0403
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or punctures.

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Please refer to Material Safety Data Sheets and the NIOSH Health and

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Safety Manual for the proper protection and care in handling, storing, and

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disposing of the chemicals and gases used in this procedure.

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5. PROCEDURE

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Note: Reference Section 3 for equipment, model numbers and manufacturers. For

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calibration purposes use those described in the manufacturer's operation and

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maintenance manuals.

5.1.
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Follow individual instruction manuals for set up and maintenance of equipment

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used in this procedure prior to beginning testing. Malfunctioning equipment must

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be repaired or replaced and properly set up and calibrated before starting all tests.

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5.2.
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Calibrate photoacoustic monitor for hydrogen cyanide using a certified hydrogen

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cyanide gas cylinder. For the general category standard the monitor is calibrated

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for the challenge concentration of 470 ppm. For the specific category standard the

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monitor is calibrated for the challenge concentration of 940 ppm.

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5.3 After the manufacturer's specified warm-up period, calibrate the Gas

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Chromatograph using the Kin-Tek gas generator with the hydrogen cyanogen and

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cyanogen permeation tube.

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5.4 Start automatic sampling mode on the gas chromatograph. Monitor and record the

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upstream and downstream concentrations.

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Set up test equipment as shown in Figure 1. The humidity reading controlled by

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the Miller Nelson system and monitored the Dew Point Hygrometer. The sample

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pickup for the hygrometer is place into the air stream via a tee after the Miller

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Nelson and before the introduction point of challenge agent. The thermocouple

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for the hygrometer is placed in the challenge gas stream immediately before the
test chamber.

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5.6
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Verify the following equipment is on:

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5.6.1
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Miller Nelson Unit.

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5.6.2 Air and water supplies.

5.6.3
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Gas Chromatograph

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5.6.4 NIOSH Service Life Apparatus Controller software program.
Procedure No. CET-APRS-STP-CBRN-0403
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5.7

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Establish the correct humidity and temperature using chilled mirror dew point

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hygrometer per the test standard in paragraph 6.3.

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Set the airflow to the required airflow for the test. Verify the airflow from the test

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fixture using the appropriate dry test meter.

5.9
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Weigh and record initial weight of the test canister on Test Data Sheet.

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c o 5.10 Take initial inhalation and exhalation resistances of the canister mounted on the

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facepiece at 85 liters per minute. Record the values on Test Data Sheet.

5.11
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Make sure the diverter valve in the system is diverting the challenge concentration

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airflow to the discharge and not into the test chamber Turn on the hydrogen

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cyanide cylinder.

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5.12
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Mount canister onto test fixture in testing chamber.

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5.13

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Turn on the hydrogen cyanide cylinder.

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5.14 Establish the test concentration of 470 ppm hydrogen cyanide for general

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category standard or 940 ppm hydrogen cyanide for specific category standard.

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5.15 Once the hydrogen cyanide concentration has been established, testing may begin.

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5.16 Direct challenge concentration airflow into test chamber

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5.17 Start timer. Airflow out of the fixture is directed into the breakthrough detector.

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Monitor and record the upstream and downstream temperatures of the air stream

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throughout testing. Record breakthrough values and times.

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5.18 Run test until breakthrough of 10 ppm hydrogen cyanide and cyanogen is

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observed or minimum service life is surpassed.

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5.19 Direct challenge concentration airflow out of the test chamber.

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5.20 Weigh and record final weight of the test canister on Test Data Sheet.

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5.21 Allow clean air to purge through the test chamber for 5 minutes.

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5.22
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Repeat steps 5.7 through 5.22 for each test described in section 6.3.

5.23
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End sampling mode program in the gas chromatograph.
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Procedure No. CET-APRS-STP-CBRN-0403
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5.24 When all tests are complete turn off hydrogen cyanide cylinder, clean regulator by

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purging with air, set temperature and humidity to zero and allow air to pass
through the system for 30 minutes.

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6. PASS OR FAIL CRITERIA

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6.1. The criterion for passing this test is set forth in 42 CFR Part 84, Subpart G,

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Section 84.63(a)(c)(d) and Subpart I, Section 84.110(c); Volume 60, Number 110,

n t June 8, 1995.

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6.2. This test establishes the standard procedure for ensuring that:

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84.63 Test requirements; general.

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(a) Each respirator and respirator component shall when tested by the applicant

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and by the Institute, meet the applicable requirements set forth in subparts H

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through L of this part.

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(c) In addition to the minimum requirements set forth in subparts H through L of

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this part, the Institute reserves the right to require, as a further condition of

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approval, any additional requirements deemed necessary to establish the

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quality, effectiveness, and safety of any respirator used as protection against

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hazardous atmospheres.

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(d) Where it is determined after receipt of an application that additional

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requirements will be required for approval, the Institute will notify the

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applicant in writing of these additional requirements, and necessary

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examinations, inspections, or tests, stating generally the reasons for such

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requirements, examinations, inspections, or tests.

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6.3
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HYDROGEN CYANIDE BENCH TEST FOR CANISTERS.

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6.3.1. General Category Standard.

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6.3.1.1. Resistance to airflow of both canister and system will be taken

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before and after each test.

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6.3.1.2. Three canisters will be tested at 64 Lpm, continuous airflow, 25

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% ± 5 % relative humidity (RH), 25 oC ±5 oC, containing 470

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ppm hydrogen cyanide Minimum service life will be 15, 30, 45 or

n t r 60 minutes as per manufacturer request.

c o 6.3.1.3. Three canisters will be tested at 64 Lpm, continuous airflow, 80

Un
% ± 5 % relative humidity (RH), 25 oC ± 5oC, containing 470
Procedure No. CET-APRS-STP-CBRN-0403
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ppm hydrogen cyanide. Minimum service life will be 15, 30, 45

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or 60 minutes as per manufacturer request.

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6.3.1.4. Three canisters will be tested at 100 Lpm, continuous airflow, 50

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% ± 5 % relative humidity (RH), 25 oC ± 5oC, containing 470 ppm

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hydrogen cyanide. Minimum service life for all canisters will be

r o l 5 minutes.

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6.3.1.5. End of service life concentration is 10 ppm, which is the sum of

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the breakthrough products of hydrogen cyanide and cyanogen.

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6.3.2. Specific Category Standard.

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6.3.2.1. Resistance to airflow of both canister and system will be taken

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before and after each test.

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6.3.2.2. Three canisters will be tested at 64 Lpm, continuous airflow, 25
% ± 5 % relative humidity (RH), 25 oC ± 5 oC, containing 940

tr o y
ppm hydrogen cyanide Minimum service life will be 15, 30, 45 or

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60 minutes as per manufacturer request.

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6.3.2.3. Three canisters will be tested at 64 Lpm, continuous airflow, 80

l l e % ± 5 % relative humidity (RH), 25 oC ± 5oC, containing 940

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ppm hydrogen cyanide. Minimum service life will be 15, 30, 45

t r o o p
or 60 minutes as per manufacturre request.

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6.3.2.4. Three canisters will be tested at 100 Lpm, continuous airflow, 50

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% ± 5 % relative humidity (RH), 25 oC ± 5oC, containing 940 ppm

r o l hydrogen cyanide. Minimum service life for all canisters will be

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5 minutes.

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6.3.2.5. End of service life concentration is 10 ppm, which is the sum of

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the breakthrough products of hydrogen cyanide and cyanogen.

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7. RECORDS AND TEST SHEETS

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7.1. All test data will be recorded on the CBRN HYDROGEN CYANIDE SERVICE

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LIFE test data sheet.

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7.2.
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All videotapes and photographs of the actual test being performed, or of the tested

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equipment shall be maintained in the task file as part of the permanent record.

7.3.
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All equipment failing any portion of this test will be handled as follows:
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Procedure No. CET-APRS-STP-CBRN-0403
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7.3.1. If the failure occurs on a new certification application, or extension of

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approval application, send a test report to the CET Section Chief and
prepare the hardware for return to the manufacturer.

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7.3.2. If the failure occurs on hardware examined under an Off-the-Shelf Audit

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the hardware will be examined by a technician and the CET Section Chief

r o l for cause. All equipment failing any portion of this test may be sent to the
manufacturer for examination and then returned to NIOSH. However, the

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hardware tested shall be held at the testing laboratory until authorized for

o
c o release by the CET Section Chief, or his designee, following the standard

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operating procedures outlined in Procedure for Scheduling, and Processing

l l e Post-Certification Product Audits, RB-SOP-0005-00.

t r o o p y
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Procedure No. CET-APRS-STP-CBRN-0403
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8.
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ATTACHMENTS

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8.1 Bench Top Set-Up.

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8.2 Data Sheet.

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Procedure No. CET-APRS-STP-CBRN-0403
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Revision History

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Revision l Date
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00

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21 September 2004 Historic document

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1.1 21 December 2005 Update header and format

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No changes to method

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