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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-0307

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DETERMINATION OF CBRN BASE GASES (AMMONIA)

Un o ll SERVICE-LIFE TEST, AIR-PURIFYING RESPIRATORS

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 Base Gases (Ammonia) Service Life Test Air-Purifying Respirators Standard Test

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Procedure submitted for Approval, Extension of Approval, or examined during Certified

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Product Audits, meet the minimum certification standards set forth in 42 CFR Part 84,

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Subpart G, Section 84.63(a)(c)(d); Volume 60, Number 110, June 8, 1995 and the

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Statement of Standard for Chemical, Biological, Radiological, and Nuclear (CBRN) Full-

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Facepiece Air- Purifying Respirator (APR) Dated March 7, 2003.

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2. GENERAL

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This STP describes the CBRN Base Gases (Ammonia) Service Life Test Air-Purifying

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Respirators Standard Test Procedure test in sufficient detail that a person knowledgeable in
the appropriate technical field can select equipment with the necessary resolution,

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conduct the test and determine whether or not the product passes the test.

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3.
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EQUIPMENT AND MATERIAL
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3.1. 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. An automated system to control the airflow,

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temperature, and humidity of an air supply for an operating system.

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Laboratory air and distilled water are supplied to the unit; the three sensors

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and controlling mechanisms are incorporated electronically. The capacity

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of the unit is airflow: 20 to 200 liters / minute +/- 2%), relative humidity:

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20 to 90 +/- 3 % and temperature ambient to 35 oC +/- 1oC

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U n l le
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Approvals:

c o n 1st Level 2nd Level 3rd Level

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3.1.2. EdgeTech Dew Prime II Hygrometer, Model 2000 or equivalent. A micro-

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processor based programmable chilled mirror dew point hygrometer . The

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hygrometer uses the dew point and ambient temperature to calculate the

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relative humidity. Ambient temperature range is: -50ºC to 130ºC ± 0.2ºC;

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relative humidity is 1% to 95% ± 0.5%.

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3.1.3. Air-Sentry IMS Ammonia Analyzer, Model 10R-NH3-4000M or

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equivalent. The analyzer is a system component that monitors the

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c o concentration of ammonia using the technology of Ion Mobility

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Spectroscopy. The analyzer range for ammonia is 1 to 3000 ppm ± 0.1 %

l l e of full scale.

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3.1.4. Air-Sentry IMS Ammonia Analyzer, Model 10R-NH3-50ppm or

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equivalent. The analyzer is a system component that monitors the

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concentration of ammonia using the technology of Ion Mobility

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Spectroscopy. The analyzer range for ammonia is 0.1 to 50 ppm ± 0.1 %
of full scale.

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3.1.5. Mass Flow Controller, Brooks Instruments, variable flow rate depending

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on use.

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

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Power supply and controller for the Brooks Mass Flow Controller or

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equivalent. The flow controllers are an integrally mounted control valve

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module with which stable gas flows can be achieved. Various flow rates

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are used with an accuracy of ± 0.7 % of rate and ± 0.2 % full scale.

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3.1.7. Dry Gas Meter. Must have NIST traceable calibration certificate.

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3.1.8. Certified cylinder of approximately 12.5 ppm NH3 and 2500 ppm NH3 in

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3.1.9. Ammonia cylinder, 99% purity

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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® fittings 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 Resistance tester consisting of a vacuum source capable of delivering 85 Lpm, a 6-
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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-APR-

r o l 007.

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4
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TESTIN\G REQUIREMENTS AND CONDITIONS

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

Un lNIOSH Standard Test Procedure entitled Determination Of Durability Test For

t r o Environmental And Transportation Conditions And Rough Handling Drop Test

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On Chemical Biological Radiological Nuclear (CBRN) Air-Purifying Respirators

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(APR) And Canisters Standard Test Procedure (STP).

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Un 4.2

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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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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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4.4
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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

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

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

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

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from the institute.

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4.5 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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4.6.1 Safety glasses, lab coats and hard-toe shoes must be worn at all times.

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4.6.2 Workbenches must be maintained free of clutter and non-essential test

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equipment.

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4.6.3

o n tWhen handling any broken glass laboratory equipment, lab technicians

and personnel must wear special gloves, which protect against lacerations

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Un
or punctures.
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4.7

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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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c o maintenance manuals.

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

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equipment must be repaired or replaced and properly set up and calibrated

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before starting all tests.

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5.2.
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After the manufacturer's specified warm-up period, adjust instruments to read

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zero and make adjustment for Labview software to read 0 ppm. Calibrate both

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ammonia analyzers using the certified gas cylinder containing the 12.5 or 2500

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ppm, during calibration make adjustment for Labview software to read the

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appropriate concentration for the detector.

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Un 5.3
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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

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test chamber.

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5.4 Verify the following equipment is on:

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5.4.1 Miller Nelson Unit.

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Air and water supplies.

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5.4.3

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NIOSH Service Life Apparatus Controller software program.

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5.5
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Establish the correct humidity and temperature as per the test standard in

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paragraph 6.3.

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5.6
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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.

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5.7 Weigh and record initial weight of the test canister on Test Data Sheet.
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5.8

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Take initial inhalation and exhalation resistances of the canister mounted on the

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facepiece and canister alone as described in RCT-APR-003 and RCT-APR-007.

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Record the values on Test Data Sheet.

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

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airflow to discharge and not into the testing chamber.

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5.10
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Mount canister onto test fixture and place in testing chamber.

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5.11 Divert 0.8 Lpm airflow from airflow line to the ammonia challenge detector.

5.12
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Turn on ammonia cylinder.

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5.13 Establish the test concentration of 2500 ppm ammonia.

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5.14
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Once the ammonia concentration has been established, testing may begin.

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5.15

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Direct challenge concentration airflow into test chamber.

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5.16 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.

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5.17
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Run test until breakthrough of 12.5 ppm is observed or minimum service life is

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surpassed. Record this data on the test data sheet.

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5.18 Direct challenge concentration airflow out of test chamber.

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

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5.20 Take final inhalation and exhalation resistances of the canister mounted on the

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facepiece and canister alone as described in RCT-APR-003 and RCT-APR-007.

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Record the values on Test Data Sheet.

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5.21
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Allow clean air to purge through test chamber for 10-15 minutes.

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5.22
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Repeat steps 5.7 through 5.21 for each test described in section 6.3.

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5.23 When all tests are completed turn off ammonia cylinder, set temperature and

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humidity to zero and allow air to pass through the system for 30 minutes.

5.

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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); Volume 60, Number 110, June 8, 1995.

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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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c o through L of this part.

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(c) In addition to the minimum requirements set forth in subparts H through L of
this part, the Institute reserves the right to require, as a further condition of

t r o p y
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 Base Gases (Ammonia) test for CBRN canisters

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

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after each test.

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6.3.2. Three canisters will be tested at 64 Lpm, continuous air flow, 25 % + 5 %

rrelative humidity (RH), 25 oC + 5 oC, and 2500 ppm ammonia. Minimum

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service life will be 15, 30, 45, 60, 90 or 120 minutes as per manufacturer

o
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6.3.3. Three canisters will be tested at 64 Lpm, continuous air flow, 80 %+ 5 %
relative humidity (RH), 25 oC + 5 oC, and 2500 ppm ammonia. Minimum

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service life will be 15, 30, 45, 60, 90 or 120 minutes as per manufacturer

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request.

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6.3.4. Three canisters will be tested at 100 Lpm, continuous air flow, 50 % + 5%

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relative humidity (RH), 25 oC + 5 oC, and 2500 ppm ammonia. Minimum
service life must be 5 minutes.

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6.3.5. End of service life concentration is 12.5 ppm ammonia.
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7. RECORDS AND TEST SHEETS

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All test data will be recorded on the determination of AMMONIA SERVICE

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LIFE test data sheet.

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7.2 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.

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7.3
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All equipment failing any portion of this test will be handled as follows:

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7.3.1 If the failure occurs on a new certification application, or extension of

l l e 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

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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

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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

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

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8 ATTACHMENTS

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8.1 Bench Top Set-up

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8.2 Data Sheet

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Attachment 8.2: Data Sheet

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Revision History

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Revision l Date
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20 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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