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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: 13 December 2005

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Procedure No. CET-APRS-STP-CBRN-0308

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DETERMINATION OF CBRN NITROGEN OXIDE

Un o ll GASES (NITROGEN DIOXIDE) SERVICE-LIFE TEST,

AIR-PURIFYING RESPIRATORS STANDARD

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TEST PROCEDURE (STP)

1.
c o PURPOSE
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This test establishes the standard procedure for ensuring that the level of protection

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provided by CBRN Nitrogen Oxide Gases (Nitrogen Dioxide) Service Life Test, Air-Purifying

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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 certification requirements set forth in

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42 CFR Part 84, Subpart G, Section 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) Full- Facepiece Air- Purifying Respirator (APR) Dated March 7, 2003.

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2.
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GENERAL
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This STP describes the Determination of CBRN Nitrogen Dioxide Service Life Test, Air-

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Purifying Respirators Standard Test Procedure in sufficient detail that a person

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r o o py
knowledgeable in the appropriate technical field can select equipment with the necessary

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

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3. 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 ±

n c o 0.3%).

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U o l l
n t r
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Approvals: 1st Level 2nd Level 3rd Level

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 Procedure No. CET-APRS-STP-CBRN-0308
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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
hygrometer uses the dew point and ambient temperature to calculate the

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

o d
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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Interscan Corporation Model RM-15-0 nitrogen dioxide detector or

c o o
equivalent. This detector is an electrochemical voltammetric sensor.

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Detector range: 0 - 1999 ppm, resolution: 1 ppm.

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3.1.5e Interscan Corporation Model RM-15-2 nitrogen dioxide detector or

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equivalent. This detector is an electrochemical voltammetric sensor.

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Detector range: 0 - 19.99 ppm, resolution: 0.01 ppm.

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3.1.6

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Interscan Corporation Model RM-54-1 nitrogen oxide detector or
equivalent. This detector is an electrochemical voltammetric sensor.

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Detector range: 0 - 199.9 ppm, resolution: 0.1 ppm.

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3.1.7 Mass Flow Controller, Brooks Instruments, variable flow rate depending

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on use.

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3.1.8 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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3.1.9 Dry Gas Meter. Must have NIST traceable calibration certificate.

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3.1.10 Certified cylinders of 200 parts per million and 1 parts per million

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nitrogen dioxide in nitrogen.

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3.1.11 Certified cylinders of 25 parts per million nitrogen oxide in nitrogen.

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3.1.12 Nitrogen dioxide cylinder, 2.5 percent purity.

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3.2 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.
 Procedure No. CET-APRS-STP-CBRN-0308
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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. 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

l l e
On Chemical Biological Radiological Nuclear (CBRN) Air-Purifying Respirators
(APR) And Canisters Standard Test Procedure (STP).

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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
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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4.3
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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

c o l e d
from the institute.

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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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4.5
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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 Normal laboratory safety practices must be observed. This includes safety

U Program.
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precautions described in the current NIOSH Pittsburgh Health and Safety

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

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 Procedure No. CET-APRS-STP-CBRN-0308
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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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C o
When handling any broken glass laboratory equipment, lab technicians

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and personnel must wear special gloves, which protect against lacerations

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or punctures.

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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c o 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.

U n 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. 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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nitrogen dioxide analyzers and the nitrogen oxide analyzer using the certified gas

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cylinder containing the 1 ppm or 200 ppm nitrogen dioxide and 25 ppm nitrogen

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oxide. During calibration make adjustment for Labview software to read the

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appropriate concentration for each detector.

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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.

l l e
5.4
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Verify the following equipment is on:

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c o n
5.4.1
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Miller Nelson Unit.

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Air and water supplies.

t r o
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5.4.3 NIOSH Service Life Apparatus Controller software program.

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5.4.4 Nitrogen dioxide cylinder, 2.5 percent purity.
 Procedure No. CET-APRS-STP-CBRN-0308
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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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o n 5.6
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Set the airflow to the required airflow for the test and the number of test being run

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at one time. Verify the airflow from the test fixture using the appropriate dry test

r o l
meter.

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

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

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5.10
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Divert 0.5 Lpm airflow from airflow line to the nitrogen dioxide challenge

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detector.

tr o y
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5.11
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Ensure that the nitrogen gas is ready for immediate flushing of regulator through

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the purge valve.

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Un 5.12
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Turn on nitrogen dioxide cylinder.

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5.13
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Establish the test concentration of 200 ppm nitrogen dioxide.

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5.14
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Direct challenge concentration airflow into test chamber.

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Start timer. Monitor effluent concentration using both the nitrogen dioxide and

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nitrogen oxide analyzers. Monitor upstream and downstream temperatures

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throughout testing, record beginning and final temperatures on the test data sheet.

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5.16 Run test until breakthrough of 1 ppm nitrogen dioxide or 25 ppm nitrogen oxide is

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observed or minimum service life is surpassed. Record this data on the test data

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sheet.

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5.17 Direct challenge concentration airflow away from test chamber.

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

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5.19
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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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 Procedure No. CET-APRS-STP-CBRN-0308
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5.20 Repeat steps 5.7 through 5.21 for each test described in section 6.3.

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

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6. PASS/FAIL CRITERIA

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

t r o Section 84.63(a)(c)(d); Volume 60, Number 110, June 8, 1995.

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o n6.2.
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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

c o d C
through L of this part.

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

tr o
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 quality,

c o n o
effectiveness, and safety of any respirator used as protection against hazardous

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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 applicant

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in writing of these additional requirements, and necessary examinations,

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

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examinations, inspections, or tests.

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6.3 Nitrogen oxide gases (Nitrogen dioxide) 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 %

t r o p
relative humidity (RH), 25 oC ± 5 oC, and 200 ppm nitrogen dioxide.

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

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manufacturer request.

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l l
Three canisters will be tested at 64 Lpm, continuous air flow, 80 % ± 5 %

o
r
relative humidity (RH), 25 oC ± 5 oC, and 200 ppm nitrogen dioxide.

o n t
Minimum service life will be 15, 30, 45, 60, 90 or 120 minutes as per
manufacturer request.

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 Procedure No. CET-APRS-STP-CBRN-0308
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6.3.4 Three canisters will be tested at 100 Lpm, continuous air flow, 50 % + 5

r o l % relative humidity (RH), 25 oC + 5 oC, and 200 ppm nitrogen dioxide.

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Minimum service life of 5 minutes.

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6.3.5 End of service life concentration is 1 ppm nitrogen dioxide or 25 ppm

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nitric oxide.

7.
r o l
RECORDS AND TEST SHEETS

n t o p y
c o 7.1. All test data will be recorded on the NITROGEN DIOXIDE SERVICE LIFE test

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data sheet.

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

t r o p y
equipment shall be maintained in the task file as part of the permanent record.

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c o n7.3.
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All equipment failing any portion of this test will be handled as follows:

U n l le
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 RCT Leader and prepare the

o n p
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

l l e
the hardware will be examined by a technician and the RCT Leader for

y
cause. All equipment failing any portion of this test may be sent to the

t r o o p
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

c o l e d
release by the RCT Leader, or his designee, following the standard

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operating procedures outlined in Procedure for Scheduling, and Processing

r o l
Post-Certification Product Audits,

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RB-SOP-0005-00.

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8. ATTACHMENTS

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8.1
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Bench Top Set-Up.

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8.2
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Data Sheet.

t o py
c o n d C
U n l le
t r o
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 Procedure No. CET-APRS-STP-CBRN-0308
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Revision History

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Revision l Date
p y Reason for Revision
00

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20 September 2004 Historic document

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1.1 13 December 2005 Update header and format

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No changes to method

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