Approvals: 1st Level 2nd Level 3rd Level 

National Institute for Occupational Safety and Health 

National Personal Protective Technology Laboratory 

P.O. Box 18070 

Pittsburgh, PA 15236 

Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005

DETERMINATION OF CBRN HYDRIDE GASES (PHOSPHINE) 

 SERVICE-LIFE TEST, AIR-PURIFYING RESPIRATORS 

STANDARD TEST PROCEDURE (STP) 

1. PURPOSE

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

the CBRN Hydride Gases (Phosphine) Service Life, Air-Purifying Respirators Standard 

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

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

Part 84, Subpart G, Section 84.63(a)(c)(d); Volume 60, Number 110, June 8, 1995 and 

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

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

2. GENERAL

This STP describes the Determination of Phosphine Service Life Test, Air-Purifying 

Respirators test in sufficient detail that a person knowledgeable in the appropriate 

technical field can select equipment with the necessary resolution, conduct the test and 

determine whether the product passes the test. 

3. EQUIPMENT AND MATERIAL

3.1. The list of necessary test equipment and materials follows: 

3.1.1. Flow-Temperature-Humidity Control System or equivalent. MillerNelson (MN) control system, Model HCS-401. An automated system to 

control the airflow, temperature, and humidity of an air supply for an 

operating system. Laboratory air and distilled water are supplied to the 

unit; the three sensors and controlling mechanisms are incorporated 

electronically. The capacity of the unit is airflow: 20 to 200 liters / 

minute +/- 2%), relative humidity: 20 to 90 +/- 3 % and temperature 

ambient to 35 o

C +/- 1oC.

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 2 of 9 

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

micro- processor based programmable chilled mirror dew point 

hygrometer. The hygrometer uses the dew point and ambient temperature 

to calculate the relative humidity. Ambient temperature range is: -50oC to 

130oC ± 0.2oC; relative humidity is 1% to 95% ± 0.5% 

3.1.3. Labview software developed for NIOSH Service Life Testing. 

3.1.4. California Analytical Instruments, Model 1314 Photoacoustic Multigas 

Monitor with UA0970 optical filter or equivalent. This monitor uses 

photoacoustic infra-red detection to measure gases that absorbs infer-red 

light. A filter is used to select the wavelength specific for the gas being 

detected. Range for phosphine is 10000 to 1.0 ppm ± 0.1 ppm. 

3.1.5. CEA Model TG-4000BA Phosphine detector or equivalent. This detector uses 

electrochemical sensor for detection of phosphine. It has an internal vacuum 

pump for drawing the sample. Range is 0 to 1 ppm.

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

on use. 

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

Power supply and controller for the Brooks Mass Flow Controller or 

equivalent. The flow controllers are an integrally mounted control valve 

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

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

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

3.1.9. Certified cylinder of approximately 1 and 300 parts per million (ppm) 

PH3. 

3.1.10. Phosphine cylinder, 99% purity, with regulator and purge valve. 

3.1.11. Nitrogen cylinder, 99% purity. 

3.2 Test fixture for mounting canisters. 

3.3 The test chamber consisting of a 12" x 111⁄2" x 7" air tight metal box with door 

opening lined with gasket material. Two 1⁄2" bulkhead Swaglok® fittings located 

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

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

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

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 3 of 9 

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

appropriate for items being tested. See description in RCT-APR-003 and RCTAPR-007. 

4. TESTING REQUIREMENTS AND CONDITIONS

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

NIOSH Standard Test Procedure entitled Determination Of Durability Test For 

Environmental And Transportation Conditions And Rough Handling Drop Test 

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

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

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

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

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 

the National Institute of Standards and Technology (NIST). 

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

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

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

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

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

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

from the institute. 

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

accordance with laboratory procedures and NIOSH/NPPTL guidance. Sound 

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

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

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

tolerance can be higher but not lower. 

4.5 Compressed gas cylinders must meet all applicable Department of Transportation 

requirements for cylinder approval as well as retesting / requalification. 

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

precautions described in the current NIOSH Pittsburgh Health and Safety 

Program. 

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

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

equipment. 

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 4 of 9 

4.6.3 When handling any broken glass laboratory equipment, lab technicians 

and personnel must wear special gloves, which protect against lacerations 

or punctures. 

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

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

disposing of the chemicals and gases used in this procedure.

5. PROCEDURE

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

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

maintenance manuals. 

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

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

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

5.2. Calibrate photoacoustic monitor for phosphine the challenge concentration of 

approximately 300 ppm. 

5.3. Calibrate the CEA phosphine monitor for the breakthrough concentration of 

approximately 0.3 ppm. 

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

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

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

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

for the hygrometer is placed in the challenge gas stream immediately before the 

test chamber. 

5.5. Verify the following equipment is on:

5.5.1. Miller Nelson Unit. 

5.5.2. Air and water supplies. 

5.5.3. NIOSH Service Life Apparatus Controller software program.

5.6. Establish the correct humidity and temperature as per the test standard in 

paragraph 6.3

5.7. Set the airflow to the required airflow for the test and the number of test being run 

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

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 5 of 9 

meter.

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

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

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

Record the values on Test Data Sheet. 

5.10. Make sure the diverter valve in the system is diverting the challenge concentration 

airflow to discharge and not into the testing chamber. 

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

5.12. At the phosphine regulator, using the purge valve introduce dry nitrogen into the 

challenge introduction for five minutes. This should purge any contaminants and 

moisture from the phosphine introduction system. The system should be clear of 

residual moisture. 

5.13. Start Nitrogen Dilution mass flow controller and set flow rate. 

5.14. Miller Nelson Unit with the humidity turned down to zero. Set airflow to system. 

5.15. Check the airflow from at the test fixture using the dry test meter. 

5.16. Shut off nitrogen purge flow, open Phosphine cylinder with phosphine mass flow 

controller set at “0”. Gradually, open mass flow controller to establish the test 

concentration for 300 ppm Phosphine in 64 or 100 liters per minute air. 

5.17. Connect tubing from the tee in the airflow line to the phosphine challenge 

detector. 

5.18. Once the test concentration of 300 ppm has been established, testing may begin. 

5.19. Direct challenge concentration airflow into test chamber. 

5.20. Start timer. Monitor effluent concentration. Monitor upstream and downstream 

temperatures throughout testing, record beginning and final temperatures on the 

test data sheet. 

5.21. Run test until breakthrough of 0.3 ppm is observed or minimum service life is 

surpassed. 

5.22. Direct challenge concentration airflow out of the test canister. 

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 6 of 9 

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

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

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

Record the values on Test Data Sheet. 

5.25. Allow clean air to purge through the test chamber. 

5.26. Repeat steps 5.6 through 5.25 for each test described in section. 

5.27. When all tests are completed, turn off phosphine cylinder, set temperature and 

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

5.28. Open dry nitrogen Purge Valve on regulator, to clear system of residual 

phosphine. Allow nitrogen to purge through system for 10 - 15 minutes. 

6. PASS OR FAIL CRITERIA

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

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

June 8, 1995. 

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

 84.63 Test requirements; general. 

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

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

through L of this part. 

(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 

approval, any additional requirements deemed necessary to establish the quality, 

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

atmospheres. 

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

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

in writing of these additional requirements, and necessary examinations, 

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

examinations, inspections, or tests. 

6.3. Hydride Gases (Phosphine) test for CBRN canisters 

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 7 of 9 

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

after each test. 

6.3.2. Three canisters will be tested at 64 Lpm, continuous airflow, 25 % ± 5 % 

relative humidity (RH), 25 o

C ± 5 oC and 300 ppm phosphine. Minimum 

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

request. 

6.3.3 Three canisters will be tested at 64 Lpm, continuous airflow, 80 % ± 5 % 

relative humidity (RH), 25 o

C ± 5 oC and 300 ppm phosphine. Minimum 

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

request. 

6.3.4. Three canisters will be tested at 100 liters / minute, continuous airflow, 50 

% ± 5 % relative humidity (RH), 25 o

C ± 5 oC and 300 ppm phosphine. 

Minimum service life must be 5 minutes. 

6.3.5 End of service life concentration is 0.3 ppm phosphine. 

7. RECORDS AND TEST SHEETS

7.1. All test data will be recorded on the PHOSPHINE SERVICE LIFE test data sheet. 

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

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

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

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

approval application, send a test report to the RCT Leader and prepare the 

hardware for return to the manufacturer. 

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

the hardware will be examined by a technician and the RCT Leader 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 

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

release by the RCT Leader, or his designee, following the standard 

operating procedures outlined in Procedure for Scheduling, and Processing 

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

8. ATTACHMENTS

8.1 Bench Top Set-Up 

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 8 of 9 

8.2 Data Sheet. Uncontrolled Copy 

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Procedure No. CET-APRS-STP-CBRN-0309 Revision: 1.1 Date: 13 December 2005 Page 9 of 9 

Revision History 

Revision Date Reason for Revision 

00 20 September 2004 Historic document 

1.1 13 December 2005 Update header and format 

No changes to method 

 

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