National Institute for Occupational Safety and Health 

National Personal Protective Technology Laboratory 

P.O. Box 18070 

Pittsburgh, PA 15236 

Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008

DETERMINATION OF CBRN HYDRIDE GASES (PHOSPHINE) SERVICE LIFE 

TEST, TIGHT-FITTING POWEREDAIR-PURIFYING RESPIRATORS (PAPR) 

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, Tight-Fitting Powered Air-Purifying Respirators 

(PAPR) 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) Powered 

Air- Purifying Respirator (PAPR). 

2. GENERAL

This STP describes the Determination of CBRN Hydride Gases (Phosphine) Service Life Test, 

Tight-Fitting Powered 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. Miller-Nelson 

(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. 

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

Approvals: 

First Level Second Level Third Level Fourth Level 

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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 

infrared detection to measure gases that absorb infrared 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 Test Meter. American Meter Co., model and size depending on air flow 

rate to be measured. Must have NIST traceable calibration certificate. 

3.1.9. Certified cylinder of approximately 1 ppm and 300 ppm phosphine. 

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 an air tight box with door opening lined with gasket 

material. Two fittings located on 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 equipment as described in standard test procedures RCT-APR-0007. 

3.5. Airflow measurement equipment as described in standard test procedure RCT-APR00012. 

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 Durability Conditions Process For Environmental, 

Transportation And Rough Handling Conditions On Chemical Biological, Radiological 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 3 of 11 

and Nuclear (CBRN) Respiratory Protective Devices (RPD) Standard Conditioning 

Procedure (SCP). 

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. 

4.6.3. When handling any broken glass laboratory equipment, lab technicians and 

personnel must wear special gloves, which protect against lacerations or 

punctures. 

4.7. 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 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 4 of 11 

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 using certified gas cylinder containing 

approximately 300 ppm phosphine. 

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. Set the required airflow for the system. Individual canisters will be tested by dividing 

115 Lpm by the number of air purifying elements elements on the system. See worksheet 

2 in appendix 8.2. Verify the airflow from the test fixture using the appropriate dry test 

meter. 

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

5.8. Take and record initial airflow measurements in accordance with RCT-APR-012. See 

section 84.1152 (b) Title 42, Code of Federal Regulations, Part 84 for minimum airflow 

requirements. 

5.9. Take and record initial inhalation resistances for tight-fitting PAPR in accordance with 

RCT-APR-007. See Sections 84.122, 84.203, 84.1157 Title 42, Code of Federal 

Regulations, Part 84 for breathing resistance requirements 

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. 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 5 of 11 

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 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. 

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 ± 30 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 selected service life time is 

surpassed. 

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

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

5.24. Take and record final airflow measurements in accordance with RCT-APR-012. See 

section 84.1152 (b) Title 42, Code of Federal Regulations, Part 84 for minimum airflow 

requirements. 

5.25. Take and record final inhalation resistances for tight-fitting PAPR in accordance with 

RCT-APR-007. See Sections 84.122, 84.203, 84.1157 Title 42, Code of Federal 

Regulations, Part 84 for breathing resistance requirements. 

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

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

5.28. 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. 

5.29. Open dry nitrogen purge valve on regulator, to clear system of residual phosphine. Allow 

nitrogen to purge through system for 10 - 15 minutes. 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 6 of 11 

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 Gas (Phosphine) test for CBRN canisters 

6.3.1. Inhalation resistance to airflow of system will be taken before and after each test. 

6.3.2. Airflow measurements of system must be taken before and after each test. 

6.3.3. Three canisters will be tested at the determined Lpm, continuous airflow, 25 % ± 

2.5 % relative humidity (RH), 25 o

C ± 2.5 oC and 300 ppm phosphine. 

6.3.4. Three canisters will be tested at the determined Lpm, continuous airflow, 80 % ± 

2.5 % relative humidity (RH), 25 o

C ± 2.5 oC and 300 ppm phosphine. 

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

manufacturer request. 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: 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 7 of 11 

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-SOP0005-00. 

8. APPENDICIES

8.1. Bench Top Set-Up 

8.2. Test Data Sheet 

8.3. Service life testing airflow calculations 

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Appendix 8.1: Bench Top Set-Up Uncontrolled Copy 

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Appendix 8.2: Test Data Sheet Uncontrolled Copy 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 10 of 11 

Appendix 8.3: Service life testing airflow calculations

Tight-fitting PAPR 

___________ Number of filtering elements on a tight-fitting PAPR System. 

115 Lpm airflow 

Airflow for service life test = 115 Lpm / number of filtering elements 

Test Flow 

4 Cartridges 3 Cartridges 2 Cartridges 1 Cartridge 

28.8 Lpm 38.3 Lpm 57.5 Lpm 115 Lpm 

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Procedure No. TEB-CBRN-STP-0509 Revision: 0.1 Date: 2 June 2008 Page 11 of 11 

Revision History 

Revision Date Reason for Revision 

0.0 21 November 2006 Original Issue 

0.1 2 June 2008 Editorial corrections – no change to technical content 

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