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National Institute for Occupational Safety and Health 

National Personal Protective Technology Laboratory 

P.O. Box 18070 

Pittsburgh, PA 15236

Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009

DETERMINATION OF HYDROGEN SULFIDE SERVICE LIFE TEST, 

AIR-PURIFYING RESPIRATORS WITH CANISTERS 

 STANDARD TESTING PROCEDURE (STP) 

1. PURPOSE

This test establishes the procedure for ensuring that the level of protection provided by airpurifying respirators with canisters (gas masks) submitted for Approval, Extension of Approval, 

or examined during Certified Product Audits meet the minimum hydrogen sulfide service life test 

requirements set forth in 42 CFR Part 84, Subpart G, Section 84.63 (a), (c), (d), and Subpart I, 

Section 84.110 (c). 

2. GENERAL

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

Respirators with canisters 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 or not the product passes the test. 

3. EQUIPMENT/MATERIAL

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

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

(250 Lpm) or equivalent. Air flow control accuracy is ± 2% F.S. Temperature 

control accuracy is ± 1° C. Humidity control accuracy is ± 3% R.H. 

3.1.2. Edge Tech Dew Prime II Hygrometer, Model 2000 or equivalent. Accuracy is ± 

0.2° C, ±0.5% RH. 

3.1.3. Radiometer America Multi-Titration System, Model DTS 800, burettes or 

equivalent. 

3.1.3. Interscan Corporation Model RM-17-2 hydrogen sulfide detector or equivalent. 

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

3.1.4. Interscan Corporation Model RM-17-0 hydrogen sulfide detector or equivalent. 

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

3.1.5. Interscan Corporation Model DS1 Dilution System or equivalent. Accuracy is 

Approvals: First Level Second Level Third Level Fourth Level 

 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 2 of 13 

 ± 5% F.S. flowmeter reading. 

3.1.6. Mass Flow Controllers, Brooks Instruments, variable flow rate depending on use, 

model series 5850S and 5853S. Accuracy is 0.7% set point and 0.2% FS. 

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

3.1.8. American Meter Co. Dry Test Meter Models DTM-325 and DTM-200.

3.1.9. "The Gilibrator", Primary Standard Airflow Calibrator or equivalent. 

 3.1.10. Gilian Gil-Air-3 Sampling Pump, or equivalent. 

3.1.11. Fisher Scientific Gas washing bottle or bubbler, catalog # 03-036 or equivalent. 

3.1.12. Erlenmeyer flasks or beakers, 100 to 500 milliliters (ml) 

3.1.13. Separatory funnel with rubber stopper, 125 ml. 

3.1.14. Aspirator bulb with tubing and stopper. 

3.1.15. Joint clamp. 

3.1.16. Pipets, 10-20 ml. 

3.1.17. Iodine (I2) (crystals) or 0.025N certified iodine solution. 

3.1.18. Potassium Iodide (KI) (granular). 

3.1.19. Sodium Thiosulfate Pentahydrate (Na2S2O3 ·5H2O , crystalline) or 0.025 Normal 

(N) certified Na2S2O3 solution. 

3.1.20. Sodium Hydroxide (NaOH) (granular). 

3.1.21. Boric Acid (granular). 

3.1.22. Starch, Soluble Potato, Powder. 

3.1.23. Certified cylinder of approximately 10 ppmv hydrogen sulfide in nitrogen. 

3.1.24. Hydrogen sulfide cylinder, 99 % purity. 

3.1.25. Electronic balance with accuracy of 0.01 grams (g). 

3.2. Test fixture for mounting canisters. The test fixture used is specific to each manufacturer 

depending on how the canister is mounted to the facepiece. In most cases chin-style 

canisters use the 40 mm thread for which we have adapters. In cases where other thread 

sizes are used, the adapters of the respirator are affixed by hot melt glue to a PVC pipe 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 3 of 13 

tee of appropriate size. Front or back mounted canisters are tested with their breathing 

tubes and adapters. 

 

3.3. The test chamber consisting of an approximately 12" x 12" x 7" air tight box, with 2 

clamp type locks on the door opening lined with gasket material, and appropriate inlet, 

outlet and sampling ports. This fixture is not commercially available. 

3.4. Refer to the following Work Instructions for further information on performing this test: 

 TEB-RCT-APR-WI-1006- Laboratory Safety Procedures for Hydrogen Sulfide Tests 

 TEB-RCT-APR-WI-1106- Calibration Procedures for Hydrogen Sulfide Tests 

TEB-RCT-APR-WI-1206- Start–Up and Shut–Down Procedures for 

 Hydrogen Sulfide Tests 

 TEB-RCT-APR-WI-1306- Using the LabView System for Hydrogen Sulfide Tests 

TEB-RCT-APR-WI-1406 – Reporting Results for Hydrogen Sulfide Tests

4. TESTING REQUIREMENTS AND CONDITIONS

4.1. Prior to beginning any testing, all measuring equipment to be used must have been 

calibrated in accordance with the testing laboratory’s calibration procedure and schedule. 

All measuring equipment utilized for this testing must have been calibrated using a 

method traceable to the National Institute of Standards and Technology (NIST) when 

available. 

4.2. Any laboratory using this procedure to supply certification test data as a contractor 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.* 

*Note 4.2 does not apply to Pretest data from applicants as required under 42 CFR 

84.64. 

4.3. 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. 

4.4. The precision and accuracy of this method was determined by validation testing of a 

single lot of commercially available multi-gas type cartridges. The results of these tests 

are shown in the table below. 

 

TEST TYPE 

MEAN SERVICE LIFE 

(MINUTES) STD. DEV. 

 

AS RECEIVED 199.55 11.51 

EQUIL. 25% RH 668.13 24.20 

EQUIL. 85% RH 565.95 51.43 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 4 of 13 

4.5. Normal laboratory safety practices must be observed. Please refer to Material Safety 

Data Sheets and the current NIOSH Pittsburgh Health and Safety Program for the proper 

protection and care in handling, storing, and disposing of the chemicals and gases used in 

this procedure. 

 

4.6. The cylinder of 99% hydrogen sulfide, as well as the calibration gas cylinders, are 

typically used inside the laboratory fume hood. If there is a release of 99% hydrogen 

sulfide outside the hood, sound an alarm, and any personnel in the laboratory should 

immediately exit from the building. THE LOWER EXPLOSIVE LIMIT OF H2S IS 

40,000 PPMV.

4.7. HYDROGEN SULFIDE BENCH TEST FOR CANISTERS 

4.7.1. Resistance to air flow of the complete respirator will be taken before and after 

each test (see 42 CFR 84.203). The standard testing procedures are described in 

TEB-APR-STP-003 and TEB-APR-STP-007. 

4.7.2. Test conditions as required by 42 CFR 84.63(a)(c)(d) and 84.110(c). 

SAMPLE CONDITION 

EQUILIBRATION 

CONDITIONS TEST CONDITIONS CONCENTRATION PPMV H2S 

 FOR 6 HOURS TEST BREAKTHROUGH 

 FRONT AND BACK CHIN STYLE 

 TEMP. FLOWRATE R.H. TEMP. FLOWRATE R.H. 

MOUNTED AND 

ESCAPE 

 ° C LPM % ° C LPM % 

1-3 

AS 

RECEIVED NA NA NA 25 64 50 10000 5000 10 

4-5 

EQUIL. 25% 

R.H. 25 64 25 25 32 50 10000 5000 10 

6-7 

EQUIL. 85% 

R.H. 25 64 85 25 32 50 10000 5000 10 

 Tolerances: 

 

PARAMETER TOLERANCE 

25°C ± 2.5°C 

32 LPM ± 0.5 LPM 

64 LPM ± 1.0 LPM 

25% R.H. ± 3% R.H. 

50% R.H. ± 3% R.H. 

85% R.H. +0/-5% R.H. 

5000 ppmv ± 10% 

10,000 ppmv ± 10% 

 

NOTES: R.H. levels greater than 85% are difficult to maintain and may cause rapid 

degradation of service life. 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 5 of 13 

Tolerance on accuracy of air flow rates exceeds specification on Miller Nelson control 

unit because flow rates are calibrated for every test. This improves the precision of the 

measurement and allows for the tighter tolerance on short-term drift. 

4.7.3. All equilibrated canisters will be resealed, kept in a position such that the 

direction of airflow would be horizontal, at room temperature, and testing shall 

begin within 18 hours. 

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. Set up the test equipment as shown in Figure 1. 

 

5.2. Calibrate the breakthrough H2S analyzer using the certified gas cylinder containing the 10 

ppmv standard. 

 

5.3. Prepare solutions as follows: (Note: commercially purchased certified solutions can be 

substituted.) 

5.3.1. 1.0 N Sulfuric acid: To a 1 liter volumetric flask containing 500 ml distilled 

water, add 28 ml concentrated sulfuric acid (H2SO4), then dilute to the 1 liter 

mark with distilled water. 

5.3.2. 1.0 N Sodium hydroxide: Dissolve 40g sodium hydroxide (NaOH) in a final 

volume of 1 liter distilled water. 

5.3.3. 0.025N Iodine solution: 

5.3.3.1. Dissolve 50g KI in 44.5 ml distilled water. 

5.3.3.2. Weigh 6.346g I2 crystals on a watch glass. 

5.3.3.3. Hold the watch glass over a 500 ml beaker. 

5.3.3.4. Wash the glass with half of the KI solution. 

5.3.3.5. Stir to dissolve crystals. 

5.3.3.6. Transfer to a 2 liter flask. 

5.3.3.7. Wash beaker with remaining KI solution and add distilled water to mark. 

5.3.4. 0.025N sodium thiosulfate solution: Dissolve 6.205 g sodium thiosulfate in a 

final volume 1 liter of distilled water. 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 6 of 13 

5.3.5. Starch Indicator: Weigh 1g boric acid and add to 100 ml of distilled water, bring 

to a boil. 

 5.3.5.1. Weigh 1-2g potato starch, add cold water to make a paste. 

 5.3.5.2. Add to boiling water and continue to boil for 1 minute. 

 5.3.5.3. Discard when starch solution becomes cloudy. 

5.4. Measure 100 ml of 1.0N NaOH into the gas bubbler. Attach Gil-Air 3 sampling pump to 

intake side of the gas bubbler. Connect outlet side of bubbler to Gilibrator. Check 1 lpm 

flow of the pump pulling through the sodium hydroxide solution. This setting will be 

used to sample the hydrogen sulfide concentration. 

5.5. Establish the correct humidity and temperature for the sample being tested as per the test 

requirements in paragraph 4.7. 

5.6. Set the airflow to the required level for the sample being tested as per the test 

requirements in paragraph 4.7. Calibrate the total airflow, including any additional flow 

arising from challenge gas flow rates and / or hygrometer flow rates, from the test fixture 

using the dry test meter. 

5.7. Weigh the canister and record the weight. 

5.8. Measure initial inhalation and exhalation resistances of the canister mounted on the 

facepiece as described in TEB-APR-STP-003 and TEB-APR-STP-007. Record values on 

the data sheet. 

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

discharge and not into the testing chamber. 

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

5.11. Open the 99% hydrogen sulfide cylinder. 

5.12. Establish the test concentration of 5,000 ppmv or 10,000 ppmv ± 10% hydrogen sulfide 

by setting the theoretical flow rate of pure hydrogen sulfide to mix with the flow of air to 

produce the required concentration (see table below). Then, set the mass flowmeter to 

that level. Adjust the flowmeter setting as required. Once the hydrogen sulfide 

concentration has been established by titration and/or dilution /measurement and is stable, 

testing may begin. 

 FLOW RATE 

FOR TEST 

FLOW RATE OF PURE 

HYDROGEN SULFIDE 

LPM 

FOR 5000 

PPMV 

FOR 10000 

PPMV 

 sccm or mL/min. 

32 160 320 

64 320 640 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 7 of 13 

 5.13. Connect tubing from the sample side of gas bubbler into the Gil-Air pump and tubing 

from the inlet side of the gas bubbler into the test gas concentration. 

 5.14. Turn Gil-Air pump on and sample at 1 lpm for 1 minute. 

 5.15. Remove the gas bubbler, and transfer the solution into an Erlenmeyer flask. 

 5.16. Rinse the gas bubbler with distilled water and transfer the washings into the flask. 

5.17. Attach the separatory funnel with a rubber stopper to the flask and clamp in place. There 

must be an air-tight seal between the funnel and flask to prevent the H2S from escaping. 

5.18. Measure 54 ml H2SO4 into the separatory funnel. 

5.19. Insert the rubber stopper of the aspirator into the top of the separatory funnel. 

5.20. Open the stopcock of the separatory funnel and aspirate the H2SO4 into the flask. 

5.21. Keeping the separatory funnel still in the flask, close the funnel stopcock and remove the 

aspirator stopper. 

5.22. Measure a known volume of 0.025N standard iodine solution (see 5.22.2) into the 

separatory funnel. The measured amount of iodine added should be in excess of the 

amount needed. 

 5.22.1. The hydrogen sulfide cannot be collected directly in iodine because the rate of 

reaction is too slow to capture it all without loss. The hydrogen sulfide is 

collected in sodium hydroxide, and released by sulfuric acid at a controlled rate. 

The sulfuric acid releases hydrogen sulfide when it reacts with the hydrogen 

sulfide-sodium hydroxide solution in the flask. The hydrogen sulfide thus 

released is immediately caught in a known excess of iodine. The excess iodine is 

back titrated with sodium thiosulfate. 

5.22.2. For example: 

Volume I2 = concentration 

 standard factor 305.6 ppmv/ml I2

 Volume I2 = 5,000 ppmv 

 305.6 ppmv/ml I2

Volume I2 = 16.4 ml I2

5.22.3. Iodine in an amount greater than 16.4 ml should be added, such as 20 ml. 

5.23. Record the amount of iodine added. 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 8 of 13 

5.24. Insert the rubber stopper of the aspirator into the top of the separatory funnel. 

5.25. Open the stopcock of the separatory funnel and aspirate the iodine into the flask. 

5.26. The solution will turn yellow. 

5.27. Remove the funnel and stopper. 

5.28. Back titrate the excess iodine of the sample concentration with 0.025N sodium thiosulfate 

dropwise until it is pale yellow. 

5.29. Add 5 ml of starch indicator. Solution will turn dark blue. 

5.30. Continue the titration until the blue color just disappears. 

5.31. Obtain the net iodine titration. For example, 

net I2 titration = volume I2 added - volume Na2S2O3 used 

 net I2 titration = 20.0 ml - 3.7 ml 

 net I2 titration = 16.3 ml I2 

 

 5.32. Calculate the concentration of hydrogen sulfide. 

Concentration (ppmv) = net I2 titration x standard factor 

Concentration = 16.3 ml I2 x 305.6 ppmv/ml I2

 Concentration = 4981 ppmv H2S 

5.33. As an alternate or additional method to measure challenge concentration, a sample is 

diluted by a factor of 11:1 or other suitable factor using the dilution system and measured 

on the detector used for challenge concentration. The dilution system is used because the 

test concentrations exceed the detector’s upper limit. Once the test concentration has 

been established, testing may begin. 

5.34. Monitor and record challenge and breakthrough temperatures, challenge RH and 

breakthrough values and times throughout testing. 

5.35. Run test until breakthrough of 10.0 ppmv is observed or minimum service life shown in 

section 6.2 is surpassed by 10%. 

5.36. At end of test, system will automatically direct challenge concentration airflow through 

diverter valve to discharge. 

5.37. Dismount canister, weigh and record final weight, and take final inhalation and 

exhalation resistances as described in TEB-APR-STP-003 and TEB-APR-STP-007. 
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Procedure No. TEB-APR-STP-0043B Revision: 2.1 Date: 20 January 2009 Page 9 of 13 

Measurement of the final inhalation and exhalation resistances is required for 

certification and audit testing. 

5.38. If there is another sample to test, repeat steps 5.7 – 5.35. 

5.39. After all tests are completed for the shift, set temperature and humidity to zero on the 

Miller Nelson system and allow clean air to pass through the system for 30 minutes. 

Purge the breakthrough and challenge detectors with clean air for 15 minutes. 

6. PASS/FAIL CRITERIA

6.1. The legal basis 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). 

6.2 Minimum service life requirements for canisters are shown below. 

 

Test atmosphere 

Canister type Test condition 

Gas or 

vapor 

Concentration 

(parts per 

million 

volume) 

Flow rate 

(liters per 

minute) 

Number of 

tests 

Maximum 

allowable 

penetration 

(parts per 

million 

volume)1

Minimum 

service life 

(minutes) 

Hydrogen 

sulfide 

Front and Back 

Mounted 

As received 

Equilibrated 

H2S 

H2S 

10,000 

10,000 

64 

32 

3 

4 

10 

10 

12 

12 

Hydrogen 

sulfide 

Chin-Style 

As received 

Equilibrated 

H2S 

H2S 

5,000 

5,000 

64 

32 

3 

4 

10 

10 

12 

12 

Hydrogen 

sulfide 

Escape 

As received 

Equilibrated 

H2S

H2S 

10,000 

10,000 

64 

32 

3 

4 

10 

10 

12 

12 

1

Minimum life will be determined at the indicated penetration. 

7. RECORDS/TEST SHEETS

7.1. Record the test data in a format that shall be stored and retrievable. 

8. ATTACHMENTS

 8.1. Figure 1. - Bench Top Set-Up 

8.2. Data Sheet 
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Procedure No. TEB-APR-STP-0043BB Revision: 2.0 Date: 14 March 2008 Page 10 of 13 

8.1. Figure 1. - Bench Top Set-Up 
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Procedure No. TEB-APR-STP-0043BB Revision: 2.0 Date: 14 March 2008 Page 11 of 13 

8.2. Data Sheet 

RB - RESPIRATOR CERTIFICATION TEAM 

 GAS & VAPOR RESPIRATOR TEST DATA SHEET (Ref.33-48,50,62) STP No.: [ ] 

 Task Number: TN- Gas Name: 

Manufacturer: Item Tested: 

RESISTANCE Maximum Allowable Resistance 

 (mm of H2O) 

 Actual Resistance 

 (mm of H2O) 

 Inhalation Exhalation Inhalation Exhalation 

 Test 

Initial Initial 

Final Initial Final 

 Result 

 1

 2

 3

 4

 5

 6

 7

 Overall Results: Pass Fail Comment: 

WEIGHTS WEIGHTS (gm) AIRFLOW (lpm)

 AND 

 AIRFLOWS Test Rate (PAPR Only)

 Test 

Con'd Conc. 

(ppmv) RH% lpm Initial Final 

 1

 2

 3

 4

 5

 6

 7 

 Overall Results: Pass Fail Comment: 
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Procedure No. TEB-APR-STP-0043BB Revision: 2.0 Date: 14 March 2008 Page 12 of 13 

DATA TABLE

 Temperature (oC) 

 Test 

 Test 

 Cond. 

 Final 

 Time (min) 

 Leakage 

 (ppmv) 

 Dns

tream 

 Upstr

eam 

 Corrected 

 Time (min) 

 1 

 2 

 3 

4 

 5 

 6 

 7 

 Overall Results: Pass Fail Comment: 

 Was all testing equipment in calibration throughout all testing: Yes No 

 Signature: Date: 

RB - RESPIRATOR CERTIFICATION TEAM Page 2

 GAS & VAPOR RESPIRATOR TEST DATA SHEET (Ref.33-48,50,62) STP No.: [ ] 

 Task Number: TN- Gas Name: 

Manufacturer: Item Tested: 

 

Additional Comments: 

Signature: Date: 
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Procedure No. TEB-APR-STP-0043BB Revision: 2.0 Date: 14 March 2008 Page 13 of 13 

Revision History 

Revision Date Reason for Revision 

1.0 14 March 2002 Historic document 

1.1 30 June 2005 Update header and format to reflect lab move from Morgantown, WV 

No changes to method 

2.0 14 March 2008 Significant rewrite of form and clarification of technical content. 

Section Change 

2.1 20 January 2009 4.7.2 Changes to column headers in table: note the most 

critical of these, sub-columns under Test Concentration, 

"Front and Back Mounted" and "Chin Style and Escape," 

revised to: "Front and Back Mounted and Escape" and 

"Chin Style"