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. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005

DETERMINATION OF o-CHLOROBENZYLIDENE MALONONITRILE (CS) 

SERVICE LIFE TEST, AIR-PURIFYING RESPIRATORS 

STANDARD TESTING PROCEDURE (STP) 

1. PURPOSE

This test establishes the procedure for ensuring that the level of protection provided by the oChlorobenzylidene malononitrile (CS) service life requirements on gas mask air-purifying 

respirators submitted for Approval, Extension of Approval, or examined during Certified Product 

Audits meet the certification requirements set forth in 42 CFR Part 84, Subpart G, Section 

84.63(a)(c)(d) and Subpart I, Section 84.110; Volume 60, Number 110, June 8, 1995. 

2. GENERAL

This STP describes the Determination of CS 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 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 

or equivalent. 

 3.1.2. UV Spectrophotometer, Spectronic Model 601 or equivalent. 

 3.1.3. Supelco Tenax- GC sample tubes custom made to the following specifications: 

10cm long, 10 mm outside diameter, 8 mm inside diameter. Front section 

contains 70 mg 35/60 mesh Tenax-GC; back section contains 35 mg 35/60 

Tenax-GC. The Tenax-GC is held in place in the sampling tube by 3 mm 

silanized glass wool plugs. A 3 mm plug also separates the two sections. The 

tubes are sealed at both ends. 

3.1.4. Digi Sense Scanning Thermocouple Thermometer Model 92800-10.

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 2 of 15 

 3.1.5. Gelman Acrodisc CR PTFE product number 4226, 1 micron pore size or 

equivalent. 

 3.1.6. Supelco 15 ml screw cap vials with hole caps and septa. 

 3.1.7. "The Gilbrator", Primary Standard Airflow Calibrator, or equivalent. 

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

 3.1.9. o-Chlorobenzylidene malononitrile (CS). 

 3.1.10. Hexanes, Spectroanalyzed grade. 

 3.1.11. Methylene chloride, Spectroanalyzed grade. 

 3.1.12. 5 ml gas tight glass syringe, volumetric flasks 10-100 ml volume, Eppendorf 

pippettors or microliter syringes 10 microliter to 500 microliter volume. 

 3.1.13. Remote control hot plate. 

 3.1.14. Electronic Balance with an accuracy of 0.001 grams (g). 

 3.1.15. Teflon tubing 1⁄2" diameter for all connections. 

 3.1.16. Tear gas generator: consists of a steel drum, 5 gallon capacity, approximately 

14" in diameter, 18" high, with removable top and ring type closure. Two holes 

are cut in the lid, one for clean air to enter the chamber and one for the challenge 

gas to pass through the canister and out into the hood. One 1⁄2" hole is cut into 

the side of the drum near the bottom. The cord from the remote control electric 

hot plate exits out the hole. Make sure the openings are well sealed with rope 

caulking, hot melt glue, or other suitable material. A 600 ml beaker containing 

CS is placed on the hot plate inside the drum and the heat regulated by the 

remote controller of the hot plate. 

 3.1.17. Test fixture for mounting cartridges and canisters. The test fixture used is 

specific to each manufacturer depending on how the cartridge, canister, or 

powered air-purifying respirator (PAPR) is mounted to the facepiece. The T-end 

has a 29/42 ground glass joint glued in place. Canisters are tested with their 

connections glued into the ground glass joint. In most cases the cartridge cups of 

the respirator are affixed by hot melt glue to a PVC pipe tee of appropriate size. 

PAPR cartridges and canisters are tested on their blower units or suitable 

substitution. 

 3.1.18. Resistance tester consisting of a vacuum source capable of delivering 85 liters 

per minute (lpm), a 6-inch slant manometer, and a 29/42 female ground glass 

joint. The resistance testers currently being used are located on the silica dust 

chamber. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 3 of 15 

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 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). 

4.2. Normal laboratory safety practices must be observed. This includes safety precautions 

described in the current ALOSH Facility Laboratory Safety Manual. 

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

4.2.2. Work benches must be maintained free of clutter and non-essential test 

equipment. 

4.2.3. When handling any glass laboratory equipment, lab technicians and personnel 

must wear special gloves which protect against lacerations or punctures. 

4.3. CS TEAR GAS BENCH TEST REQUIREMENTS

 4.3.1. Resistance to air flow will be measured before each test (see 84.122). 

 4.3.2. Three "as received" canisters or cartridges will be tested at 64 lpm, continuous air 

flow, 50 + 5 percent relative humidity (RH), approximately 25 degrees Celsius 

(°C), and 3 ppm (23.1 mg/m3

) of CS. 

 4.3.3. Two canisters or cartridges will be equilibrated at room temperature by passing 

25 percent RH air through them at 64 lpm for 6 hours and then testing them at 

25 + 5 percent RH, approximately 25°C, and 64 lpm continuous flow rate 

containing 3 ppm of CS. 

 4.3.4. Two canisters or cartridges will be equilibrated at room temperature by passing 

85 percent RH air through them at 64 lpm for 6 hours and then testing them at 

85 + 5 percent RH, approximately 25°C, and 64 lpm continuous flow rate 

containing 3 ppm of CS. 

 4.4 CS TEAR GAS BENCH TEST FOR TIGHT FITTING POWERED AIR-PURIFYING 

RESPIRATORS

4.4.1. Resistance to air flow and PAPR airflow will be measured before each test. 

 (see 84.122). 

 4.4.2. Three "as received" canisters or cartridges will be tested at 115 lpm, continuous 

air flow, 50 + 5 percent RH, approximately 25 degrees Celsius (°C), and 3 ppm 

(23 mg/m 3

) of CS. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 4 of 15 

 4.4.3. Two canisters or cartridges will be equilibrated at room temperature by passing 

25 percent RH air through them at 115 lpm for 6 hours and then testing them at 

25 + 5 percent RH, approximately 25°C, and 115 lpm continuous flow rate 

containing 3 ppm of CS. 

4.5. CS TEAR GAS BENCH TEST FOR VALVELESS GAS MASKS

4.5.1. Resistance to air flow will be measured before each test (see 84.122). 

 4.5.2. Three "as received" canisters will be tested at 64 lpm, continuous air flow, 

50 + 5 percent RH, approximately 25 degrees Celsius (°C), and 3 ppm of CS. 

 4.5.3. Two canisters will be equilibrated at room temperature by passing 25 percent 

RH air through them at 64 lpm for 6 hours and then testing them at 25 + 5 

percent RH, approximately 25°C, and 64 lpm continuous flow rate containing 3 

ppm of CS. 

 4.5.4. Two canisters will be equilibrated at room temperature by passing 85 percent 

RH air through them at 64 lpm for 6 hours and then testing them at 85 + 5 

percent RH, approximately 25°C, and 64 lpm continuous flow rate containing 3 

ppm of CS. 

 4.5.5. One completely assembled gas mask with an as received canister will be tested 

with a breathing machine with a rate of 24 respirations per minute with a minute 

volume of 40 liters. A breathing cam with a work rate of 622 Kp-m/min. shall be 

used. The gas mask will be challenged with an atmosphere at 25°C, 50 + 5 

percent RH, and 3 ppm of CS. The air exhaled through the gas mask will be 

35°C + 2° with 95 + 3 percent RH. 

 4.5.6. One completely assembled gas mask with a canister preconditioned at 64 lpm 

continuous air flow, 25 percent RH, and approximately 25°C, will be tested with 

a breathing machine with a rate of 24 respirations per minute with a minute 

volume of 40 liters. A breathing cam with a work rate of 622 Kp-m/min. shall be 

used. The gas mask will be challenged with an atmosphere at 25°C, 25 + 5 

percent RH, and 3 ppm of CS. The air exhaled through the gas mask will be 

35°C + 2° with 95 + 3 percent RH. 

4.5.7. One completely assembled gas mask with a canister preconditioned at 64 lpm 

continuous air flow, 85 percent RH, and approximately 25°C, will be tested with 

a breathing machine with a rate of 24 respirations per minute with a minute 

volume of 40 liters. A breathing cam with a work rate of 622 Kp-m/min. shall be 

used. The gas mask will be challenged with an atmosphere at 25°C, 85 + 5 

percent RH, and 3 ppm of CS. The air exhaled through the gas mask will be 

35°C + 2° with 95 + 3 percent RH. 

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.

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 5 of 15 

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, calibration, and maintenance of 

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

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

all tests. 

 5.2. Prepare solutions: 

 5.2.1. Prepare solvent solution of 20 methylene chloride in hexane. Add 100 ml 

methylene chloride to a 500 ml volumetric flask. Dilute to mark with hexanes. 

 5.2.2. CS stock solution 400 ug/ml: accurately weigh approximately 20 mg CS. 

Record exact weight. Dissolve in 10 ml of 20 methylene chloride in hexane 

solvent solution. Add to a 50 ml volumetric flask and fill to mark with solvent. 

Determine exact CS ug/ml stock solution and record. 

 5.2.3. Example: If 0.0264 g of CS is used for the stock solution. 

0.0264 g = 26400 ug therefore 26400 ug = 528.0 ug/ml 

 50 ml 

528.0 ug/ml = 0.528 ug/ul of CS stock solution 

 5.3. Prepare standards: 

 5.3.1. Prepare a group of standards by adding 20, 40, 50, 100, 200, and 400 ul aliquots 

of stock solution to 10 ml volumetric flasks and dilute to mark with solvent. 

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

 5.5. Turn on UV Spectrophotometer and set wave length to 305 nm and allow to warm up. 

 5.6. Measure the absorbance of the standards using the 20 percent methylene chloride in 

hexane solution as the zero absorbance. Check zero absorbance before each 

concentration sample and reset if strayed. 

 5.6.1. Example: 20 ul aliquot standard. 

20 ul x 0.528 ug/ul CS stock solution = 10.56 ug of total CS in 10 ml or 5.28 

ug/5 ml. 

 5.7. Plot the concentration of each standard as ug/5 ml vs. absorbance. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 6 of 15 

5.7.1. Example: The absorbance reading of the 20 ul standard is plotted against the 

standard concentration of 5.28 ug/5 ml. 

5.8. Determine desorption coefficient: 

 5.8.1. Add 75 mg Tenax-GC to three 15 ml screw cap vials. Add 25 ul of stock 

solution to the resin and let stand overnight. (This result will be ug recovered.) 

 5.8.2. Add 75 mg Tenax-GC to three 15 ml screw cap vials. Prepare three blanks by 

adding 25 ul. of solvent to the resin and let stand overnight. (This result will be 

ug blank) 

 5.8.3. Next morning add 5 ml solvent to each vial and swirl to thoroughly wet the 

contents. Let the samples stand for approximately 10 minutes with occasional 

mixing. Zero the UV spectrophotometer, using the solvent as the zero sample. 

 5.8.4. Using a 5 ml syringe with an Acrodisc filter attached, withdraw the samples from 

the vials and put the filtrate in the UV sample cell. Measure and average the 

absorbance of the three stock vials. Measure and average the absorbance of the 

three blank vials. 

 5.8.5. Determine the ug/5 ml reading of the averages from the calibration chart and 

calculate and record the desorption coefficient as follows: 

 Desorption Coefficient = ug recovered - ug blank

 ug added 

Where ug added = % stock solution in ug/ml x 25 ul

1000 

 5.9. Turn on Miller Nelson System and set up CS generation system and let warm up. 

 5.10. Prior to actual gas testing, a zero blank sample of a canister or cartridge needs to be 

collected for comparison of breakthrough values. Mount a canister or cartridge onto a 

test fixture and place in a clean test chamber. Allow clean 64 lpm air to enter the 

canister/cartridge. Attach the Tenax sample tube to a sample line connected to the Gil 

Air pump and sample at 1 lpm for 30 minutes in the airstream exiting the canister/ 

cartridge. Seal both ends after sampling and set aside. This sample will be used as the 

zero blank. 

 5.11. Working in a well ventilated hood, cover the bottom of a 600 ml beaker with CS. Cover 

the top of the beaker with aluminum foil held in place with a rubber band. Punch a 1⁄2" 

hole in the aluminum foil and place the beaker on the hot plate inside the generator. (CS 

will need to be added at intervals during testing to maintain test concentration.) Seal and 

lock the lid. Turn on heater. 

 5.12. Determine test concentration in air: (this must be done at regular intervals during testing 

to monitor the test concentration.) Mount a concentration canister/cartridge onto the lid. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 7 of 15 

This will be used to establish the concentration prior to testing of the actual test canister/ 

cartridge by determining the heat setting that is needed to produce approximately a 

3 ppm CS concentration. 

 5.12.1. Pull a 1liter test concentration sample through the sampling tube. Seal the 

sample tube until ready to analyze. 

 5.12.2. Using a small file, score and cut the tube keeping the sections intact. Remove the 

glass wool plug and discard. Do not add the plugs to the vial. Add the Tenax 

resin from the front section to a 15 ml vial. Mark vials “front section sample”. 

 5.12.3. Remove the middle plug from the tube and discard. Add the resin from the back 

section to a different vial. Mark vial “Back Section Sample”. 

 5.12.4. Add 5 ml solvent to both vials and gently swirl to thoroughly wet the contents. 

Let the samples stand for approximately 10 minutes with occasional swirling. 

 5.12.5. Withdraw the solution from each vial using separate 5 ml syringes with an 

attached Acrodisc filter attached for each vial. Then add the filtrate from each 

vial to a UV cell and measure the absorbance vs. the solvent blank. The solvent 

blank is redetermined just prior to each absorbance measurement. 

 5.13. Determine the weight from the calibration chart and calculate the concentration as 

follows: 

 ug sample = ug front + ug back 

 Corrected ug sample = ug sample 

 Desorption coefficient 

 Concentration in mg/m3 = Corrected ug sample 

 Sample volume in liters 

 5.14. Once the test concentration has been established, testing may begin on the actual test, 

cartridge or canister. Turn off heater and air flow and remove the lid. Remove and 

discard the concentration canister/cartridge in sealed bag. 

 5.15. Weigh a new canister/cartridge and record the weight. 

 5.16. Take inhalation and exhalation resistances of the canister/cartridge mounted on the 

facepiece at 85 lpm. 

 5.17. Replace the concentration canister/cartridge with the test canister or cartridge, and lock 

into place. Turn on air and adjust the heater to the predetermined setting. 

 5.18. Take a 30 liter sample of the effluent of the canister/cartridge using the sample tubes and 

Gil-Air pump. Several samples must be taken during testing to determine breakthrough. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 8 of 15 

 5.19. Analyze the sample following steps 5.12.1 through 5.13 using the 30 liter clean air 

sample from step 5.10 as the zero blank. Replace the zero blank sample to the vial and 

save for further breakthrough comparisons. 

 5.20. When the concentration of the effluent of the canister/cartridge reaches 0.05 ppm or the 

service life exceeds 480 minutes, the test is stopped. 

 5.21. Turn off hot plate. 

 5.22. Turn off air. 

 5.23. Remove test canister/cartridge and place in plastic bag and weigh. Adjust for weight of 

the plastic bag. 

5.24. Turn off Miller Nelson System. 

6. PASS/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; 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. 

 84.110 Gas masks; description. 

(a) Gas masks including all completely assembled air purifying masks designed for use as 

respiratory protection during entry into atmospheres not immediately dangerous to life or 

health or escape only from hazardous atmospheres containing adequate oxygen to support 

life are described as follows: 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 9 of 15 

(1) Front-mounted or back-mounted gas mask. A gas mask which consists of a full 

facepiece, a breathing tube, a canister at the front or back, a canister harness, and 

associated connections. 

(2) Chin-style gas mask. A gas mask which consists of a full facepiece, a canister which 

is usually attached to the facepiece, and associated connections. 

(3) Escape gas mask. A gas mask designed for use during escape only from hazardous 

atmospheres which consists of a facepiece or mouthpiece, a canister, and associated 

connections. 

(b) Gas masks shall be further described according to the types of gases or vapors against 

which they are designed to provide respiratory protection, as follows: 

 Type of front-mounted or back-mounted gas mask:

 Acid gas1 2 3

 Ammonia 

 Carbon monoxide 

 Organic Vapor 1 2 3

 Other gas(es) and vapor(s) 1 2 3

 Combination of two or more of the above gases and vapors.1 2 3

 Combination of acid gas, ammonia, carbon monoxide, and organic vapors.1 2 3 

 Type of chin-style gas mask:

 Acid gas 1 2 3

 Ammonia 

 Carbon monoxide 

 Organic vapor 1 2 3 

 Other gas(es) and vapor(s) 1 2 3 

 Combination of two or more of the above gases and vapors.1 2 3

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 10 of 15 

 Type of escape gas mask: 

 Acid gas 1 2 3 4

 Ammonia 4

 

 Carbon monoxide 

 Organic vapor 1 2 3 4

 Other gas(s) and vapor(s) 1 2 3 4 

 Combination of two or more of the above gases and vapors.1 2 3 4

-------------------------------------------------- 

1

 Approval may be for acid gases or organic vapors as a class or for specific acid gases or organic vapors. 

2

 Not for use against gases or vapors with poor warning properties (except where MSHA or Occupational 

Safety and Health Administration standards permit such use for a specific gas or vapor), or those which 

generate high heats or reaction with sorbent materials in the canister. 

3

 Use of the gas mask may be limited by factors such as lower explosive limit, toxicological effects,and 

facepiece fit. Limitations on gas mask service life and sorbent capacity limitations shall be specified by 

the applicant in instructions for selection, use and maintenance of the gas mask. 

4

 Eye protection may be required in certain concentrations of gases and vapors. 

(c) Gas masks for respiratory protection against gases and vapors other than those 

specified in paragraph (b) of this section, may be approved upon submittal of an 

application in writing for approval to the Certification and Quality Assurance Branch 

listing the gas or vapor and suggested maximum use concentration for the specific type of 

gas mask. The Institute will consider the application and accept or reject it on the basis 

of effect on the wearer's health and safety and any field experience in use of gas masks 

for such exposures. If the application is accepted, the Institute will test such masks in 

accordance with the requirements of this subpart. 

7. RECORDS/TEST SHEETS

 7.1. All test data will be recorded on the o-CHLOROBENZYLIDENE MALONONITRILE 

(CS) 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. 

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8. ATTACHMENTS

 8.1 Tear gas generator. 

 8.2 Data Sheet. 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 12 of 15 

Tear Gas Generator 

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Procedure No. RCT-APR-STP-0050 Revision: 1.1 Date: 26 July 2005 Page 13 of 15 

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. 

(ppm) RH% lpm Initial Final 

1 

2

3

4

5

6

7

 Overall Results: Pass Fail Comment: 

DATA TABLE Temperature (oC) 

 Test 

 Test 

 Cond. 

 Final 

 Time (min) 

 Leakage 

 (ppm) Dn

stream 

 Upst

ream 

 Corrected 

 Time (min) 

 1 

 2 

 3 

 4 

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 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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Revision History 

Revision Date Reason for Revision 

1.0 19 March 2002 Historic document 

1.1 6 June 2005 Update header and format to reflect lab move from Morgantown, WV 

No changes to method 

 

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