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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: 21 December 2005

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Procedure No. CET-APRS-CBRN-STP-0410

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DETERMINATION OF CBRN FORMALDEHYDE SERVICE-LIFE TEST,

Un o ll AIR-PURIFYING ESCAPE RESPIRATORS


STANDARD TEST PROCEDURE (STP)

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1. PURPOSE

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

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the CBRN Formaldehyde Service Life Test, Air-Purifying Escape Respirators Standard

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

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

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

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

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Full- Facepiece Air- Purifying Escape Respirator (APER) Dated September 30, 2003.

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2.
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GENERAL

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c o C o
This STP describes the Determination of CBRN Formaldehyde Service Life Test, Air-

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Purifying Escape Respirators Standard Test Procedure test in sufficient detail that a

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person knowledgeable in the appropriate technical field can select equipment with the

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

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o n t
the test.

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3.
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EQUIPMENT AND 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

t r o py
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 Lpm +/- 2%), and relative humidity (10-

c o n C
98 +/- 3%) and temperature (20-30 0C +/- 0.3%).

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U n l le
t r o
Approvals:

c o n 1st Level 2nd Level 3rd Level

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Procedure No. CET-APRS-CBRN-STP-0410
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3.1.2. EdgeTech Dew Prime II Hygrometer, Model 2000 or equivalent. A micro-

r o l p y
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. Amersham Biosciences High Precision Pump, Model P-500 with

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reservoir. Flow rate range: l ml / hr to 400 ml / hr ±1.5% of setting.

n t o p y
c o 3.1.4. Interscan Corporation, Model RM-16-2, formaldehyde detector or

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equivalent. See Picture 3. Used for detection of breakthrough

l l e concentration. Detector range: 0 - 1999 ppb, resolution: 1 ppb.

t r o p y
3.1.5. Dry Gas Meter. Must have NIST traceable calibration certificate.

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

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3.1.7. Permeation Tubes of formaldehyde. Used for the calibration of both high

tr o y
and low range formaldehyde detectors.

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3.1.8. Miller Nelson Research, Model SV-2000, Vaporizer system or equivalent.

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Used for vaporizing formaldehyde solution.

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3.1.9. 40 Liter glass jug. Used for mixing of formaldehyde vapor.

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3.1.10. Gilibrator, Primary Standard Airflow Calibrator or equivalent.

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

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3.1.12. Graduated impinger, 25ml.

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3.1.13. Para-formaldehyde, purified grade.

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3.1.14. Sodium Thiosulfate (granular) or 0.1N certified sodium thiosulfate
solution.

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3.1.15. Starch, Soluble Potato, Powder.

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3.1.16. Iodine, 0.1N certified solution.

U r o l
3.1.17. Sodium Bisulfite, granular.

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3.1.18. Sodium Carbonate, anhydrous powder.

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Procedure No. CET-APRS-CBRN-STP-0410
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3.1.19. Glacial acetic acid.

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3.1.20. Heated magnetic stirrer and stir bar.

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3.2 Test fixture for mounting canister.

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

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Un 3.4.
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Resistance tester consisting of a vacuum source capable of delivering 85 liters per

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minute, a 6-inch water column slant manometer and a 29/42 female ground glass

t r ojoint.

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4. TESTING REQUIREMENTS AND CONDITIONS

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U n 4.1
l le
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

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

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Respirators (APER) 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

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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 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

n t r
from the institute.

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

U n le
accordance with laboratory procedures and NIOSH/NPPTL guidance. Sound

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

n t r
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

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tolerance can be higher but not lower.
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Procedure No. CET-APRS-CBRN-STP-0410
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4.5 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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Normal laboratory safety practices must be observed. This includes safety

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precautions described in the current NIOSH Pittsburgh Health and Safety

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Program.

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

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

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equipment.

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4.6.3e When handling any glass laboratory equipment, lab technicians and

t r o p y
personnel must wear special gloves, which protect against lacerations or

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punctures.

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U n
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

tr o y
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 maintenance
manuals.

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5.1
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Prepare solutions (must be made at least 24 hours in advance)

c l e
Un 5.1.1

r o l
12.5 % Paraformaldehyde solution: In a 2000 ml beaker containing 1000

t y
ml distilled water and a stirring bar, add 125 g paraformaldehyde. Stir and

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heat the solution to 80EC using the heated magnetic stirrer. Place a watch

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glass over the top of the beaker or cover with aluminum foil to prevent

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excessive water loss. Continue stirring and heating until the solution

l e
clarifies (about 24 hours). Filter the solution if not clear after 24 hours.

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Store in covered bottle or flask.

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5.2. Follow the individual instruction manuals for set up and maintenance of

n c o d
equipment used in this procedure prior to beginning testing. Malfunctioning

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

U o l
starting all tests.

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5.3.
n t
After the manufacturer's specified warm-up period, calibrate the formaldehyde

o
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analyzers using a Kin-Tec generator and permeation tubes to generate

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approximately 1 ppm.
Procedure No. CET-APRS-CBRN-STP-0410
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5.4.

o yle
Set the high precision pump for delivery of calculated formaldehyde to obtain 250

t r p
ppm for a general test category or 500 ppm for a specific test category at the

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testing airflow. See appendix 8.2.

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5.5. Set up test equipment as shown in Figure 1 or Figure 2 depending on the test

r o l
parameters in section 6.3.

n t 5.5.1
p y
For section 6.3.2 test: The airflow is controlled by the Mass Flow

o
c o Controller. Humidity and temperature readings are monitored by a Dew

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Point Hygrometer. The sample pickup for the hygrometer is place into the

l l eair stream via a tee after the Miller Nelson and before the introduction
point of challenge agent. The thermocouple for the hygrometer is placed in

t r o p y
the challenge gas stream immediately before the test chamber.

o
n
5.5.2 For section 6.3.3 and 6.3.4 tests: The airflow, humidity and temperature

c o d C
are controlled by the Miller Nelson system. The temperature and humidity

U n l le
is monitored a Dew Point Hygrometer. The sample pickup for the
hygrometer is place into the air stream via a tee after the Miller Nelson

tr o y
and before the introduction point of challenge agent. The thermocouple for

o n p
the hygrometer is placed in the challenge gas stream immediately before

o
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the test chamber.

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Un 5.6.
l e
Verify the following equipment is on:

l y
r o
5.6.1

t o p
Air and water (if needed) supplies.

o n 5.6.2
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Miller Nelson Research Flow-Temperature-Humidity Control System.

c l e
Un 5.6.3

r o l
Miller Nelson Research Vaporizer system.

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5.6.4
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Amersham Biosciences High Precision Pump.

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c o C
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5.7 Set the airflow to the required airflow for the test. Verify the airflow from the test

l e
fixture using the appropriate dry test meter.

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5.8
r o py
Establish the correct humidity and temperature depending on the test parameters

t o
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in section 6.3.

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5.8.1 Fill pump reservoir with distilled H2O. Insert needle from pump to top of

U o l
column. Start the high precision pump flow using the calculated value

r
from section 5.3. Allow 15 minutes for equalization system. Make sure

o n t
distilled H2O is delivered to the heated vaporizing element.

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5.8.2 Determine the humidity readings for distilled H2O.
Procedure No. CET-APRS-CBRN-STP-0410
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o l 5.8.2.1
y le
For section 6.3.2, the humidity value should be reading

t r o p according to the specification required (25 % ± 5%). If the

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humidity readings are not with in the specification, make

o d
adjustments to the incoming compressed air or the room

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temperature to establish the specification.

r o l 5.8.2.2 For section 6.3.3 and 6.3.4, the humidity readings can be

n t o p y adjusted using the Miller Nelson Controller to the specification

c o C
required (50 % ± 5% or 80% ± 5%).

Un 5.9
l e d
Fill pump reservoir with 12.5 % paraformaldehyde solution, weigh and record

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weight of the reservoir. Insert needle from pump to top of column. Start the high

t r o p y
precision pump flow. Allow 30-40 minutes for equalization of concentration.

o
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Make sure formaldehyde is delivered to the heated vaporizing element.

c o d C
U n
5.10
le
Weigh and record initial weight of the test canister on Test Data Sheet.

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5.11

tr o y
Take initial inhalation and exhalation resistances of the canister mounted on the

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

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C
Record the values on Test Data Sheet.

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Un 5.12
l e
Make sure diverter valve in the system is diverting the challenge concentration

l y
airflow to discharge and not into the testing chamber.

t r o o p
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5.13 Mount canister onto test fixture and place in testing chamber.

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5.14 Determine the concentration of the formaldehyde vapor being generated.

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5.14.1 Add 10 ml 1% sodium bisulfite solution to two impingers. Connect the

o n p
two impingers together from outlet of one impinger to inlet of second

o
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impinger.

Un 5.14.2
l ed
Attach Gil-Air 3 sampling pump to intake side of the first impinger.

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o y
Connect outlet side of second impinger to Gilibrator. Check 1 Lpm flow

n t r o p
of the pump pulling through the sodium bisulfite solution. This setting

C
will be used to sample the formaldehyde concentration. Remove outlet

n c o d
side from Gilibrator.

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U 5.14.3
o l l
Connect tubing from the sample side of the first impinger into the Gil-

n t r
Air pump and tubing from the inlet side of the second impinger to the
test concentration.

c o
Un
5.14.4 Turn on sampling pump and sample for 30 minutes at 1 Lpm.
Procedure No. CET-APRS-CBRN-STP-0410
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Shut off sampling pump and transfer the contents of the two impingers

t r p
into an Erlenmeyer flask. Rinse the impinger stem and body and transfer

o
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the washings to the flask.

c o l e d
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5.14.6 Place a stir bar in the flask and place the flask on the magnetic stirrer.

r o l Begin stirring.

n t 5.14.7
p y
Add 1 ml starch solution.

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c o C
Un d
5.14.8 Add 0.1N Iodine dropwise until solution is dark blue.

l l e
5.14.9 Add 0.1N sodium thiosulfate dropwise until blue color is gone indicating

t r o p y
neutralization of the excess iodine.

o
c o n d C
5.14.10 Slowly add 0.01N iodine dropwise from a 50 ml buret until the first

U n l le
appearance of a faint blue color.

tr o y
5.14.11 Add 25 ml sodium carbonate buffer solution. The blue color should

o n p
disappear if formaldehyde is present.

o
c d C
Un
5.14.12 Record the initial buret reading of the 0.01N Iodine.

l l e
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5.14.13 Slowly add the 0.01N Iodine until the appearance of a faint blue color.

t r o o p
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5.14.14 Record the final buret reading.

c o l e d
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5.14.15 Calculate the concentration of formaldehyde using the formula in

r o l
Attachments 8.3. Adjust the flow from the high precision pump and

t y
repeat steps 5.12 through 5.26 if concentration of 500 ppm ± 10% is not

o n p
obtained. If the concentration if correct attach sample line from high

o
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range detector to the tee in the system. This detector will be used to

Un d
monitor the challenge concentration throughout the length of the test.

l e
Turn on the strip chart recorder to record the concentration.

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t r o py
5.14.16 Once the formaldehyde concentration has been established, testing may

o
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begin.

n c o e d
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5.14.17 Direct challenge concentration airflow into test chamber.

U r o l
5.14.18 Start timer. Airflow out of the fixture is directed into the breakthrough

o n t
detector. Monitor and record the upstream and downstream
temperatures of the air stream throughout testing.
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Procedure No. CET-APRS-CBRN-STP-0410
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5.14.19 Run test until breakthrough of 10 ppm is observed or minimum service

r o l p y
life is surpassed. Record this data on the test data sheet.

n t C o
5.14.20 Weigh and record on the test data sheet the final weight of test canister.

c o l e d
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5.14.21 Repeat steps 5.7 through 5.20 for each test described in section 6.3.

r o l
5.14.22 Turn off pump and heating mantel.

n t o p y
c o 5.14.23 Allow clean air to purge through system for 10-15 minutes.

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Un
6.
l e d
PASS OR FAIL CRITERIA

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6.1.

t r o p y
The criterion for passing this test is set forth in 42 CFR Part 84, Subpart G,

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

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

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tr o y
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

l e
through L of this part.

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

o n t C
of this part, the Institute reserves the right to require, as a further condition

d
of approval, any additional requirements deemed necessary to establish the

c l e
Un
quality, effectiveness, and safety of any respirator used as protection against

o l
hazardous atmospheres.

r
n
(d)
t p y
Where it is determined after receipt of an application that additional

o
c o C
requirements will be required for approval, the Institute will notify the

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applicant in writing of these additional requirements, and necessary

l e
examinations, inspections, or tests, stating generally the reasons for such

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o y
requirements, examinations, inspections, or tests.

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6.3. FORMALDEHYDE BENCH TEST FOR CANISTERS.

n c o e d
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6.3.1. General Category Standard.

U r o l
6.3.1.1. Resistance to airflow of both canister and system will be taken

o n t before and after each test.

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6.3.1.2. Three canisters will be tested at 64 Lpm, continuous air flow, 25
Procedure No. CET-APRS-CBRN-STP-0410
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% ± 5 % relative humidity (RH), 25 oC ± 5 oC and 250 ppm

r o l p y
formaldehyde. Minimum service life will be 15, 30, 45, 60 or 90
minutes as per manufacturer request.

n t C o
o d
6.3.1.3. Three canisters will be tested at 64 Lpm, continuous air flow, 80

c l e % ± 5 % relative humidity (RH), 25 oC ± 5 oC and 250 ppm

Un o l formaldehyde. Minimum service life will be 15, 30, 45, 60 or 90

r
minutes as per manufacturer request.

n t o p y
c o 6.3.1.4. Three canisters will be tested at 100 Lpm, continuous air flow,

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Un
50 % ± 5 % relative humidity (RH), 25 oC ± 5 oC and 250 ppm

l e d formaldehyde. Minimum service life for all canisters must be 5

r o l minutes.

p y
o n t o
6.3.1.5. End of service life concentration is 10 ppm formaldehyde.

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nc le d
6.3.2. Specific Category Standard.

U r o l
y
6.3.2.1. Resistance to airflow of both canister and system will be taken

o n t p
before and after each test.

o
c d C
Un
6.3.2.2. Three canisters will be tested at 64 Lpm, continuous air flow, 25

l l e % ± 5 % relative humidity (RH), 25 oC ± 5 oC and 500 ppm

y
formaldehyde. Minimum service life will be 15, 30, 45, 60 or 90

t r o o p
minutes as per manufacturer request.

o n d C
6.3.2.3. Three canisters will be tested at 64 Lpm, continuous air flow, 80

c l e
Un
% ± 5 % relative humidity (RH), 25 oC ± 5 oC and 500 ppm

r o l formaldehyde. Minimum service life will be 15, 30, 45, 60 or 90

t y
minutes as per manufacturer request.

o n o p
c C
6.3.2.4. Three canisters will be tested at 100 Lpm, continuous air flow,

Un d
50 % ± 5 % relative humidity (RH), 25 oC ± 5 oC and 500 ppm

l l eformaldehyde. Minimum service life for all canisters must be 5

o y
minutes.

n t r o p
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6.3.2.5. End of service life concentration is 10 ppm formaldehyde.

n c o e d
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7. RECORDS AND TEST SHEETS

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7.1.
r o l
All test data will be recorded on the FORMALDEHYDE SERVICE-LIFE test

n t
data sheet.

o
c
Un
7.2. All videotapes and photographs of the actual test being performed, or of the tested
Procedure No. CET-APRS-CBRN-STP-0410
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equipment shall be maintained in the task file as part of the permanent record.

r o l
7.3.
p y
All equipment failing any portion of this test will be handled as follows:

n t C o
o d
7.3.1. If the failure occurs on a new certification application, or extension of

c l e
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approval application, send a test report to the CET Leader and prepare the

r o l hardware for return to the manufacturer.

n t p y
7.3.2. If the failure occurs on hardware examined under an Off-the-Shelf Audit

o
c o the hardware will be examined by a technician and the CET Team Leader

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Un d
for cause. All equipment failing any portion of this test may be sent to the

l l e manufacturer for examination and then returned to NIOSH. However, the


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

t r o p y
release by the RCT Leader, or his designee, following the standard

o
n
operating procedures outlined in Procedure for Scheduling, and Processing

c o d C
Post-Certification Product Audits,

U n l le
RB-SOP-0005-00.

8.
r o
ATTACHMENTS

t y
o n o p
C
8.1 Figure 1- Bench Top Set-Up.

c d
Un 8.2
l e
Calculations for formaldehyde delivery.

l y
8.3
r o
Data Sheet.

t o p
o
8.4
n d C
Qualitative analysis and calculations for determining concentration of challenge

c l e
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formaldehyde vapor.

r o l
n t o p y
c o C
Un l l ed
t r o o py
c o n d C
U n l le
t r o
c o n
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Procedure No. CET-APRS-CBRN-STP-0410
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Attachments 8.2: Calculations for formaldehyde delivery

r o l p y
Calculations for formaldehyde concentration.

n t C o
o d
1 ppm = 1.23 mg / m3

c l e
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Airflow (L/hr) = Airflow (L / min) x 60 min

r o l
Injection rate (ml/hr) = Conc (ppm) X 30 (g / mol) X Airflow (L/hr)

n t o p y 22.4 x 106 X 1.04 g/ml X 12.5%

c o C
Un l l e d
t r o o p y 64 Lpm 100 Lpm

c o n d C
e
250 ppm 10 ml/hr 15 ml/hr

U n o l l 500 ppm 20 ml/hr 30 ml/hr

n tr p y
c o C o
Un l ed
r o l py
n t C o
c o l e d
Un r o l
n t o p y
c o C
Un l l ed
t r o o py
c o n d C
U n l le
t r o
c o n
Un
Procedure No. CET-APRS-CBRN-STP-0410
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Attachment 8.4: Qualitative analysis and calculations for determining concentration of challenge

r o l
formaldehyde vapor

p y
n t o
CALCULATION OF FORMALDEHYDE CONCENTRATION

C
c o l e d
Un l
The formaldehyde equivalent Fe is given by the formula:

t r o y
Fe= ( (N) I ) x 0.15 mg.

o n o p .01

c C
Un d
Where (N) I is the normality of the standardized iodine. This formula is based on the fact that the

l e
equivalent weight of formaldehyde is 15 gm., which means that 1 ml. of 0.01N iodine is

l
equivalent to 0.15 mg. of formaldehyde.

t r o o p y
c o n C
The amount of formaldehyde in the sample volume collected is given by the formula:

d
U n l le Fc = final buret reading - initial buret reading x Femg

tr o y
Fc = total ml. .01 iodine used x 0.15 mg

o n o p
c d C
Un
Formaldehyde concentration in ppm is given by the following formula:

l l e
y
x 103

o
ppm = Fc x 24.45 x 760 x T+273

t r o p V MW P 298

o n Where:
d C
c l e
V = volume of sample collected (30 lpm)

Un l
MW = molecular weight formaldehyde (30.03 g/mole)

tr o
P = pressure in mm of mercury in the lab

y
T = temperature in EC of the lab

o n o p
Assuming that T is equal to 25EC and p is equal to 760 mm mercury, the ppm formula simplifies
to:
c C
Un l ed
HCHO (ppm) = Fc x 27.14 assuming volume of sample collected 30 liters

l
t r o o py
n C
HCHO (ppm) = ml. 0.01 Iodine used x 0.15 mg x 27.14

n c o e d
U o l l
n t r
c o
Un
Procedure No. CET-APRS-CBRN-STP-0410
o p
Revision: 1.1 y Date: 21 December 2005 Page 13 of 13

d C
le
Revision History

r o
Revision l Date
p y Reason for Revision
00

n t C o
21 September 2004 Historic document

o d
1.1 21 December 2005 Update header and format

c l e
Un
No changes to method

r o l
n t o p y
c o C
Un l l e d
t r o o p y
c o n d C
U n l le
tr o y
o n o p
c d C
Un l l e
y
t r o o p
o n d C
c l e
Un r o l
n t o p y
c o C
Un l l ed
t r o o py
c o n d C
U n l le
t r o
c o n
Un

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