Procedure No. RCT-CBRN-STP-0002 Page 1 of 31 

National Institute for Occupational Safety and Health 

National Personal Protective Technology Laboratory 

Respirator Branch 

626 Cochrans Mill Road 

Pittsburgh, Pennsylvania15236 

Date: December 14, 2001. NOTE: The Respirator Branch maintains an updated 

index of current procedures. 

DETERMINATION OF OPEN CIRCUIT, SELF-CONTAINED BREATHING APPARATUS (SCBA) 

PERFORMANCE DURING DYNAMIC TESTING AGAINST CHEMICAL AGENTS 

OF SARIN (GB) VAPOR AND DISTILLED SULFUR MUSTARD (HD) 

VAPOR AND LIQUID STANDARD TESTING PROCEDURE (STP) 

1. PURPOSE 

1.1 This test establishes the procedures for ensuring the level of respiratory protection provided under 

special Chemical, Biological, Radiological, and Nuclear (CBRN) requirements for Open-circuit 

Self-Contained Breathing Apparatus (SCBA) with Full Facepiece submitted for Approval, 

Extension of Approval, or examined during Certification Product Audits, meet the minimum 

certification standards set forth in Title 42 CFR, Part 84, Subpart G, Section 84.63(c). 

1.2 This procedure is used to test SCBA systems against Sarin GB vapor or Distilled Sulfur Mustard 

(HD) vapor and/or liquid, while the mask is operated in dynamic mode by means of a breather 

pump connected to the mouth area of the manikin. The mask is installed on a head/upper torso 

form known as a Simulant Agent Resistant Test Manikin (SMARTMAN). The SMARTMAN is 

enclosed in an air-tight exposure chamber. Instrumentation is integrated under one static chamber 

platform capable of generating and controlling challenge concentrations and detecting precise 

agent permeation of a tested respirator. Sampling ports, associated detection systems and 

exhalation engineering controls in the SMARTMAN are used to detect the presence of agent at 

known sampling areas of the eye and oral/nasal regions. 

2. GENERAL 

The STP describes a test entitled “ Determination of Open Circuit Self-Contained Breathing 

Apparatus (SCBA) Performance During Dynamic Testing Against Chemical Agents (GB and 

HD)” 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 

3.1. List of necessary test equipment follows: 

3.1.1. Head/upper torso form, SMARTMAN, or equivalent, (see picture 1). The 

SMARTMAN is made of cast zinc, hollow shell, and comprises the head, neck, 
Procedure No. RCT-CRBN-STP-0002 Page 2 of 31 

shoulders, and upper chest. The SMARTMAN is manufactured by ILC Dover, 

Frederica, DE. The head features a medium-size anatomically correct surface 

consisting of dimensional eyes, nose, ears, mouth orifice, and chin. The facial 

features are on a movable section of the head to facilitate installing and removing 

a peripheral seal, which is made of rubber and fits into a channel between the 

face and the permanent part of the head. The seal is inflated to press against the 

inside of the facepiece seal area to assure against leakage. The surface of the 

face of the SMARTMAN is connected in several places to outside sampling ports 

by means of stainless steel tubing that is located inside the form and passes out 

the bottom. The largest tube, about 1 1/4” diameter, leads from the mouth area to 

the breather pump. One tube connects to the center of the left eye and is 

generally used to monitor the upper, or eye, area of the interior of the mask. One 

tube connects to the lower middle forehead above the bridge of the nose, and can 

be used to monitor pressure, or differential pressure when connected by means of 

a manometer to the nose area. There are two metal tubes protruding outward 

from the oral/nasal region; one can be used to measure differential pressure, 

while the second one is used to monitor presence of agent. The four tubes are 1⁄4” 

diameter. The SMARTMAN is mounted and sealed to the floor of an exposure 

chamber, which is raised by four legs to allow the tubing to exit and connect to 

the external monitoring devices. A large channel is molded at the bottom of the 

SMARTMAN to allow the anchoring of respirator system shrouds as they are 

intended per manufacturer instructions. 

Picture 1: Head/Upper Torso Manikin, SMARTMAN 

3.1.2. Leak detector Model TDA-99M, or equivalent, (see picture 2). The TDA-99M is 

manufactured by Air Techniques, Inc. The TDA-99M is one of the primary 

technician tools for accessing leaks in the mechanical seals of the respirator and 

fitting the face piece to the SMARTMAN prior to actual introduction of agent. 

The TDA-99M is used to confirm the proper facepiece seal and integrity of the 

respirator after it has been mounted on the SMARTMAN. The device generates 

a mineral oil (Brand Name-“Emery 3004”) aerosol that is used to detect leakage 

into the interior of the respirator. With the respirator properly installed on the 
 

Procedure No. RCT-CBRN-STP-0002 Page 3 of 31 

SMARTMAN and the breather pump operating at manufacturer specifications, 

the TDA-99M generates a liquid particulate aerosol at a concentration of 

100mg/m3 Aerosol is introduced into the agent exposure chamber. The interior of 

the mounted SMARTMAN mask is monitored for presence of the aerosol. The 

leak detector compares the concentration of aerosol inside with the concentration 

outside, and calculates a percent penetration. 

Picture 2: Leak detector Model TDA-99M 

3.13 Miniature Continuous Air Monitoring System, (MINICAMS) (or 

equivalent)(Picture 3). The MINICAMS, manufactured by OI Analytical, is a 

gas chromatograph equipped with a hydrogen flame emission detector and a 

preconcentrator tube. The preconcentrator tube is a small tube containing an 

adsorbent material to scrub out agent vapor contained in a sample of air drawn 

through it for a set time period. The tube is then heated to desorb the agent and 

introduce it into the column and subsequently the detector. By preconcentrating 

the agent, the detection limit is lowered. The MINICAMS unique software 

calculates the amount of agent detected over a specified period of time. The 

Limit of Detection (LOD) is equal to 20% of the TWA. Residual contamination 

is the amount of challenge agent lingering in the breathing zone of the respirator 

when a new, clean unit is mounted on the SMARTMAN. Residual 

contamination is quantified at the beginning of each test / evaluation, the 

detection instrumentation must remain stable for a period of 30 minutes prior to 

the initiation of any test / evaluation. 
 

Procedure No. RCT-CRBN-STP-0002 Page 4 of 31 

Picture 3: Miniature Continuous Air Monitoring System, (MINICAMS) 

3.1.4. Syringe pump, Sage Model M365 or equivalent (Picture 4). This multirange, 

variable rate infusion pump is used to inject liquid agent at a controlled rate into 

an air stream to generate a vapor challenge. The challenge concentration can be 

varied over a wide range to accommodate the requirements. The liquid agent is 

contained in a syringe connected by a flexible cannula (a small tube for insertion 

into a body cavity or into a duct or vessel) to the dilution airline. The plunger of 

the syringe is driven at a controlled rate by the pump to deliver a constant flow of 

agent. The concentration of agent is adjusted by changing the speed setting of 

the pump. (Rate Flow Range = 20.0 ml /min. – 0.3 ml/hr, Flow Accuracy = +/­

5% Nominal) 

Picture 4: Syringe pump, Sage Model M365 
Procedure No. RCT-CBRN-STP-0002 Page 5 of 31 

3.1.5. Flow-Temperature-Humidity Control System or equivalent (see picture 5). This 

system, referred to as the Miller-Nelson (MN) control system, manufactured by 

Miller-Nelson Research, Inc., is 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, and the unit output is air of the 

required volume/flow (200-50 L/min.+/- 2%), and relative humidity (20-80 +/- 

3%) and temperature (20-30 0

C +/- 0.3%). 

Picture 5: Flow-Temperature-Humidity Control System 

3.1.6.	 Exposure Chamber, or equivalent, (Picture 6). The exposure chamber is 

constructed of clear, chemical resistant sheets (Plexiglas ® or Lexan). The floor 

is thicker than the sides and top in order to support the weight of the 

SMARTMAN, which weighs approximately 85 pounds. The front panel is 

removable, and is held in place with clamps on each edge. The dimensions are 

approximately 2 ft. cubed. There are four Plexiglas legs attached to the bottom to 

hold the chamber above the floor of the hood and allow room for the tubing and 

the face adjustment handle. A M12A1 military air purifying collective filter is 

installed on top of the chamber to filter the air that passes out of the chamber. 

There are ports in the sides to accommodate tubing for the challenge 

concentration and clean purge air. An electric fan is installed near the top front to 

achieve a well-mixed challenge concentration. A “Clean Exposure Chamber” is a 

unit used to perform a fit and leak check on a test unit (no agents used in this 

chamber) before it is installed in the agent exposure chamber. 
 

Procedure No. RCT-CRBN-STP-0002 Page 6 of 31 

Picture 6: Exposure Chamber 

3.1.7.	 Mixing Chamber, or equivalent, (Picture 7). This chamber is fabricated of PVC 

pipe, with caps on both ends and three baffles fixed inside to ensure mixing of 

agent vapor and air. A pressure gauge, mounted on the chamber, indicates 

internal mixture pressure and serves as a safety pressure indicator. Maximum 

pressure is indicated per manufacturer pressure gauge instructions and markings. 

Picture 7: Mixing chamber 

3.1.8. Breather Pump, manufactured by Jaeco Fluid Systems, Inc., Model E1R1, or 

equivalent. (Picture 8). This is the standard United States Army breather pump 

used to simulate a person’s breathing for testing of filters and other items. It is a 
 

Procedure No. RCT-CBRN-STP-0002 Page 7 of 31 

double pump, operated by a single electric motor. The original pump was 

modified by substituting a variable speed motor for the single speed motor, thus 

allowing the number of strokes per minute to be varied. The pump controls a 

gearbox with a Scotch Yoke that produces the sinusoidal breathing pattern. . The 

sinusoidal pattern starts at zero flow rate, rises to a maximum, or peak, flow of 

approximately π (3.1416) times the rated flow rate in liters per minute, and drops 

back to zero. The exhalation stroke of the pump follows the same sinusoidal 

pattern. The tidal volume (volume per breath) can be adjusted up to 1.5 liters. 

Picture 8: Breather Pump 

3.1.9. Mass Flow Controllers (or equivalent). Manufactured by Tylan Electronic or 

Brooks Instruments are used to control the flow of sample to the MINICAMS 

and the flow of laboratory air to flush out the exposure chamber when the agent 

challenge is removed. The mass flow controllers are sized to meet the 

requirements. Flows are controlled to +/- 2% of set point. A M-18 (military air 

purifying collective filter) is positioned in-line between the exposure chamber 

and the breathing pump. 

3.1.10. Challenge Detector (GB): A MIRAN (or equivalent) will be used as a detector 

for GB. The MIRAN is an infrared absorption based detector that uses a long 

path length cell up to 20 meters, into which the air sample is introduced. 

Standardization is accomplished by injecting several different concentrations of 

agent and using Lab-View and Excel to calculate the regression. 
 

 

 

 

 

 

Procedure No. RCT-CRBN-STP-0002 Page 8 of 31 

3.1.11.	 Challenge Detector (HD): A gas chromatograph equipped with a flame 

ionization detector (FID) or a MINICAMS equipped with FID (or equivalent) 

will be used to detect Distilled Sulfur Mustard (HD). Standardization is 

accomplished by injecting several different concentrations of agent and using 

Lab-View and Excel to calculate the regression. 

3.1.12.	 Air Compressor & Cascade System: An air-compressed system capable of 

maintaining upper limit of 4500psi and a lower limit of 500psi. The system 

must be capable of simulating the pressure decay curve from full rated tank 

pressure to the point where the low pressure alarm on the SCBA activates. The 

SCBA system should be returned to fully rated tank pressure, continuing the 

process until the test is terminated. The decay cycles may be continuous or 

stepwise. 

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. 

4.2. System Test Conditions 

4.2.1 Breathing Machine 

Airflow = 40 liters per minute 

Respirations = 36 +/- 2 Strokes per minute 

 Tidal Volume = 1.1 liter 

4.2.2 High Pressure Compressed Air Supply, Grade D Compressed Air or Grade E 

Liquified Air (Source for SCBA Operating System) 

Pressure Decay Profile = Rated SCBA Service Pressure to low pressure 

alarm 

Tank capacity = 2400 liters (minimum) 

Temperature = 25+5 0

C 

Oxygen: 19.5 to 23.5% 

CO by Volume: Less than 10ppm 

CO2 by Volume: Less than 1000ppm 

Condensed Hydrocarbons by Weight: Less than 5 mg/m3 

Odor: No Odor Detectable by Olfactory Senses 

Dew Point: Less than –50 degrees F at 1 atmosphere per OSHA 

1910.134 (i) (4) (iii) 

4.2.3 Miller-Nelson air flow into exposure chamber 

 Airflow Rate

 GB airflow = 50 L/min 

 HD airflow = 50 L/min 

Relative Humidity = 25+5% 

Temperature = 25 + 3o

C 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Procedure No. RCT-CBRN-STP-0002 Page 9 of 31 

4.2.4 SMARTMAN Sampling Point 

A single Nasal port to supply dual MINICAM detectors. 

4.2.5 Sarin (GB) Vapor Test 

 Challenge Concentration = 2000 + 10% mg/m3 

Equipment Concentration Upper Limit = 15 ng/200mL 

Challenge Time (disseminator on) = 30 minutes + 10 seconds 

Monitor & Hold Time = 5.5 hours 

Syringe Injection Rate = as required based upon syringe pump used 

Syringe Injected Volume = as required based upon syringe pump used 

4.2.6 Distilled Sulfur Mustard (HD) Liquid and Vapor Test 

4.2.6.1 HD Liquid Application 

Drop Size = 20 microliters 

Total Volume = 0.86 milliliters (43 drops of 20 micro liters) 

Facepiece (Appendix A) = 25 drops 

Associated Hardware (Appendix B) = 18 drops 

Use of an external shroud or hood attached to the facepiece requires 

contamination droplets to be placed on those areas of the shroud 

covering the areas of the depicted facepiece diagram. Droplet 

application on a shroud stresses the same facepiece areas identified for 

the non-shrouded facepiece but instead of applications being on bare 

facepiece material they are on the shroud covering that depicted 

area/seam/joint/interface. 

4.2.6.2 HD Vapor Challenge 

 Challenge Concentration = 300 + 10% mg/m3 

Equipment Concentration Upper Limit = 40 ng/500mL 

Challenge Time (pump on) = 30 minutes + 10 seconds 

Monitor & Hold Time = 5.5 hours 

Syringe Injection Rate = as required based upon syringe pump used 

Syringe Injected Volume = as required based upon syringe pump used 

4.2.7. Test Termination Parameters: The test will be terminated to protect the detectors 

from over-saturation. The termination point should be set at or above the highest 

calibration point. 

4.2.8. Compressed air inlet pressure is rated cylinder pressure per manufacturer 

instructions. Duration of test determines the amount of compressed air required 

to maintain the SCBA at manufacturer operating compressed air specifications. 

Compressed air source provides required high pressure air over the entire 

duration of the test. Maximum air pressure is 4500 psig but may vary depending 

on SCBA air cylinder rating to 3000 psig or 2216/2200psi. Minimum air 

pressure required is 500psi. At the minimum air pressure reading in the tested air 
 

 

Procedure No. RCT-CRBN-STP-0002 Page 10 of 31 

cylinder valve area of the SCBA, initiate airflow from second cylinder and 

isolate first cylinder for recharging. The compressed air cycle continues until the 

end of the specified test. 

4.3 Safety: Normal laboratory safety practices must be observed. This includes all 

safety precautions described in the current Appalachian Laboratory for 

Occupational Safety & Health (ALOSH) Facility Laboratory Safety Manual, U.S. 

Army Soldiers and Biological Chemical Command Laboratory Safety Manual, 

and/or equivalent manuals. 

. 

4.3.1. Safety glasses, lab coats, and assigned respirator must be worn at all times. 

4.3.2. Work surfaces must be maintained, free of clutter and non-essential test 

equipment. 

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

must wear gloves, which protect against lacerations or punctures. 

4.3.4.	 Laboratory personnel must be trained in safe operating procedures appropriate 

for the test. 

4.3.5. Surety lab procedures outlined in applicable SOPs are required to be on hand. 

Annual training classes focus on the familiarization of required occupational 

safety and health subjects in accordance with specified surety lab procedures. 

4.3.6.	 Please refer to Material Safety Data Sheets and appropriate Health and Safety 

manuals, or other appropriate documentation for the proper protection and care in 

handling, storing, and disposing of the chemicals and gases used in this 

procedure.

 4.4. MINICAMS 

4.4.1 A Laboratory MINICAMS is used as the detector for agent 

penetration/permeation of the SCBA. It consists of a monitor, PC computer, 

Stream Selection System, Linear Mass Flowmeter and optional printer or 

recorder. 

4.4.2. A small volume of air is drawn through a preconcentrator tube containing an 

adsorbent material: GB sample volume is approximately 200 ml/min and HD 

sample volume is approximately 500 ml/min. Agent in the sample is adsorbed on 

the material. Later in the cycle the tube is heated to desorb the agent, which then 

flows through a gas chromatograph column to a flame emission detector. 

Because the total agent in the sample is detected at one time instead of 

continuously, the detection limit is much lower. The total quantity of agent 

detected is calculated back to the sample volume and is expressed as ng/L. 
 

 

Procedure No. RCT-CBRN-STP-0002 Page 11 of 31 

4.4.3 Operation of the MINICAMS requires the use of compressed air, hydrogen, and 

nitrogen, of a high purity. The operating manual recommends operating 

parameters (temperature, timing, pressures, etc.) and cycle times (3, 5, 10 or 15 

min.), depending on the application. GB analysis requires a 3 minute cycle and 

HD requires a 5 minute cycle. 

4.4.4. The MINICAMS is installed in accordance with the operating manual. The 

appropriate optical filter for GB or HD must be installed in front of the 

photomultiplier tube. In principle, when GB or HD burns in a hydrogen flame, a 

chemical species (phosphorus or sulfur) is formed that emits radiation at a unique 

wavelength. The optical filter isolates the radiation and allows it to pass into the 

photomultiplier tube (PMT), whose output voltage is correlated with the quantity 

of agent burned in the flame. 

4.4.5. Set up the MINICAMS in accordance with operating manual and the method for 

the agent that is being used. In order to quantify the agent in the sample, the 

MINICAMS must be standardized. Standardization is accomplished by injecting 

a small quantity (1.0 or 2.0 uL) of a standard solution of the agent onto the 

preconcentrator tube during the INJECT segment of the test cycle. The standard 

solutions of agent are made in isopropanol or hexane, spectrophotometric grade. 

At least three injections of each quantity of agent should be injected. By pressing 

the F2 key on the keyboard, the data is saved and a standard curve is calculated 

and displayed. 

4.4.6 Pretest activities for the MINICAMS are as follows: 

Start the MINICAMS 

Set or verify operational parameters for appropriate agent 

Perform standardization 

Record ASCII file name on Data Sheet (Appendix A&B) 

Standby for start of testing 

4.5. Agent vapor generator 

4.5.1. The vapor challenge for SMARTMAN testing is generated by injecting the 

required quantity of liquid agent into the volume of air that passes through the 

exposure chamber to give the challenge in mg/m3. This is accomplished by a 

combination of controlled airflow from the Miller- Nelson Air controller and a 

syringe pump for injecting the agent through a heated tee into the air stream. 

Determine the volume of air needed to pass through the exposure chamber per 

minute (flow rate) and the quantity of agent necessary to give the specified 

challenge concentration for this flow rate. From the pump operating manual 

select the syringe size and pump rate that will inject the required amount of agent 

per unit time. Draw up the total amount of agent needed into the syringe, with a 

small excess, connect one end of the cannula (the small flexible tube that is 

inserted into the air duct) to the syringe, and the other end to the heated tee in the 
 

 

 

Procedure No. RCT-CRBN-STP-0002 Page 12 of 31 

air duct. Clamp the barrel of the syringe onto the pump and move the plunger 

drive until it contacts the end of the plunger. Turn on the power to the pump. 

The plunger will be activated and agent will be injected into the air stream as a 

vapor from the heated tee. The mixture passes into the mixing chamber where it 

is thoroughly mixed, ready to be introduced into the exposure chamber for the 

test. 

4.6. Miller-Nelson (MN) Controller 

4.6.1. The Miller Nelson unit receives compressed air from the laboratory air supply 

system. Operate the Miller Nelson according to the manufacturer’s instructions. 

The sensors for relative humidity and temperature must be calibrated, as must be 

the flow controller, since it is important that the total flow through the test system 

be known in order to supply the requisite amount of agent from the syringe 

pump. 

4.6.2. Set the readout panels on the Miller Nelson to approximately 50 L/min. flow (see 

4.2.3) and the 25 +/- 5% relative humidity. The temperature is normally set at 

room temperature, 25 ± 3o

C. Allow the air to flow through the mixing chamber 

and the M18 filter until it is time to start the test. 

4.7. Syringe pump. 

4.7.1. A syringe pump is used to inject liquid agent into the dilution air stream at a 

controlled rate such that the concentration of agent in air is that required for the 

challenge specified for the test. The injection rate must remain constant for the 

entire period. The syringe pump controls allow the pump rate to be changed by 

using a switch. 

4.7.2. Select the size syringe that will hold sufficient agent for the challenge period and 

the total volume of air required. Fill the syringe to the volume determined and 

attach the syringe to the fitting on the flexible cannula. The cannula is normally 

made of plastic with Luer locks on each end. One end of the cannula is attached 

to the heated tee in the dilution airline. Set the syringe in the holder and clamp it 

in place. Move the drive block until it is firmly against the end of the plunger. 

4.7.3. Set the switch on the pump to the setting required for the size syringe and the 

injection rate. Turning on the power switch will start the drive block pushing the 

plunger of the syringe to begin generating the agent challenge concentration. 

4.8.	 TDA-99M Aerosol Leak Detector 

4.8.1.	 The TDA-99M leak detector is used to detect leaks into the SCBA after it has 

been installed on the SMARTMAN headform. Connect the SCBA to the air 

supply system using a cylinder valve mounting fixture. See Appendix E for a 

drawing of the fixture. Because of the length of time, 360 minutes, the SCBA is 

operated using air supplied to the SCBA from a cylinder system. Ensure that 
 

Procedure No. RCT-CBRN-STP-0002 Page 13 of 31 

installation procedures for the SCBA valve follow the manufacturer’s installation 

procedures for torque and that the seal (gasket or O-ring) is a new seal provided 

by the manufacturer. 

4.8.2. Turn on the power and let the detector equilibrate, according to the 

manufacturer’s instructions. The SCBA should be operating. Turn on the 

breather pump to activate the test mask. Connect the detector inlet to a sample 

line from the SMARTMAN. When aerosol is being generated, direct the wand to 

various portions of the facepiece and all mechanical seals or joints to detect any 

leak paths. Any leaks found must be corrected. Insure the SCBA does not go 

into negative pressure. If negative pressure is observed, terminate test and 

recheck/trouble shoot compressed air lines and face seal. If no localized leaks 

are found, replace the front panel of the exposure chamber. 

4.8.3. Connect the TDA-99M to a port into the exposure chamber and fill the chamber 

with aerosols. Maintain a constant aerosol concentration of 100 mg/m3

 inside the 

exposure chamber for 30 minutes. Check the display on the TDA-99M for 

detection of aerosol inside the facepiece. If there is evidence of leakage, attempt 

to find and eliminate the leak. When the detector indicates a maximum percent 

penetration of 0.001% or <0.0010 % assume there is no leak in the facepiece and 

begin the test 

4.9. Quality Control Measures 

4.9.1. SMARTMAN Leak Test: Because the SMARTMAN is made of cast zinc, it is 

possible for leak paths to form through the metal casting to allow agent vapor to 

pass through from the headform cavity into the interior of the mask mounted on 

the headform. Install a peripheral seal on the headform and inflate it. Flood the 

interior of the headform with helium. Use the probe of the helium leak detector 

to check the entire surface and the seal for presence of helium. Any leak found 

must be eliminated. This test is to be performed on each new or reconditioned 

SMARTMAN and monthly on the head-forms when they are in use. 

4.9.2.	 Standardization of Instrumentation: Standardize the MINICAMS by using liquid 

standard solutions of the agents at various concentrations. These solutions are to 

be made in accordance with CAT IOP #214, Preparing Standard Agent Solutions 

for Instrumentation, or equivalent laboratory procedures. A stock solution is the 

primary solution made by weighing a quantity of agent into a volumetric flask 

and diluting to volume. This solution may be used for two weeks, unless 

deterioration is noted before that time. The stock solution is diluted further to 

make a series of standard solutions that are used to standardize the MINICAMS. 

The standard solutions may be used for one week, unless MINICAMS analyses 

indicate that the solutions are deteriorating. Class A glassware must be used for 

all volumetric work. Calibration curves should have a minimum correlation 

value of r2

 = 0.999 for GB and r2 = 0.99 for HD. 
 

Procedure No. RCT-CRBN-STP-0002 Page 14 of 31 

4.9.3.	 Determination of Flows: Since flow rates are used in several aspects of this test, 

it is necessary to use calibrated flow meters to set the flows used in the 

instruments. Flow meters are calibrated by the Army TM&DE and Metrology 

Laboratory, or equivalent using instruments traceable to NIST. Flow meters to 

be checked against calibrated meters are the Miller-Nelson Air Flow Controller, 

electronic flow meters used for the MINICAMS preconcentrator tube and the 

breather flow from the breather pump. 

4.9.4 Leak Testing: SCBA leak testing using the TDA-99M Aerosol Tester is 

performed on the facepiece after installation on the SMARTMAN and while the 

breather pump is operating. With the wand, move the aerosol challenge over all 

parts of the facepiece and test unit. If there is no leak, the display on the TDA99M should read 0.000 % penetration. Do not start a test until a value < 

0.0010% is indicated. 

4.9.5 Detector Response: Check the response of the detector, MINICAMS before and 

after each test. This is done by injecting an aliquot of standard solution that 

contains a known concentration of agent near the mid-range of the standard 

curve. Inject the aliquot into the end of the heated sample line from the oronasal 

sampling port; it is necessary to disconnect the line from the bottom of the 

chamber to do this. This is called a “check shot”. Repeat it at the end of the test 

to assure that the detector has not changed during the test. The response of the 

detector should fall on the standard curve at the value expected for the amount of 

agent in the aliquot, or within 10% of that value. Record results of check shot in 

Laboratory Notebook. If the checkshot does not reproduce a verifiable result, 

repeat the checkshot. If the second checkshot is not within the 10% parameter, 

the test is invalid. 

5. PROCEDURE (Vapor Challenge GB or Liquid/Vapor Challenge HD) 

5.1. Assemble SCBA per manufacturer’s instruction with the exception of the air cylinder and 

connect the compressed air system capable of supplying high pressure breathing air to the 

SCBA Insure air inlet pressure gauge reads the SCBA rated service pressure +/- 50 psig. 

Insure SCBA air pressure gauge reads in the full range. 

5.2.	 Take a digital photograph of assembled unit for use later. 

5.3.	 Mount unit on the SMARTMAN in the “clean” exposure chamber. The facepiece should 

be mounted to the SMARTMAN per the manufacturers’ instructions 

5.4.	 The test SCBA must be connected to the compressed air supply system using a cylinder 

valve mounting fixture. See Appendix E for a drawing of the fixture. Ensure that 

installation procedures for the valve follow the manufacturer’s installation procedures for 

torque and that the seal (gasket or O-ring) is a new seal provided by the manufacturer. . 

Insure inlet pressure gauge does not exceed the SCBA rated service pressure at any time. 
 

 

 

Procedure No. RCT-CBRN-STP-0002 Page 15 of 31 

5.5. Turn on Miller-Nelson and breathing pump. Insure that the SCBA is in the pressure 

demand mode. 

5.6. Using the TDA 99M, leak test the SCBA in the operational pressure demand mode. 

Connect the detector inlet to a sample line from the SMARTMAN. When aerosol is 

being generated, direct the wand to various portions of the facepiece and all mechanical 

seals and joints to detect any leaks. The aerosol will be detected inside the facepiece if it 

finds a leak path. If any leaks are found, they must be corrected. If no localized leaks are 

found, replace the front panel of the exposure chamber. Connect the TDA-99M to a port 

into the exposure chamber and fill the chamber with the aerosol challenge. Maintain 100 

mg/m3

 aerosol challenge inside the chamber for five minutes. Check the display on the 

TDA-99M for detection of aerosol inside the facepiece. If there is evidence of leakage, 

attempt to find and eliminate the leak. When the detector indicates a minimum percent 

penetration of 0.0010, assume there is no leak in the facepiece and begin the test. 

5.7.	 Remove SCBA from “clean” chamber and install on SMARTMAN in the appropriate 

agent exposure chamber. 

5.8.	 Mount unit on the SMARTMAN in the “hot” exposure chamber. Repeat steps 5.3 - 5.5, 

except that once the chamber is sealed and no leaks are confirmed, the aerosol challenge 

is discontinued. 

5.9. Use only one of the nasal sampling ports for facepiece sampling. 

5.10.	 Background Characterization. A background characterization must be run before every 

test run/evaluation. The instrumentation should be monitored for a period of 60 minutes 

prior to the initiation of the test. Confirm that background level is less than the lowest 

point on the MINICAM calibration curve. The background characterization must be 

defined prior to placing the test respirator on the SMARTMAN. 

5.11.	 Set up standard operational mode of test equipment. Ensure all test equipment is within 

calibration. 

5.12.	 Set Miller-Nelson for air flow into exposure chamber set to deliver required rate 

 Airflow Rate

 GB airflow = 50 L/min 

 HD airflow = 50 L/min 

 Relative Humidity = 50+5% 

Temperature = 25 + 3o

C 

5.13.	 Load liquid agent in syringe and set syringe pump to correct flow rate to achieve the 

required agent challenge concentration. See items 4.2.5 (GB) or 4.2.6.2 (HD). 

5.14.	 Ensure MINICAM is calibrated, perform “check shot” and ready for operating mode. 
Procedure No. RCT-CRBN-STP-0002 Page 16 of 31 

5.15. Ensure that the challenge concentration instrument is calibrated and a check shot has 

been performed and it is ready for analysis. Monitor chamber concentration during the 

60 minute Background Characterization period. Characterization readings should reflect 

steady state conditions. 

5.16.	 Time zero or the start of the test is when the chamber concentration reading is above the 

lowest calibration point after drops have been applied to the SCBA and/or vapor is 

introduced into the chamber. 

5.17. Liquid Application of HD droplets: Liquid drops are delivered to the surface of the 

SCBA to test permeation. A total of 43 droplets (size of 20 micro liters each) are 

specified. Placement of the droplets, via syringe on to the system is specified in 

(Appendix A & B). Mark location of actual droplets on a digital photograph of the 

equipment being tested. Photographs must be maintained in the Task Folder. The 

Appendices A& B are schematics for the suggested location of the agent drops. Liquid 

application of HD occurs before the vapor challenge of HD begins. If an external shroud 

is mounted on the facepiece, apply droplets per standard diagram but on surfaces of the 

shroud that mirror the routine faceblank areas. 

5.18.	 Introduce agent challenge [Sarin (GB) or Distilled Sulfur Mustard (HD)] to exposure 

chamber. Turn the valve in the line from by-pass to the mixing chamber to direct flow to 

the exposure chamber. The total flow to the chamber is approximately 50 L/min from 

Miller Nelson, which includes enough excess to make up for the clean air exhausted from 

the mask into the chamber and maintain the constant challenge as required. The 

concentration of challenge agent is calculated on the basis of the mass balance of quantity 

of agent injected and total dilution airflow being introduced into the chamber. The 

syringe flow rate is set to introduce the quantity of agent necessary to generate the 

challenge concentration required. Record when the MINICAMS begin monitoring the 

interior of the mask. It may be required to start the MINICAMS before introducing agent 

into the chamber so that the first sampling period will coincide with the first agent 

challenge. This will indicate whether there is an initial penetration of agent into the mask 

that might not be detected if the first sampling occurs a minute or two after introduction 

of the challenge. 

5.18.1. The syringe pump should run for the prescribed challenge period of 30 minutes + 

10 seconds. At the end of the challenge period, turn off the syringe pump. 

Record the total volume, elapsed time and air flow rate delivered from the MillerNelson. These values will be recorded in the laboratory notebook and test data 

sheets (Appendix C & D). 

5.18.2. The Flame Ionization Detector (FID) with a sample loop connected to a gas 

chromatograph will be used to monitor the challenge concentration in the 

exposure chamber, which will be recorded on the computer at a given time. 

5.19.	 System Hold or Monitor Time 
 

 

Procedure No. RCT-CBRN-STP-0002 Page 17 of 31 

5.19.1. For HD, continue flushing the chamber with the Miller-Nelson, with the 

breathing machine operating at the same rate for 5.5 hours. MINICAMS should 

continue to analyze until Equipment Concentration Upper Limit for the detector 

is reached or the 5.5 hours is elapsed. 

5.19.2. For GB, continue flushing the chamber with the Miller-Nelson, with the 

breathing machine operating at the same rate for 5.5 hours. 

5.20. Test Surveillance 

5.20.1. The technician should monitor the test to make sure all components of the system 

function and collect data as required. 

5.21. Termination of Test 

5.21.1. When the full time for the test has elapsed, terminate the test. Turn off breather 

pump. Depressurize the SCBA by terminating the compressed air feed, purge the 

air from the SCBA by opening the purge valve, and allow air to drain while the 

primary air cylinder valve is open. When gauge reads 0 on SCBA, close purge 

valve and close air cylinder valve. Disconnect SCBA in accordance with local 

lab safety procedures Perform a check shot of agent to assure that the detection 

system is still operating correctly. Take an aliquot of one of the mid-range 

standard solutions of agent with a microliter syringe and inject it into the nasal 

sampling port by disconnecting the line from the bottom of the exposure 

chamber. The MINICAMS response should be that indicated on the standard 

curve for the amount of agent contained in the aliquot. The response must be 

within 10% of the correct value for the test to be valid. 

5.21.2. Turn off the MINICAMS. Turn off Miller-Nelson airflow through the exposure 

chamber. Open the chamber front panel. Remove the test item (separate it into 

components) and double-bag the components. Remove the bagged components 

to the decontamination hood for temporary storage, decontamination, monitoring, 

and disposal. Wipe down the interior of the chamber and the SMARTMAN. 

Dispose of cleaning materials according to local hazardous waste SOP. 

5.21.3. Timeline or Sequence of Activities 

Validate instrumentation and check shot 

Helium Leak check peripheral seals (if applicable) 

Install SCBA in clean exposure chamber 

Challenge SCBA with TDA-99M for 5 minutes 

Install SCBA in exposure chamber 

Challenge SCBA with TDA-99M for 5 minutes 

 Start MINICAMS 

Monitor background behind the mask and chamber concentration 

 Add droplets (HD only)
 
 

Procedure No. RCT-CRBN-STP-0002 Page 18 of 31 

 Close exposure chamber 

Start makeup air using Miller-Nelson 

 Start syringe pump 

 Record Start Time

 Challenge Time (30 minutes) 

 Stop syringe pump 

 Hold Time (5.5 hours) 

End of Test 

Check shoot instrumentation 

5.22. Data Analysis 

5.22.1. Technician is responsible for accurately maintaining a laboratory notebook and 

all required records. Hardcopies of data should be annotated when pertinent 

events occur, such as a checkshot or test start time. Supervisor must pre-approve 

any deviation from standard test method and signoff in technician’s notebook. 

Notebooks should be signed and dated, copies of all hardcopies of data that are 

generated shall be kept in the assigned task folder with NIOSH Task number. 

5.22.2. Technician must complete all required Test Data Sheets (Appendix C & D). 

Originals of all Test Data Sheets must be completed and retained in the task file. 

5.22.3. Transfer the permeation data from the MINICAMS computer into a computer for 

analysis by Microsoft Excel. Display the data on a spreadsheet. Because 

MINICAMS data is formatted on separate pages, there are gaps in the lines of 

data. These gaps must be deleted so that the data are in one continuous table. 

Next, the actual sample data must be separated from the blanks into another 

table. This table will contain data from the nasal area and associated time 

markers. . The resulting table will each have two columns, time and nanograms. 

Convert the nanograms into a concentration, ng/L, by multiplying nanograms by 

a factor obtained by dividing the actual sample volume (typically 200 mL) into 

1000 mL/L (the factor in this case is 5/L. Example: 1.73 ng x 5/L = 8.65 ng/L). 

Using Excel’s Chart Wizard feature, a plot of concentration vs. time can be 

visualized and printed, using all the data in the table. 

Transfer the permeation data; the challenge concentration data, the environmental 

data and the leak check data into a computer for analysis by Microsoft Excel. 

Display the data on a spreadsheet and store a copy of the computer file in with 

the test file. 

Leak Check data: Plot the leak check data versus time with its associated error 

bars. 

Environmental data: Plot the environmental data versus time with its associated 

error bars. 
 

 

 

 

 

 

 

 

 

Procedure No. RCT-CBRN-STP-0002 Page 19 of 31 

Challenge Concentration data: Plot the challenge concentration versus time with 

its associated error bars. Plot the Ct versus time with its associated error bars. 

Permeation data: Plot Permeation concentration data versus time. If 

MINICAMS is collecting the permeation data the following directions apply. 

Because MINICAMS data is formatted on separate pages, there are gaps in the 

lines of data. These gaps must be deleted so that the data are in one continuous 

table. Next, the actual sample data must be separated from the blanks into 

another table. This table will contain data from the nasal area and associated 

time markers. The resulting table will each have two columns, time and 

nanograms. 

To convert nanograms into a concentration, mg/m3

, use this calculation: 

mg mg 103 mL 103 L = Αx xΒx x xΕ 3 6	 3

m 10 ng L m

where: 

Α = Mass Recovered (ng) 

1 Β =

Sample Flow Rate (mL/min) 

1 Ε =

Sample Time (min) 

6. PASS\FAIL CRITERIA 

6.1. The criterion for passing this test is set within the regulatory authority of 42 CFR, Part 

84, Subpart G, Section 84.63(c); Volume 60, Number 110, June 8, 1995. A compound, 

two tier pass/fail criterion must be met. The criterion is: 

6.1.1. Sarin (GB) Penetration Test: 

Challenge: 2000 mg/m3 for 30 minutes 

Test Time: 360 minutes 

 Dual Pass/Fail Criteria: 

a) Maximum agent breakthrough: 2.1 mg-min/m3 (integrated concentration 

 over time or CT) 

b) Maximum Peak Excursions: 0.087 mg/m3: Three consecutive data points at or 

exceeding the peak value constitutes a failure. 

Note: Overall CT limit of 2.1 mg-min/m3

 including peaks cannot be exceeded. 

6.1.2. Distilled Sulfur Mustard (HD) Penetration and Permeation Test: 
 

 

 

 

Procedure No. RCT-CRBN-STP-0002 Page 20 of 31 

Challenge: 300 mg/m3 for 30 minutes plus 43 maximum 20 Fl liquid droplets 

 Test Period: 360 minutes 

 Dual Pass/Fail Criteria: 

a) Maximum agent breakthrough: 6.0 mg-min/m3 (integrated concentration 

 over time or CT) 

b) Maximum Peak Excursions: 0.60 mg/m3 Three consecutive data points at or 

exceeding the peak value constitutes a failure. 

Note: Overall CT limit of 6.0 mg/m3

 including all peaks cannot be exceeded. 

6.1.3 Precision and accuracy must be determined for each instrument. 

6.2. This test establishes the procedures for ensuring the level of respiratory protection 

provided under special Chemical, Biological, Radiological, and Nuclear (CBRN) 

requirements for Open-circuit Self-Contained Breathing Apparatus (SCBA) with Full 

Facepiece submitted for Approval, Extension of Approval, or examined during 

Certification Product Audits, meet the minimum certification standards set forth in Title 

42 CFR, Part 84, Subpart G, Section 84.63(c). 

7. RECORDS\TEST SHEETS 

7.1. All test data will be recorded on the test data sheets (Appendix C & D). GRADE D Air 

quality control certificates are required to be on file for the current compressor output air. 

Grade D air routine maintenance checks and procedures are required to be filed and 

capable of confirming the quality of used Grade D air in support of SCBA certification. 

7.2. All videotapes and photographs of the actual test being performed by SBCCOM/NIOSH 

personnel, or of the test 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 a failure occurs on a new certification application, or extension of approval 

application, SBCCOM will send a test report to the RCT Leader and prepare any 

uncontaminated hardware for return to the manufacturer. 

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

hardware will be examined by SBCCOM technician and the SBCCOM 

Laboratory Manager for cause. All equipment failing or passing any portion of 

this test will be contaminated with chemical warfare agent and will be disposed 

of in accordance with SBCCOM chemical surety practices. 


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