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. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005

DETERMINATION OF FULL-FACEPIECE, TIGHT-FITTING, NEGATIVE-PRESSURE, 

AIR-PURIFYING RESPIRATOR (APR) PERFORMANCE DURING DYNAMIC TESTING 

AGAINST CHEMICAL AGENT DISTILLED SULFUR MUSTARD (HD) 

 VAPOR AND LIQUID CBRN STANDARD TEST PROCEDURE (STP) 

1. PURPOSE

1.1 This document establishes the procedures for ensuring the level of respiratory 

protection provided by chemical, biological, radiological, and nuclear (CBRN) 

protection requirements for full facepiece, tight fitting, negative pressure, P100, 

CBRN Capacity X, air-purifying respirator (APR) 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(a)(c)(d) and Federal Register, Volume 60, Number 110, June 8, 

1995. 

1.2 The purpose of this standard test procedure (STP) is to describe the test conditions 

and procedures necessary to test and certify CBRN APR certification 

applications. A CBRN APR is a complete tight fitting and full face blank, 

properly outfitted with manufacturer unique components and a properly designed 

manufacturer specified APR canister that is installed per the manufacturer’s 

installation requirements outlined in current user instructions. This procedure is 

used to test CBRN APR systems against distilled sulfur mustard (HD) vapor and 

liquid physical states, while the respirator is operated in dynamic mode by means 

of a breather pump connected to the breathing zone of a manikin headform. 

Instrumentation is integrated under this static chamber platform for the purpose of 

generating and controlling challenge concentrations and detecting precise agent 

permeation and penetration of a tested respirator. This procedure is a separate test 

under the NIOSH NPPTL Respirator Branch, Certification, Evaluation and 

Testing Section (CET) heading of CET-APRS-STP-CBRN-0351 for challenge of 

sulfur mustard (HD) vapor and liquid. This procedure is designed to rigorously 

test the evaluated respirator as a dynamic breathing system and generate 

repeatable independent pass or fail results under laboratory conditions.

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2. GENERAL

2.1 This STP describes a test titled “Determination Of Full Facepiece, Tight Fitting, 

Negative Pressure, Air-Purifying Respirator (APR) Performance During Dynamic 

Testing Against Chemical Agent Distilled Sulfur Mustard (HD) Vapor And 

Distilled Sulfur Mustard (HD) Liquid” in sufficient detail that a team of persons 

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 AND MATERIALS

3.1 SMARTMAN®, Headform/Upper Torso or Equivalent (Figure 1). Manufactured 

by ILC Dover, Frederica, Delaware, The Simulant Agent Resistant Test Manikin, 

a.k.a. SMARTMAN®, is a cast zinc, hollow shell headform representing a static 

uniform surface that outlines a medium sized human male head, neck, shoulders 

and upper chest stature. The head features an anatomically correct semi-static 

surface consisting of dimensional eyes, nose, ears, mouth orifice, forehead and 

chin. The features are on a movable section of the head to facilitate installing and 

removing a peripheral front face seal, which is made of silicone 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. A face seal adjustment handle allows standard mechanical pressure to be 

exerted for securing the face seal. 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, 11⁄4′′ in diameter, leads from the mouth area to the breather pump. Four 

 Figure 1. Headform/upper torso manikin, SMARTMAN®. 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 3 of 39 

smaller tubes are present. One tube connects to the center of the left eye; it is 

blocked off. A tube connects to the lower middle forehead above the bridge of the 

nose; it is blocked off. There are two metal tubes protruding outward from the 

oral/nasal region, they are in use. One is used to measure differential pressure by 

means of a magnehelic gauge, while the second one is used to monitor presence 

of agent. These four tubes are 1⁄4′′ in 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. 

Average weight of hollow zinc headform is 85 pounds. 

3.2. Leak Detector Model TDA-99M or Equivalent (Figure 2). Manufactured by Air 

Techniques International in Owings Mills, Maryland, the TDA-99M is one of the 

primary tools for accessing aerosol leaks in the mechanical seals of the respirator 

and proper fit of a respirator to a clean SMARTMAN® headform under non-toxic 

oil aerosol conditions. The device generates a polyalphaolefin (Emery 3004 

manufactured by the Henkel Corporation, Emery Group or equivalent) aerosol 

that is used to detect leakage in the respirator. With the respirator properly 

installed on the SMARTMAN® and the breather pump operating at manufacturer 

specifications, the TDA-99M generates a liquid particulate aerosol at a 

concentration of 100 mg/m3

. This aerosol is introduced by the TDA-99M’s pump. 

The respirator interior is monitored for the presence of aerosol. The leak detector 

compares the concentration inside with the concentration outside, and calculates a 

digital percent penetration value. 

 Figure 2. Leak detector model TDA-99M. 

3.3 MINIature Continuous Air Monitoring System, MINICAMS® or Equivalent 

(Figure 3)). Manufactured by OI Analytical, the MINICAMS® is a gas 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 4 of 39 

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 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. The limit of 

detection (LOD) is equal to 20% of the 8-hour time weighted average (TWA) for 

the specific chemical agent being detected. Residual contamination is the amount 

of challenge agent lingering in the breathing zone of the respirator when a new, 

clean respirator is mounted on the SMARTMAN®. Residual contamination is 

quantified at the beginning of each test and the MINICAMS® output must remain 

stable for a period of 60 minutes prior to the initiation of any test. Minimum of 

two MINICAMS® are required in order to continuously monitor the interior of 

the respirator. 

Note: Next generation MINICAMS® and support equipment require successful NIOSH 

validation testing (V-test) documentation before implementation of the next generation 

equipment used for NIOSH certification/approval testing. 

Figure 3. MINIature Continuous Air Monitoring System, 

(MINICAMS®). 

3.4 Syringe Pump, Sage® Model M365 or Equivalent (Figure 4). This multi-range, 

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 cavity or vessel, to the dilution airline. The plunger of the syringe is driven 

at a controlled rate by the pump to deliver a calculated 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 to 0.3 L/hr, and flow accuracy of ± 5% nominal. 

Technicians must be proficient on the pump’s user instructions. 

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 Figure 4. Syringe pump, Sage® Model M365 

Note: Next generation syringe pumps or equivalent equipment and support equipment for 

data logging/automation, require successful NIOSH validation testing (V-test)

documentation before implementation of the next generation equipment used for NIOSH 

certification/approval testing. 

3.5. Flow-Temperature-Humidity Control System or Equivalent (Figure 5).

Manufactured by Miller-Nelson Research, Inc., this system, referred to as the 

Miller-Nelson® Control System, is an automated system to control the airflow, 

temperature, and humidity of an air supply for an operating respirator system. 

Laboratory specified 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 (50–200 L/min ± 2%), and relative 

humidity (20%–80% ± 3%) and temperature (20°C–30°C ± 0.3%). 

 Figure 5. Miller-Nelson® flowtemperature-humidity control system. 

3.6 Exposure Chamber or Equivalent (Figure 6). The respirator exposure chamber is 

constructed of clear, chemical resistant material (Plexiglas® or Lexan®) or other 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 6 of 39 

equivalent material. The floor must be constructed efficiently to support the 85-

pound SMARTMAN®. The front panel is removable and is held in place with 

clamps on each edge. The dimensions are approximately 2 ft3

. Four legs made out 

of the same chemically resistant material are attached to the bottom to hold the 

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

face adjustment handle. A M12A1 military specified air-purifying canister 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 challenge concentration 

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

achieve a mixed challenge concentration. A clean exposure chamber is a unit used 

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

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

chamber is a chamber used to perform testing of the respirator unit, using live 

agent. 

3.7 Agent Mixing Chamber or Equivalent (Figure 7). This chamber is fabricated of 

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

of chemical warfare agent vapor and air. A pressure gauge, mounted on the 

mixing chamber, indicates internal mixture pressure and serves as a safety 

pressure indicator. Maximum pressure is indicated per laboratory standard 

operating procedures. A heating blanket is wrapped around the chamber to 

facilitate chemical vaporization. This is the primary mixing area that allows the 

chemical agent syringe pump flow and the regulated airflow from the Miller 

Nelson controller to mix and generate a specified concentration of chemical 

warfare agent. When the mixture is not being passed into the exposure chamber 

for a test, it is passed through a scrubber filter (an M18 military specification 

canister or equivalent). 

 Figure 6. Exposure chamber. 

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 Figure 7. Mixing chamber. 

3.8. Breather Pump, Model E1R1® or Equivalent (Figure 8). Manufactured by Jaeco 

Fluid Systems, Inc., it is a breather pump used to replicate breathing. It is a double 

pump, operated by a single electric motor. The pump design is a modified 

variable speed motor generating varied strokes per minute. Planetary gears and a 

Scotch Yoke, producing a sinusoidal breathing pattern, control the pump. The 

sinusoidal pattern starts at zero flow rate, rises to peak flow of approximately 

π (3.1416) times the rated test certification flow rate in L/min and drops back to 

zero. The exhalation stroke of the pump is the same sinusoidal pattern. The 

volume per breath or tidal volume is adjustable up to 1.5 liters. 

 Figure 8. Breather pump. 

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3.9 Mass Flow Controllers or Equivalent. Manufactured by Tylan Electronic or 

Brooks Instruments. Mass flow controllers 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 flow requirements. Flows are controlled to ± 2% of set point. 

3.10 Ambient Air Analyzer, MIRAN® Model 205B and Model 1A, or Equivalents

(Figures 9 and 10). Manufactured by Thermo Environmental Instruments, Inc. in 

Franklin, Massachusetts, these are infrared absorption based detectors that uses a 

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

Model 250B is used to monitor the challenge concentration of the vapor and 

liquid phases of HD. The Model 1A is reserved for analyzing the Sarin (GB) 

concentration. 

NO PHOTO CURRENTLY AVAILABLE ON MODEL 205B 

Figure 9. MIRAN® analyzer, model 205B.

NO PHOTO CURRENTLY AVAILABLE ON MODEL 1A 

Figure 10. MIRAN® analyzer, model 1A.

3.11 Respirator Systems Required for Testing: 

3.11.1 Required Quantities: Quantity of respirators for HD Live Agent Testing 

(LAT) is per NIOSH/NPPTL CBRN APR Statement of Standard, Table 7, 

Test Sequence and Quantity Matrix. Overall HD LAT quantity is three 

complete respirator systems. An additional three respirator systems are 

reserved for the Sarin (GB) LAT. One respirator system is tested as a 

qualifier in this STP and is commonly known as the Qualifier Live Agent 

Test (QLAT). Remaining two respirator systems are tested in sequence 

and are commonly known as the Remainder Live Agent Tests (RLAT).In 

the case of canisters, 125 canisters only, go through hot, cold, humidity, 

vibration and 117 of the 125 are manually dropped as a final conditioning 

action before being tested in one of five types of service life tests. LAT 

penetration and permeation testing is one of those five types of service life 

tests for CBRN APR protocol. Initially, one respirator is required in a HD 

“Qualifier Application” “as is”. Overall, of the two total “as is” qualifier 

respirators, one is live agent tested against HD and the other is reserved 

for live agent testing against GB. Then, four environmentally conditioned 

canisters come out of environmental testing and of those four canisters, 

two go to HD RLAT and two go to GB RLAT utilizing environmentally 

conditioned like item respirators. In other words, two CBRN APR “as is” 

candidate respirators are live agent tested first before or in parallel to any 

subsequent CBRN APR statement of standard tests commence. The two 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 9 of 39 

qualifier respirators must each pass their respective LAT under an initial 

Qualifier Application to proceed on in the remaining test protocol. Upon 

confirmation that the Qualifier Application is a success and completion of 

environmental conditioning, remainder LAT is completed by randomly 

selecting Task Number respirator systems for follow on remainder LAT, 

GB and HD, in accordance with CBRN APR Statement Of Standard, 

Paragraphs 4.7 and 4.9. Respirators designated as spare queue conditioned 

respirators are stored and available for use by the testing laboratory in 

situations where ongoing test processes are compromised by installation 

power failures, inaccurate test processing or other mid-test termination 

events identified by the test laboratory manager. In most cases, spare 

queue respirators are not to be used for additional certification testing 

because the applicant or manufacturer requests it. NIOSH should be 

informed of all testing of spare queue inventory conducted by the testing 

laboratory. 

3.11.2 Qualifier LAT: HD LAT canisters and face blanks should be received 

from the appropriate NIOSH/NPPTL sanctioned source in “as tested or as 

is” condition. No alterations to the environmentally tested canisters are 

authorized prior or during live agent systems testing. At the NIOSH tenant 

laboratory initial certification qualifier application inventory, canisters 

received “as is” in the ready-to-use/minimum use configuration packaging 

are required to be unopened, regardless of type of original packaging, and 

delivered to LAT lab upon completion of satisfactory certification 

inventory. 

3.11.3 Remainder LAT: Commencement of HD RLAT is contingent upon 

testable canisters completing all required NIOSH/NPPTL CBRN APR 

environmental factors testing and processing prior to any live agent 

testing. Environmentally pre-conditioned canisters are attached, per 

manufacturer instructions, to available compatible application faceblanks 

prior to live agent testing by qualified and designated laboratory live agent 

testing technicians only. Environmentally pre-conditioned canisters should 

be received in minimum packaging configuration and administratively 

labeled with the start and end dates of environmental testing, the type of 

damage, if any, observed, the manufacturer, the name of the individual 

responsible for the environmental testing including a contact phone 

number and the laboratory’s name. Only the manufacturer’s inlet and 

outlet plugs that come with the canister are to be used to seal up the 

canister after environmental testing. If no plugs are provided, no other 

form of sealant is authorized. Start of live agent testing must commence 

within 12 hours of receiving the environmentally conditioned canisters 

and facepieces. Any canister damage during environmental 

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testing/processing is required to be preserved, not altered and noted on 

administrative markings for shipment to LAT lab. 

3.11.4 HD live agent systems test canisters and respirators should be labeled 

prior to actual live agent testing with the following administrative 

information: 

— NIOSH task number (TN number) 

— Model of APR 

— Other routine information that will allow the lab to accurately track 

receipt, time in test, test results, noted observations, required retest, 

status of testing, disposal and trend analysis is required to be managed 

and available for review upon request by current representative of 

NIOSH/NPPTL. 

— NOTE: Accurate labeling of post-tested respirators is mandatory in 

support of post-test incident investigations. 

4. TESTING REQUIREMENTS AND CONDITIONS

4.1. Any laboratory using this procedure to supply certification test data to NIOSH 

will be subject to the provisions of the NIOSH Supplier Qualifications Program 

(SQP). This program is based on the tenets of ISO/IEC 17025, the NIOSH Manual 

of Analytical Methods and other NIOSH guidelines. An initial complete quality 

system audit and follow on audits are requirements of the program. Additional 

details of the program and its requirements can be obtained directly from the 

Institute. 

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

accordance with laboratory procedures and NIOSH/NPPTL guidance. Sound 

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

tolerance range of expected data performance of a plus or minus 25% of a 95% 

confidence interval of the stated standard requirement. NIOSH/NPPTL P&A 

tolerance can be higher but not lower. 

4.3. 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). 

4.4. System Test Conditions:

4.4.1. Breathing Machine: 

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— Airflow = 40 liters per minute (Lpm) 

— Respirations = 36 ± 2 strokes per minute 

— Tidal Volume = 1.1 liters 

4.4.2. Miller-Nelson® Airflow Settings into Exposure Chamber: 

Airflow Rate: The actual value here is experiment/method dependent. The 

value eventually used must be documented. Determine an appropriate 

airflow rate based upon obtaining a stable concentration and upon the 

volume of the exposure chamber, considering the agent challenge 

concentration desired, volume of chamber, breather airflow, and dilution 

air exhaled from the APR. 

Relative Humidity: 50% ± 5% RH. 

Temperature: 25°C ± 3°C 

4.4.3. SMARTMAN® Sampling Point: 

Breathing zone sampling point is a single SMARTMAN® nasal port that 

allows sequential dual MINICAMS® detections. 

4.4.4. Mustard (HD) Exposure Test: 

4.4.4.1. HD vapor: General. 

— Vapor Challenge Concentration = 50 mg/m3 ± 10%. 

— Vapor Challenge Time (disseminator on) = 30 minutes, 

but no longer than 31 minutes. 

— Monitor & Hold Time = 7.5 hours. 

— Total Test Time = 8.0 hours. 

— Syringe Injection Rate = as required based upon syringe 

pump used. 

— Syringe Injected Volume = as required based upon 

syringe pump used. 

4.4.4.2. Mustard (HD) agent vapor generated is required to be 

Chemical Agent Standard Analytical Reference Material 

(CASARM) grade. Agent purity analysis must be NIST 

traceable, documented and meet CASARM agent purity 

requirements. Proper CASARM storage requirements per local 

regulation are required to be adhered to. 

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4.4.4.3. Vapor test termination is at the indicated 8 hours plus required 

check shots before and after entire test period. In the interest of 

conserving agent quantities and preserving technician personhours, a LAT is terminated if at any point in the entire 8-hour 

period, the respirator detection methods for the breathing zone 

can show repeatable system failure within the pass or fail 

protocol described in this current STP. This failure is required 

to be witnessed by a minimum of two qualified laboratory 

personnel and noted in the laboratory journal for follow on 

documentation. 

4.4.4.4. Vapor challenge concentration exposure will start immediately 

after the test chamber has been closed and sealed properly. 

4.4.4.5. HD liquid: General. 

 Drop size: 20 microliters (μL). 

 Liquid challenge concentration: Minimum is 0.43 mL (thirtytwo 20 μL drops) and maximum is 0.86 mL (forty-three 20 μL 

drops) depending on type of respirator tested. 

 Droplet allocation: Thirty-two drops are used for chin and 

cheek style respirators with or without hydration facility and 

one single connected canister. Forty-three drops are used for a 

non-facepiece mounted APR, which consists of 32 droplets on 

the faceblank area and 11 droplets on components such as 

breathing hose(s), multiple canisters, communications device 

interface, electrical power interface and other noted critical 

interfaces as determined by NIOSH/NPPTL during 

configuration analysis. 

Droplet schematics: Three NIOSH/NPPTL schematics of HD 

agent droplet placement for CBRN APR application (Facepiece 

mounted and non-facepiece mounted) are enclosed. 

The listing is as follows: 

Appendix A: Chin style, biocular, no drink component. 

Appendix B: Chin and cheek style, monocular, and drink 

Component. 

Appendix C: Chin and cheek style, biocular, drink component 

and communications interface. 

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External shroud or hood: Use of an external shroud or hood 

attached to the facepiece does not represent the worst case 

configuration and will therefore be removed, if possible, prior 

to LAT. Facepiece second or third skins layers must be 

explicitly specified in the application submission as a required 

part of the CBRN APR configuration prior to LAT. If they are 

not, the worst case that will be tested is with the second skin 

removed. If a hood or shroud is permanently attached to the 

facepiece, the respirator 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 nonshrouded facepiece but instead of applications being on bare 

facepiece material they are on the shroud covering that 

depicted area/seam/joint/interface. All other defined criteria 

apply. 

Vapor time: The application of vapor HD droplet starts the 

official total test duration time from when the first droplet is 

applied and MINICAMSs are actively sampling at this time. 

HD vapor challenge time is a different subset time 

management of the total test time of 8 hours and could be 

managed independent of the total test time to allow accuracy of 

HD vapor and liquid exposure. 

Liquid time: HD liquid agent is applied to respirator at the 6th

hour during the test procedure. Total time that CBRN APR 

candidate system is exposed to both HD vapor and HD liquid 

(Liquid Time) is 2 hours, the last 2 hours of the total 8-hour 

test time period. 

4.4.4.6. Mustard (HD) agent liquid is required to be Department of 

Defense, US Army CASARM grade. Agent purity analysis 

must be NIST traceable, documented and meet US Army 

CASARM agent purity requirements. Proper CASARM 

storage requirements per local regulation are required to be 

adhered to. 

4.4.5. Test Termination Parameters: The termination of the HD liquid 

application test is in accordance with the total liquid/vapor test duration 

time of 8 hours plus the before and after test check shots. The test will be 

terminated to protect the detectors from over-saturation provided a 

candidate APR shows failing criteria prior to the 8-hour mark. The 

termination point should be set at or above the highest calibration point for 

each one of the MINICAMS® in use. 

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4.5. Safety and Training. Normal laboratory safety practices are required. Laboratory 

specific regulations such as US Army Regulation 50-6, Chemical Surety apply as 

required. The practices include all safety precautions described in the current 

Centers for Disease Control and Prevention (CDC) General Laboratory Health 

and Safety Manual, the applicable US Army Regulations, the U.S. Army Soldiers 

and Biological Chemical Command Laboratory Safety Procedures, and any other 

equivalent manuals and periodicals. 

4.5.1. Safety glasses, lab coats, assigned respirator, butyl apron and butyl gloves 

are required be available, worn and replaced as laboratory standard 

operating procedures apply. 

4.5.2. Work and walking surfaces must be maintained free of clutter and nonessential test equipment. 

4.5.3. When handling any glass laboratory equipment, lab technicians and 

personnel must wear approved gloves, which are rated appropriate in 

accordance with current safety and hygiene plans. 

4.5.4. Laboratory personnel are required to be trained on this STP and 

documentation is required to be available for review of said training. 

Personnel are required to be trained and qualified per local requirements in 

all applicable standard operating procedures (SOP) appropriate for the test. 

4.5.5. The responsible technician must be knowledgeable about the specific 

CBRN APR being tested and should be able to readily identify all CBRN 

APR hardware components, subassemblies and accessories and be able to 

support accurate trouble shooting of the CBRN APR and subassemblies to 

ensure it is operating in a correct negative pressure mode. The responsible 

technician must be able to properly align and fit the respirator facepiece on 

the SMARTMAN® headform without malformation or destruction of any 

CBRN APR material. 

4.5.6. All LAT equipment passing or failing these NIOSH test protocols will be 

treated as hazardous materials in accordance with local laboratory 

procedures and methods. Disposal of such contaminated CBRN APR 

materials is the responsibility of the testing laboratory. In accordance with 

this STP, respirator manufacturers are released of equipment 

accountability once equipment is formally tested in the appropriate 

NIOSH recognized test laboratory. Manufacturer warning and caution 

statements for the respirators are subject to legal interpretation and most 

likely will not apply once the respirator has been contaminated by toxic 

chemical warfare agents and processed thru the decontamination 

procedure. 

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4.5.7. 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. 

Refer to appropriate material safety data sheets, manufacturer’s 

instructions and available current health and safety manuals, or other 

appropriate documentation for the proper protection and care in handling, 

storing, and disposing of the contaminated respirators, canisters, 

subassemblies and chemicals used in this procedure. 

4.6. Equipment Pre-Test Conditions: MINICAMS®

4.6.1. Background Reading: A laboratory MINICAMS®, as opposed to a field 

MINICAMS®, is used as the detector for agent permeation and 

penetration of the CBRN APR. It consists of a monitor, PC computer, 

linear mass flow meter and optional printer or recorder. Before the APR is 

placed on the exposure SMARTMAN®, the MINICAMS® are required to 

show steady state background readings lower than the lowest point on the 

current MINICAMS® calibration curves. This is accomplished per local 

laboratory procedures but a clean M40 mil spec respirator mounted on the 

SMARTMAN® head form may be used. The SMARTMAN® is then 

allowed to breathe for the required time (8, 12, 48, 72 hours etc.) until a 

steady state background is achieved that is lower than the lowest current 

calibration curve point indicated on the respective MINICAMS® 

performance results. The LAT for certification is not authorized to start 

without the background readings of the assigned SMARTMAN® system 

(tested respirator and headform) being within the limits specified above. 

4.6.2. Unit of Measure. A small volume of air is drawn through a preconcentrator tube containing an adsorbent material: HD sample volume is 

per the determined value. 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. 

4.6.3 Sample Cycle. Operation of the MINICAMS® requires the use of 

compressed house 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 

laboratory application. CBRN APR HD analysis requires a 6-minute 

cycle. The two MINICAMS® are required to be synchronized so that one 

MINICAMS® sampling begins when the other MINICAMS® sampling 

ends. Raw data results confirm this requirement. 

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4.6.4. HD Detection Principle. The MINICAMS® is installed in accordance with 

the operating manual and local lab SOP. The appropriate optical filter for 

HD must be installed in front of the photomultiplier tube. In principle, 

when HD burns in a hydrogen flame, a chemical element (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. 

4.6.5. Standardization. MINICAMS® are configured in accordance with the 

operating manual and the specific method for the chemical warfare 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 μL) of a known standard solution of 

the agent onto the pre-concentrator tube during the INJECT segment of 

the test cycle. The standard solutions of agent are made in 

spectrophotometric grade isopropanol. At least three injections of each 

quantity of agent should be injected per LAT sequence. 

4.6.7. 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 

— Standby for start of testing 

4.7. Equipment Pre-Test Conditions: SMARTMAN® HD Vapor Generation and 

Liquid Application 

4.7.1. Vapor Concentration. 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, taking into account the volume 

of air discharged into the chamber from the exhalation air of the APR. 

Ramp-up Time: Conditions for each individual system will have to be 

determined for each laboratory setup to achieve the required ramp up time 

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for CBRN APR exposure concentration. The ability to accurately detect 

and quantify this agent ramp up time is a requirement for the testing 

laboratory and ramp up time and agent duration exposure time graphs 

should be available to confirm agent exposure duration in accordance with 

the procedures of this STP. 

4.7.2. Concentration Verification Summary:

HD Setup (Mass Balance Analysis Concept or another demonstrated 

equivalent concept is used to confirm repeatable HD quantity sampling 

and amount of agent used per test.) 

— Chamber size = 8 ft3

— Target Vapor Challenge Concentration = 50.00 mg/m3

 ± 10%. 

— Ramp-Up Time = 1–2 minutes (Time from initial start of syringe 

pump to 50 mg/m3

, lowest acceptable challenge concentration.) 

— Dilution Air from Breather Pump = 40 L/min 

— Miller-Nelson® Challenge Mixing Air = 50 L/min 

— Example: Syringe Rate for Challenge Injection = 1.0 mL/min 

— Total HD vapor challenge in 30 minutes = 0.25 mL 

— Add HD liquid challenge at the 6-hour mark = 0.43–0.86 mL of 

liquid droplets. 

4.7.3. Agent Dispersion. 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 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.

4.8. Equipment Pre-Test Conditions: Miller-Nelson® Controller

4.8.1. The Miller-Nelson® unit receives compressed air from the laboratory 

house air supply system. Operate the Miller-Nelson® according to the 

manufacturer’s instructions. The sensors for relative humidity and 

temperature must be calibrated, as well as the flow controller, since it is 

important that the total flow through the test system be known in order to 

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supply the requisite amount of agent from the syringe pump. Insure the 

total flow value is logged in the technician’s lab logbook prior to 

commencing each actual LAT. 

4.8.2. Set the readout panels on the Miller-Nelson® according to paragraph 

4.2.2. Ensure the Miller-Nelson® is properly configured for current test 

procedure and all required airlines are secure to inlet ports of 

SMARTMAN® and Miller-Nelson® systems. Allow the clean air to flow 

through the mixing chamber and the M18 filter until it is time to start the 

test. 

4.9. Equipment Pre-Test Conditions: Syringe Pump

4.9.1. 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. Manual setting of the syringe pump 

controls allows the pump rate to be changed by using a turn knob. 

4.9.2. 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. 

4.9.3. 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. Turning off the power switch will stop the drive block from 

pushing against the plunger and stop the challenge agent concentration 

flow at the predetermined time. 

4.10. Equipment Pre-Test Conditions: TDA-99M Aerosol Leak Detector

4.10.1. The TDA-99M leak detector is used to detect oil particulate aerosol leaks 

into the CBRN APR after it has been installed on the SMARTMAN® 

headform cold box. Ensure the canister and all components are correctly 

mounted and tightened per the current manufacturer instructions and 

specifications. The APR is operated under negative pressure using air 

supplied to the APR from the Miller-Nelson® filtered house air of the 

laboratory. Ensure that procedures for the APR follow the manufacturer’s 

installation procedures for gasket seal and facepiece donning and 

interface. The canister and gasket, if provided, should be the same product 

that has undergone recent NIOSH/NPPTL environmental factors testing or 

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in the “as is” ready-to-use condition. Ensure the seal, threaded interface, 

inlet and outlet areas and canister housing are not changed in any manner 

prior to or during the LAT. However, if the canister or canister interface 

thread is deformed from environmental testing, continue with the test by 

attaching the canister per manufacturer instructions. Do not make any 

corrections for canister deformities at this time. Ensure the lab book is 

annotated and digital photos are taken and available for follow up incident 

review if necessary. 

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

manufacturer’s instructions. The APR should be in static non-breathing 

mode. Turn on the breather pump to activate the negative pressure test 

respirator. 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. If no localized leaks are found, replace the front 

panel of the exposure chamber and start the actual TDA-99M test. 

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

chamber with aerosol. Maintain a constant aerosol concentration inside the 

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

detection of aerosol inside the facepiece. When the detector indicates a 

maximum penetration of less than 0.0010 % for 30 minutes, continue with 

the next item in the LAT procedure. If there is evidence of leakage, 

attempt to find and eliminate the leak. If a leak is detected during the 

process isolate the canister by using a dedicated clean Teflon tube to draw 

clear air from outside the chamber in accordance with local laboratory 

SOP. Ensure Teflon tube data and configuration drawing is annotated in 

lab book. 

4.11. Equipment Pre-Test Conditions: Quality Control Measures

4.11.1. SMARTMAN® Leak Test: Because the SMARTMAN® is made of cast 

zinc, it is possible for leak paths, after extensive LAT or incorrect 

assembly, to form through the metal casting, allowing chemical warfare 

agent vapor to pass through the headform cavity into the interior of the 

respirator mounted on the headform. To check for these invisible leak 

paths, install a clean peripheral seal on the headform and inflate it to 

maximum pressure of 3 psi. Flood the interior of the headform with a 

known rated helium concentration and purity. Use the probe of the helium 

leak detector to check the entire surface and the seal for presence of 

helium. Any leak found by the helium leak probe procedure must be 

diagnosed and eliminated, if possible. The leak test is to be performed 

initially on each new or reconditioned SMARTMAN® and monthly on the 

SMARTMAN® headforms when they are in continuous daily use. 

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4.11.2. 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 US Army, ECBC 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 of r2

 = 0.99 for HD. Agent solutions must be stored 

at 4°F or lower. 

4.11.3. Calibration 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 US Army Test Methods 

& Development Equipment (TM&DE) and Metrology Laboratory, in 

accordance with ISO 17025 procedures or equivalent and use instruments 

traceable to NIST. Flow meters to be checked against calibrated meters are 

the Miller-Nelson® airflow controller, all electronic flow meters used for 

the MINICAMS® preconcentrator tube and the flow meters from the 

breather pump and the syringe pump agent injector. 

4.11.4. Aerosol Leak Testing: APR 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. Allow the TDA-99M to stabilize in 

its initial detection procedure. When readings are stable within ± 2 end 

place digits of 0.0000, the TDA-99M aerosol tester is ready to begin 

detecting potential leak paths. If there is no leak, the display on the TDA99M should read 0.0000% penetration. 

4.11.5. MINICAMS® Detector Response: Check the response of the 

MINICAMS® detector, before and after each LAT. 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 response 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 check 

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shot does not reproduce a verifiable result, repeat the check shot. If the 

second check shot is not within the 10% parameter, the test is invalid. A 

quantifiable check shot should be made at the maximum, within 3 hours of 

the start of the actual test and at the APR end of test 8-hour mark. 

5. PROCEDURE

5.1 HD LAT (0351)

5.1.1 Assemble APR per manufacturer’s instructions. Ensure the packaged 

canister is received as specified in paragraph 3.11 and CBRN APR 

Statement of Standard, Paragraph 4.10, Table 7, Note 2. The last note here 

identifies the canisters only being in being in the “minimum 

manufacturer’s recommended packaging”, which is interpreted as the 

ready-to-use assembly for the canister. Facepieces will be tested “as is” 

when submitted in the qualifier application, conditioned in the remainder 

application and married up with appropriate ready-to-use or conditioned 

canisters in accordance with CBRN APR Statement of Standard. 

5.1.2 Take digital photographs of the assembled unit prior to start of LAT. 

These photographs are required to be available for NIOSH/NPPTL review 

and they should accurately and clearly indicate how the actual manual 

placement of the HD droplets occurred at the 6-hour mark, prior to vapor 

testing re-commencing. 

5.1.3 Mount the respirator on the SMARTMAN® in the clean exposure 

chamber. The facepiece should be mounted to the SMARTMAN® per the 

manufacturers’ operating user instructions with special emphasis on head 

harness fitting and canister tightness. Ensure all parts of the facepiece are 

mounted and seated correctly on the headform. If a shroud or other 

accessory is being tested as part of the respirator system, ensure that they 

are mounted properly and serviceable. If batteries are required for 

communications devices, ensure they are in place and the communications 

device is turned on. Monitor the communications device for malfunctions 

during the course of the test and visually check it and other accessories at 

the termination of the test for visible cracks or breaches of the airflow 

boundary i.e., compromises of form, fit or function. 

5.1.4. Turn on the breathing pump. Insure that the APR is in the negative 

pressure mode by conducting negative pressure seal check(s) with 

protected hand over required surfaces of the tested respirator per on hand 

current manufacturer operating instructions or use instructions. Use the 

integrated SMARTMAN® magnehelic pressure gauge as required to 

support confirmation of negative pressure cycles. Magnehelic pressure 

gauge should be used only as a qualitative indicator of APR performance 

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and it can serve as a tool for observation purposes. Do not allow the tested 

CBRN APR to go into or maintain positive pressure for any reason such as 

misdirected house air from air flow tubing cracks, kinks or failure 

5.1.5. Using the TDA-99M, leak test the APR in the negative pressure mode. 

Connect the detector inlet to a sample line from the SMARTMAN®, 

allow the APR to breathe, and create a stable value on the TDA-99M. 

When the 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 by the authorized laboratory 

technicians or manager only. If a leak is found through the canister, 

connect a clean airline from outside the exposure chamber. 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 the aerosol challenge inside the 

chamber for 30 minutes of continuous TDA-99M operations below 

0.0010% penetration. If penetration exceeds 0.0010%, the TDA-99M 

alarm sounds or the digital readout shows higher values, stop the 30-

minute test, re-analyze the system and begin a new 30-minute test period. 

The APR must pass a continuous 30-minute test at ≤ 0.0009% penetration 

parameters in separate clean exposure chamber and an agent exposure 

chamber to be considered qualified to progress on in the agent testing. If 

after repeated attempts a successful leakage test cannot be achieved, the 

laboratory manager may use alternative means to seal the facepiece to the 

headform such as sealing the facepiece and nosecup to the headform using 

non-toxic adhesive with the concurrence of the NIOSH/NPPTL. All 

adhesive designated for CBRN certification use is required to undergo 

verification testing (V-test) prior to use as a CBRN LAT capable 

substance successful performance to the given STP using three 

consecutive V-test trial samples. If the respirator continues to fail the 

TDA-99M, the manufacturer must supply confirmed MSDS on the type of 

particulate being picked up by the TDA-99M. In addition, the 

manufacturer must obtain an analysis by a third party laboratory 

confirming the manufacturer’s MSDS, the particulates must be determined 

to be non-toxic in the acute and chronic human toxicology perspective. 

5.1.6. Before the APR facepiece can be placed on the SMARTMAN® in the 

agent exposure chamber, the MINICAMS® must have shown a steady 

state background lower than the lowest point on the calibration curves. 

This is accomplished by installing a M40 mil spec respirator on the 

SMARTMAN®. Ensure a new or sanitized decontaminated M40 

respirator is used. The SMARTMAN® should be allowed to breathe until 

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the steady state background is lower than the lowest calibration curve 

point indicated on the respective MINICAMS®. 

5.1.7. Remove APR from clean exposure chamber and install on 

SMARTMAN® in the HD agent exposure chamber. 

5.1.8. Mount the respirator on the SMARTMAN® in the agent exposure 

chamber. Conduct a TDA-99M 30-minute test by repeating steps of 

paragraph 4.8, with the exception that once the agent exposure chamber is 

sealed and no leaks are confirmed with the TDA-99M, the TDA-99M 

aerosol challenge is discontinued. Ensure the agent exposure chamber is 

purged of Emery oil particulates for at least 15 minutes. Insure that the 

removal of the TDA-99M test hardware does not disturb the established 

seal of the APR facepiece to the SMARTMAN® system. Remove the 

clean airline from the canister system, if it was used to isolate leaks. 

5.1.9. Turn on the Miller-Nelson® flow, temperature and humidity controller. 

5.1.10. MINICAMS® Background Characterization. A background 

characterization must be run before every agent test. The MINICAMS® 

should be monitored for a period of 60 minutes prior to the initiation of the 

chemical agent warfare test. Confirm that background level is less than the 

lowest point on the MINICAMS® calibration curve. If the background 

level is not less than required, trouble shoot the SMARTMAN® system, 

do not start the test, advise laboratory manager and if necessary remove 

the APR facepiece, decon the headform, re-don the facepiece and restart 

the procedure for characterization as necessary. If the APR is removed 

from the head form, restart the test procedure from paragraph 5.1.3. 

5.1.11. Set up standard operational mode of test equipment. Ensure all test 

equipment is within calibration. 

5.1.12. Set Miller-Nelson® for airflow into exposure chamber set to deliver 

required rates. See paragraph 4.4.2. 

5.1.13. Load liquid agent in syringe and set syringe pump to correct flow rate to 

achieve the required agent challenge concentration. See paragraph 4.7. 

5.1.14. Ensure MINICAMS® are calibrated, the check shot is complete and 

acceptable and ready for the operating mode. Annotate the check shot 

times and concentrations. 

5.1.15. Ensure that the challenge concentration instrument is calibrated and is 

ready for analysis. Monitor agent exposure chamber during the 60 minutes 

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background characterization period. Characterization reading should 

reflect a steady state condition. 

5.1.16. HD Vapor Application:

5.1.16.1. Time zero plus 1 second or start of the agent test is when the 

first confirmed vapor state of HD is applied to the interior of 

the agent exposure chamber while the MINICAMS® are 

actively sampling. Vapor is pumped in for 30 minutes, turned 

off and agent decay cycle is monitored for 5.5 hrs. At the 6-

hour mark, pre-defined liquid droplets are applied per the exact 

enclosed droplet appendix or a NIOSH approved modified 

droplet appendix. Hotbox is closed back up as fast as possible 

and remaining test cycle time and detection operation proceeds 

up to the 8-hour mark. Droplet application should be 

expeditious, safe and done in a timely manner. Annotate the 

time zero plus 1 second and the HD liquid application time 

period and liquid exposure time. Visual observation of the 

tested APR for the last 2 hours of testing is highly 

recommended. 

5.1.16.2. The 30-minute vapor exposure begins when HD vapor is 

injected into the HD exposure chamber. Annotate this starting 

time. Ensure time management is accomplished that allows the 

efficient tracking of two simultaneous events: one clock for 

total test time from start of HD exposure for 8 hours and 

another clock for HD vapor at 30 minutes. If necessary, the 

vapor clock can convert to the liquid agent clock at the 6-hour 

mark. 

5.1.16.3. Introduce HD vapor agent challenge to the agent exposure 

chamber. Turn the valve inline from bypass of the mixing 

chamber to direct flow from the mixing chamber to the internal 

ambient space of the agent 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 monitored using the appropriate MIRAN® detector. 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 is required to start the MINICAMS® before 

introducing agent into the chamber so that the first sampling 

period will coincide with the first agent challenge. 

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5.1.16.4. The vapor syringe pump should run for the prescribed 

challenge period of 30 minutes, but no more than 31 minutes. 

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

Record the total volume used by the syringe pump, the elapsed 

time and the airflow rate delivered from the Miller-Nelson®. 

These values will be recorded in the laboratory notebook and 

test data sheets. Ensure syringe flow is off and the mixing 

chamber airflow line is bypassed so uncontaminated air is 

flowing through the Miller-Nelson® to the agent exposure 

chamber, simulating weathering.

5.1.17. Liquid Application of HD droplets: 

5.1.17.1. Liquid drops are delivered to the surface of the APR to test 

permeation of material surfaces. A minimum of 32 and a 

maximum of 43 droplets (20 μL each) are specified. Placement 

of the droplets, via syringe or equivalent glove box methods, 

on to the system is specified in Appendixes A, B and C of this 

STP. The droplets will be placed on the equipment per the 

numerical sequence and note inserts identified in the 

appendixes. Photographs of this manual droplet application 

process should be maintained in the task number folder. The 

liquid application of HD occurs at the 6-hour mark, after 

the vapor challenge begins and ends. The droplets usually 

stay until the test cycle ends.

5.1.17.2. CBRN APRs with hose assemblies, chest or back mounted 

canisters or specific submittal mandatory components require 

the maximum droplet quantity of 43 drops. HD droplets 1-32 

apply to the facepiece and the canister. Droplets 33 to 43 are 

applied in accordance with the stated appendixes. If no hose 

assembly or a modified hose assembly is used, droplets 33 to 

43 are used on any Y adapters, communications devices, or 

other respirator mandatory submittal application items in 

accordance with droplet patterns enclosed and conducive to 

targeting seams, material interfaces and obvious breathing 

airflow channel areas. 

5.2.17.3 The droplet placement sequence is in accordance with local 

laboratory policy and is recommended to start at the top of the 

face blank, working left to right, to the bottom of the face blank 

and follow the droplet number sequence identified in 

Appendixes A, B and C of this STP. Prior to actual droplet 

application, technicians should prepare by marking location of 

actual droplets on a digital photograph of the equipment being 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 26 of 39 

tested and use this “dotted” schematic during the course of 

testing. If an external shroud is permanently mounted on the 

face blank, apply droplets per standard schematic based on 

respirator configuration but on surfaces of the shroud that 

mirror the routine face blank areas. If not permanently affixed, 

remove the shroud prior to test in order to test the “worst case 

configuration”. 

5.2.17.4. Guidelines for identification of test configuration for exposure 

to GB/HD are stated in the current version of the CBRN APR 

Statement of Standard. The focus is on obvious pressure 

boundary concerns and any protective material surface that 

appears to be a possible concern related to penetration or 

permeation. The test configuration should conform to one of 

the enclosed appendixes. If the test configuration does not 

conform, notify NIOSH/NPPTL as soon as possible, provide a 

digital of the respirator if required and await a new NIOSH 

droplet application schematic. 

5.2.17.5. Once the last droplet is applied, conduct a visual check of the 

breathing APR to ensure it is in still in negative pressure mode, 

no parts or accessories are out of place and that there is no 

immediate destruction of material due to the recent exposure to 

HD droplets. Mount the front panel of the agent exposure 

chamber. If APR starts to disintegrate immediately during or 

just after droplet application occurs, finish the droplet 

application process and close up the box immediately. Allow 

the test to run, monitoring the pass or fail criteria and terminate 

in accordance with paragraph 4.4.

5.2.18. A detector is used to monitor the challenge concentration in the exposure 

chamber. This will be recorded on a computer with compatible software 

capable of accurately depicting the agent concentration versus time. 

5.2.19. System Hold or Agent Decay Monitor Time involves the continuance of 

flushing the agent exposure chamber with the Miller-Nelson® 

uncontaminated air to allow the simulation of the natural effects of 

ambient environmental conditions while the persistent vapor effects of HD 

react. Ensure the breathing machine operates at the same rate for the 

remaining 7.5 hours. 

5.2.20. Test Surveillance: The laboratory technicians should monitor the entire 

test to make sure all components of the system function, collect data as 

required and monitor the breakthrough concentration to protect the 

MINICAMS® against saturation. If the system is failing, the 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 27 of 39 

MINICAMS® must capture three maximum peak excursions to document 

the APR’s failure before MINICAMS® can be taken off line from 

detecting 

5.2.21. Procedures for Termination of Test: 

5.2.21.1. The test should be terminated when the full time for the test has 

elapsed or three confirmed quantifiable consecutive maximum 

peak excursions are verifiable at any time in the test trial cycle. 

The pass/fail criteria on Ct are determined after 8-hour 

completion and raw data tabulation. To terminate the test, turn 

off breather pump. 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 agent contained in the aliquot. The 

response must be within 10% of the correct value for the final 

check shot test to be valid. 

5.2.21.2. Turn off the MINICAMS® per laboratory SOP. Turn off 

Miller-Nelson® airflow through the exposure chamber. 

Remove the test respirator; separate it into components as 

necessary and double-bag the components in accordance with 

laboratory SOP. Remove the bagged components to the 

decontamination hood for temporary storage. If requested, a 

manufacture representative may review the items at this time to 

perform reverse engineering analysis. The test respirator will 

then be decontaminated, monitored and disposed of according 

to laboratory SOP. Wipe down the interior of the agent 

exposure chamber and the SMARTMAN® using approved 

decontaminating solution. Dispose of cleaning materials 

according to laboratory SOP. Test Service Agreements (TSA) 

between the manufacturer and the test laboratory on materials 

swatch testing or entire respirators is authorized off line from 

the timeline of the conduct of this standardized test procedure. 

However, in support of the TSA testing concept, the 

NIOSH/NPPTL CBRN Respirator Research and Development 

(R&D) Test Program, current letter, provides for prioritized use 

of dedicated NIOSH test equipment in support of research and 

development that is separate and distinct from certification. 

5.2.22. Example step sequence of activities for HD liquid and vapor CBRN APR 

test. 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 28 of 39 

1. Conduct M40 preparation and background contamination assessment. 

2. Install APR in clean exposure chamber. 

3. Close clean exposure chamber and ensure APR is breathing. 

4. Challenge clean APR with TDA-99M for 30 minutes 

5. Verify that clean APR has passed TDA-99M, retest/refit, go to next 

step or if failure, substitute failed APR with a new untested APR. 

Ensure an environmentally pre-tested canister or a qualifier canister is 

used and properly labeled for LAT. 

6. Install APR in agent exposure chamber. 

7. Photograph APR. 

8. Close agent exposure chamber, ensure APR is in negative pressure 

mode and start breathing pump. 

9. Challenge APR with TDA-99M for 30 minutes in the agent exposure 

chamber. 

10. Start MINICAMS®. 

11. Monitor background inside the mask and do chamber 

concentration/check shot. 

12. Conduct characterization for 60 minutes. 

13. Ensure front panel is readily available for replacement on agent 

exposure chamber. 

14. Start makeup air using Miller-Nelson Controller while simultaneously 

starting ambient challenge concentration detection profile software, if 

not already started. 

15. Start syringe pump. 

16. Record start time of MINICAMS®. 

17. Initiate challenge agent. 

18. Record 30-minute vapor start time. 

19. Record challenge agent start time, vapor exposure. 

20. Ensure chamber ambient challenge concentration is ramping up as 

expected. 

21. Monitor MINICAMS® for detection, noted penetration peaks and 

saturation prevention. 

22. Stop syringe pump at 30-minute mark, but no later 31 minutes. 

23. Record stop time for challenge agent vapor exposure. 

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24. Record hold time start (7.5 hours). 

25. At 5.5-hour mark, conduct final preparations for HD droplet 

application. 

26. At the 6-hour mark, apply droplets per required appendix. 

27. Remain with test platform, monitor APR for visible cracks, 

catastrophic breakage or failure criteria. Monitor clock exposure times, 

do not exceed 8 hours total and ensure respirator does not convert to 

positive pressure for any reason. Testing laboratory is responsible for 

meeting all STP compliance requirements concerning test time; check 

shots, concentrations and pass/fail criteria assessment and 

determination. 

28. Eight hours, end test. 

29. Record end time and local time at 8.0 hours 

30. Conduct check shot instrumentation 

31. Record check shot results and time of last end of test check shot. 

32. Prepare system for decon and removal of tested components. 

5.2.23. Data Analysis 

5.2.23.1. Lead 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 catastrophic failure, obvious airflow boundary cracks, 

accessory cracks/failure, check shots and test start and end 

times. Lab supervisor must gain NIOSH approval prior to preapproving any deviation from NIOSH standard test procedure 

and signoff in the technician’s notebook as to the appropriate 

NIOSH approved change. 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. 

5.2.23.2. Laboratory manager and technician must complete all required 

test data sheets in accordance with Appendix D. Originals of 

all test data sheets must be completed and retained in the task 

file. Test data sheets for CBRN APR candidates are managed 

by digital exchange of pre-formatted blank file forms easily 

transferred in standard email. No NIOSH DEIMS electronic 

forms exist for CBRN APR test data collection. NIOSH 

DEIMS, current version, will assign TNs, maintain the CBRN 

APR test queue and process all initial, lab and final reviews. 

NIOSH DEIMS for CBRN APR should be reviewed, at the 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 30 of 39 

minimum, every three days by the lab technician supervisor, 

principal investigator or equivalent. While an application is 

active and has information for update, the transfer of applicable 

files should be updated daily with all applicable information to 

allow timely feedback and prevention of miscommunication. 

Key fob holders of testing lab are required to insure all 

summary data sheets are reviewed for accuracy prior to final 

submission to NIOSH/NPPTL in a timely manner. 

5.2.23.3. Transfer the permeation data from the MINICAMS® computer 

into a computer for analysis by Microsoft Excel. This table will 

contain data from the nasal area and associated time markers. 

The resulting table will each have four columns: 1) elapsed 

time 2) volume collected 3) sample collection time and 4) 

nanograms per sample. Convert the nanograms into a 

concentration, ng/L, by multiplying nanograms by a factor 

obtained by dividing the actual sample volume (typically 200 

mL but may be considerably less) into 1000 mL/L (Example: 

1.73 ng x 1/0.2 L = 8.65 ng/L). Convert nanograms/liter to 

milligrams/cubic meter by dividing by 1000 (Example: 8.65 

ng/L / 1000 = 0.0865 mg/m3

). Ct (concentration x time) is 

calculated by multiplying the collection duration time times the 

concentration (Example: 0.0865 mg/m3

 x 2 min = 0.173 

mg·min/m3

). The cumulative Ct is calculated by adding the Ct 

value for each sample time. Using Excel’s chart wizard feature, 

a plot of concentration vs. time and the Ct vs. time can be 

generated and printed using all the data in the table. 

5.2.23.4. Challenge Concentration Data: Using the computations 

generated from Paragraph 5.2.23.3 above. Plot the challenge 

concentration versus time and produce two data graphs that 

track total detection events covering any maximum peak 

excursions over 8.0 hours and total concentration over time 

known, as Cumulative Ct, covering the total 8.0 hours of 

potential cumulative and instantaneous dosages. If the test is 

terminated prior to the completion of 8.0 hours due to APR 

failure, MINICAMS® saturation preventive measures or other 

situations as outlined, laboratory technician, supervisor or 

equivalent is responsible for accurately recording all applicable 

maximum peak excursions and cumulative Ct detected in the 

tested time. 

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6. PASS OR FAIL CRITERIA

6.1. The criterion for passing is set within the authority of 42 CFR, Part 84, Subpart 

G, Section 84.63(a), (c) & (d) and Federal Register, Volume 60, Number 110, 

June 8, 1995. A two-fold pass or fail criterion is required to be met for successful 

passing of HD testing. The criterion is: 

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

Challenge: 50 mg/m3

 + 10% for 30 minutes (but not more than 31 

minutes) proceeded by a maximum of forty-three (43) 20-FL liquid 

droplet application at the 6-hour mark. 

Test Time: 8.0 hours. 

Two-fold Pass or Fail Criteria: 

a) Maximum Agent Breakthrough (Ct) = 3.0 mg·min/m3

. Concentration 

integrated over minimum service life is Ct and it is based on a detection 

sample time of approximately 2 minutes for 8 hours. The Ct data value, 

including all maximum peak excursion data points, must not be exceeded 

for the duration of the test. 

b) Maximum Peak Excursions = 0.30 mg/m3. Three consecutive data 

points at or exceeding the peak value constitutes a failure where each test 

value is based on detection sample time of approximately 2 minutes for 8 

hours. 

NOTE: Any visible respirator deterioration in assigned material components such 

as breakage, distortion, hazing of lens, cracking or separation shall also constitute 

a system warning and qualify as a failure based upon lab manager final 

determination with consultation from NIOSH/NPPTL. 

NOTE: Any APR test that fails as a result of laboratory test equipment failure or 

malfunction, laboratory electrical power loss or incorrect technician operating 

procedures/actions will be considered by NIOSH/NPPTL as a test termination and 

immediate mandatory retest upon lab supervisor confirmation. In this case, the 

testing laboratory, at no additional cost to NIOSH/NPPTL or the manufacturer 

concerned, retests the respirator. 

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 Full Facepiece, Tight Fitting, Negative Pressure, P100, APR

submitted for approval, extension of approval, or examined during certification 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 32 of 39 

product audits, meet the minimum certification standards set forth in 42 CFR, 

Part 84, Subpart G, Section 84.63(a)(c)(d). 

7. RECORDS AND TEST DATA SHEETS

7.1. All test data will be recorded in the NIOSH DIEMS and STP recognized 

formatted CBRN APR test data sheets (Appendix D). All applicable data, graphs 

and photographs taken or prepared by laboratory technicians, technician 

supervisors or the equivalent will remain on file at the actual lab where the test 

was conducted, and is required to be retrievable within 24-hour notification and 

maintained in accordance with local administrative SOPs and NIOSH/NPPTL 

Respirator Branch CET historical filing requirements. 

7.2. All videotapes and photographs of the actual test being performed by testing 

laboratory 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 (qualifier or 

remainder application), testing laboratory will send a test report to the 

NIOSH NPPTL Respirator Branch, Equipment Evaluation 

Team/Certification Evaluation and Testing (CET) “Team Leader” and 

await further instructions on return of any uncontaminated hardware to the 

manufacturer. 

7.3.2. If the failure occurs on hardware examined under NIOSH directed off-theshelf audit, the hardware will be examined by a technician and the 

Laboratory Manager for cause. All equipment failing or passing any 

portion of this test will have been contaminated with chemical warfare 

agent. Upon request, the contaminated equipment can be viewed by 

designated NIOSH personnel in support of incident investigation 

proceedings. Upon completion of NIOSH proceedings, the equipment is 

disposed of in accordance with testing laboratory chemical surety 

practices. 

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Appendix D 

CBRN APR HD LAT Certification Test Data Summary Sheet

 (Test Data Sheet 1 of 3)

1. TEST TITLE: Determination of Full Facepiece, Tight Fitting, Negative Pressure, P100, AirPurifying Respirator (APR) Performance During Dynamic Testing Against Chemical Agent 

Distilled Sulfur Mustard (HD) Vapor and Distilled Sulfur Mustard (HD) Liquid. 

A. Task Number (TN): _____________________________________________ 

B. Manufacturer: ________________________________________________ 

C. APR Model #/Type: __________________________________________ 

D. Test Start Date of Qualifier Application: _____________________________ 

E. Test Start Date of Remainder Application: ______________________ 

F. Test End Date of Remainder Application: ______________________ 

G. Primary P/N and Subject for LAT Configuration:______________________ 

2. REQUIREMENT: 

Three of each CBRN Full Facepiece, Tight Fitting, Negative Pressure, Air-Purifying 

Respirators (APR) shall demonstrate no permeation or penetration of Distilled Sulfur 

Mustard (HD) vapor and Distilled Sulfur Mustard (HD) liquid equal to or greater than the 

stated maximum peak excursions and the stated cumulative concentration over time (Ct) 

including all maximum peak excursion data points for the duration of the eight (8) hour 

test. HD vapor challenge concentration will start immediately after the test chamber has 

been sealed. Minimum Service Life for liquid exposure starts after the first liquid drop is 

applied. Liquid volume used is dependent on components used with the respirator. 

Minimum volume of 0.43 mL and maximum volume of 0.86 mL is based on the 

respirator final tested configuration of one APR canister on a specific respirator 

assembly. Three consecutive sequential test data points at or exceeding 0.3 mg/m3 will 

collectively constitute a failure where each test value equals to or exceeds 0.3 mg/m3 and 

is based on a detector sample time of approximately 3 minutes. The cumulative Ct, 

including all maximum peak excursion data points, must not be exceeded for the duration 

of the test. Liquid agent is applied to the complete respirator at hour 6 of the test cycle. 

The test period begins upon initial generation of HD vapor concentration and ends at 8 

hours. 

 OVERALL RESULT: PASS or FAIL

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 37 of 39 

CBRN APR HD LAT Certification Test Data Summary Sheet

 (Test Data Sheet 2 of 3)

3. SUPPORTING REQUIRED DATA: 

A. Has Canister expired prior to LAT in accordance with User Instructions? YES or NO. 

B. Is Canister bent, cracked or disfigured prior to any portion of LAT? YES or NO. 

C. Does Canister to facepiece connection violate Form, Fit or Function? YES or NO. 

D. Is Facepiece fully serviceable prior to any portion of LAT? YES or NO. 

E. Are Sub Assemblies free of visible deformations or aberrations? YES or NO. 

HD CBRN APR LAT Certification Summary Continuum: 

Task Number: _______________________ STP No.: ___________________ 

Manufacturer: _______________________ Reference No.: ___________________ 

Test Title: Determination of Full Facepiece, Tight Fitting, Negative Pressure, Air-Purifying 

Respirator (APR) Performance During Dynamic Testing Against Chemical Agent Distilled Sulfur 

Mustard (HD) Vapor and Distilled Sulfur Mustard (HD) Liquid. 

F. Did each APR pass or fail maximum peak excursions? PASS or FAIL 

G. Did each APR pass or fail Ct? PASS or FAIL 

H. Was all lab test equipment verified calibrated prior to LAT? PASS or FAIL 

QUALIFIER TEST # 1 Total Test Time Max Peak Excursions Ct RESULT

(e.g., TN – HD 1 480 minutes or less Quantity failing Value Pass or Fail) 

REMAINDER TEST # 2 Total Test Time Max Peak Excursions Ct RESULT

(TN – HD 2) Same as above (sab). sab sab sab 

REMAINDER TEST # 3 Total Test Time Max Peak Excursions Ct RESULT

(TN – HD 3.) sab sab sab sab 

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Procedure No. CET-APRS-CBRN-STP-0351 Revision: 0.1 Date: 24 October 2005 Page 38 of 39 

CBRN APR HD LAT Certification Test Data Summary Sheet

 (Test Data Sheet 3 of 3)

4. COMMENTS: 

(e.g., CBRN APR candidate was tested in minimum packaging configuration for initial 

Qualifier Application. CBRN APR passed initial Qualifier Application LAT. However, 

when conditioned configuration was tested in Remainder Application tests, candidate 

CBRN APR failed max peak excursion criteria and exhibited canister thread dents and 

bends as a result of environmental conditioning prior to Remainder LAT.) 

5. SIGNATURES: 

A. Laboratory Technician: _________________________ Date: _______________ 

 (Signature) 

 ________________________ 

 (Printed Name) 

B. Laboratory Supervisor: _________________________ Date: _______________ 

 (Signature) 

 ________________________ 

 (Printed Name) 

Legible Signatures infer concurrence with test summary findings as indicated above. 

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Revision History 

Revision Date Reason for Revision 

0 23 December 2003 Interim Guidance Version: Initial version dated March 18, 

2003 was converted from an interim guidance STP to a draft 

final STP dated December 24, 2003. Integration of actual 

DIEMS test data sheet was standardized between the STP and 

the NIOSH administrative project management system 

(DIEMS). Incorporated new third party laboratory name 

change: SBCCOM to RDECOM.

0.0 30 September 2004 Final STP Version: Incorporated next generation equipment 

guidance on MINICAMS® and syringe pump into STP.

0.1 24 October 2005 Update header and format to reflect lab move from Morgantown, 

WV 

No changes to method 

 

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