ASTM D4600-22

Standard Test Method for Determination of Benzene-Soluble Particulate Matter in Workplace Atmospheres

SIGNIFICANCE AND USE
5.1 This test method provides a means of evaluating exposures to benzene-soluble particulate matter in a concentration range that can be related to occupational exposures.
SCOPE
1.1 This test method describes the sampling and gravimetric determination of benzene-soluble particulate matter that has become airborne as a result of certain industrial processes. This test method can be used to determine the total weight of benzene-soluble materials and to provide a sample that may be used for specific and detailed analyses of the soluble components.  
1.2 The limit of detection is 0.05 mg/m3 by sampling a 1 m3 volume of air.
Note 1: Other volatile organic solvents have been used for this determination and whereas a less toxic solvent for this analysis might be desirable, the substitution of a solvent other than benzene is unwise at this time. A tremendous volume of environmental sampling data based on benzene-soluble determinations has been accumulated over many years in several industries.2 Some of the determinations have been used in epidemiological studies. Furthermore, the use of benzene is specified in existing United States federal standards.3 As a result, it appears imprudent to use a different solvent until the qualitative and quantitative relationship of analyses derived from benzene and a substitute solvent is established. With proper care, benzene can be safely used in the laboratory.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 28-Feb-2022
• ICS: 13.040.30 - Workplace atmospheres
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.04 - Workplace Air Quality

Relations

• Refers: ASTM D1356-20a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Sep-2020
• Refers: ASTM D1356-20 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Mar-2020
• Refers: ASTM D1357-95(2019) - Standard Practice for Planning the Sampling of the Ambient Atmosphere
• Effective Date: 01-Aug-2019
• Refers: ASTM D4840-99(2018)e1 - Standard Guide for Sample Chain-of-Custody Procedures
• Effective Date: 15-Aug-2018
• Refers: ASTM D1356-15a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Oct-2015
• Refers: ASTM D1356-15 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Jul-2015
• Refers: ASTM D1356-14b - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Dec-2014
• Refers: ASTM D1356-14a - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-May-2014
• Refers: ASTM D1356-14 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 15-Jan-2014
• Refers: ASTM D5337-11 - Standard Practice for Flow Rate for Calibration of Personal Sampling Pumps
• Effective Date: 15-Nov-2011
• Refers: ASTM D1357-95(2011) - Standard Practice for Planning the Sampling of the Ambient Atmosphere
• Effective Date: 01-Oct-2011
• Refers: ASTM D1356-05(2010) - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-Apr-2010
• Refers: ASTM D4840-99(2010) - Standard Guide for Sampling Chain-of-Custody Procedures
• Effective Date: 01-Feb-2010
• Refers: ASTM D1356-05 - Standard Terminology Relating to Sampling and Analysis of Atmospheres
• Effective Date: 01-May-2005
• Refers: ASTM D1357-95(2005) - Standard Practice for Planning the Sampling of the Ambient Atmosphere
• Effective Date: 01-Mar-2005

Overview

ASTM D4600-22 is the Standard Test Method for the Determination of Benzene-Soluble Particulate Matter in Workplace Atmospheres, developed and published by ASTM International. This test method provides a precise and reliable means to assess occupational exposure to benzene-soluble particulate matter (BSPM) within industrial settings. Widely referenced in the fields of occupational safety, air monitoring, and industrial hygiene, ASTM D4600-22 enables laboratories and industrial hygienists to sample workplace atmospheres, gravimetrically determine total BSPM, and generate samples for further component analysis. Its procedures and requirements align with international standards for air quality and workplace health monitoring.

Key Topics

• Sampling and Gravimetric Determination
  The method details protocols for collecting airborne particulate matter using personal sampling pumps and glass-fiber filters, followed by extraction with benzene and accurate gravimetric analysis.

• Detection Limits and Sensitivity
  This standard achieves a limit of detection as low as 0.05 mg/m³ when sampling 1 cubic meter of air, providing effective monitoring capabilities for compliance purposes.

• Occupational Exposure Evaluation
  ASTM D4600-22 plays a critical role in evaluating worker exposures to benzene-soluble fractions, especially in industries where airborne particulate emissions are a concern.

• Chain of Custody and Quality Control
  Strict protocols for sample chain-of-custody (referencing ASTM D4840), use of field and laboratory blanks, and thorough documentation ensure integrity and traceability of results.

• Interpretation and Reporting
  The method supports comprehensive reporting of sample handling, analytical results, and quality assurance data to underpin occupational health decisions.

• Safety Considerations
  The standard emphasizes the handling of benzene-a known hazardous substance-according to established health, safety, and environmental practices.

Applications

• Industrial Hygiene and Occupational Safety
  Used extensively in refineries, coke plants, production facilities, and industries handling coal tar pitch volatiles, this method helps assess employee exposure to hazardous airborne particulates.

• Regulatory Compliance
  ASTM D4600-22 supports compliance with United States federal standards and workplace air quality regulations that specifically reference benzene-soluble measurements.

• Epidemiological and Exposure Studies
  BSPM measurements obtained via this test method inform epidemiological studies focused on long-term health impacts from industrial air contaminants.

• Environmental Air Sampling
  Although designed for workplace monitoring, the method may be employed in ambient air sampling for community health assessments adjacent to industrial operations.

• Laboratory Analysis and Research
  The gravimetric sample produced can be used for detailed chemical analysis of soluble particulate components, supporting research into the composition of airborne hazards.

Related Standards

For a comprehensive workplace air quality management program, ASTM D4600-22 should be considered alongside these related standards and references:

• ASTM D1356 - Terminology Relating to Sampling and Analysis of Atmospheres
• ASTM D1357 - Practice for Planning the Sampling of the Ambient Atmosphere
• ASTM D4840 - Guide for Sample Chain-of-Custody Procedures
• ASTM D5337 - Practice for Flow Rate Adjustment of Personal Sampling Pumps
• ASTM D8358 - Guide for Assessment and Inclusion of Wall Deposits in the Analysis of Single-Stage Samplers
• ISO/IEC 17025 - General Requirements for the Competence of Testing and Calibration Laboratories

Keywords: benzene-soluble particulate matter, workplace atmospheres, air monitoring, gravimetric analysis, industrial hygiene, ASTM D4600, exposure assessment, coal tar pitch volatiles, occupational safety, sampling and analysis

By implementing ASTM D4600-22, organizations can ensure accurate, internationally recognized methodologies for the determination of benzene-soluble particulates, supporting healthier workplace environments and regulatory compliance.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4600 − 22
Standard Test Method for
Determination of Benzene-Soluble Particulate Matter in
Workplace Atmospheres
This standard is issued under the fixed designation D4600; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 Thistestmethoddescribesthesamplingandgravimetric
Barriers to Trade (TBT) Committee.
determination of benzene-soluble particulate matter that has
becomeairborneasaresultofcertainindustrialprocesses.This
2. Referenced Documents
test method can be used to determine the total weight of
2.1 ASTM Standards:
benzene-soluble materials and to provide a sample that may be
D1356 Terminology Relating to Sampling and Analysis of
used for specific and detailed analyses of the soluble compo-
Atmospheres
nents.
D1357 Practice for Planning the Sampling of the Ambient
3 3
1.2 The limit of detection is 0.05 mg/m by sampling a 1 m
Atmosphere
volume of air.
D4840 Guide for Sample Chain-of-Custody Procedures
NOTE 1—Other volatile organic solvents have been used for this
D5337 Practice for Flow RateAdjustment of Personal Sam-
determination and whereas a less toxic solvent for this analysis might be
pling Pumps
desirable, the substitution of a solvent other than benzene is unwise at this
D8358 GuideforAssessmentandInclusionofWallDeposits
time. A tremendous volume of environmental sampling data based on
in the Analysis of Single-Stage Samplers for Airborne
benzene-soluble determinations has been accumulated over many years in
several industries. Some of the determinations have been used in Particulate Matter
epidemiological studies. Furthermore, the use of benzene is specified in
2.2 Other Documents:
existing United States federal standards. As a result, it appears imprudent
ISO/IEC 17025 General requirements for the competence of
to use a different solvent until the qualitative and quantitative relationship
testing and calibration laboratories
of analyses derived from benzene and a substitute solvent is established.
With proper care, benzene can be safely used in the laboratory.
3. Terminology
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3.1 Definitions: For definitions of terms used in this test
standard. method, refer to Terminology D1356.
1.4 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 By the use of a personal sampling pump, air is pulled
throughaglass-fiberfilterheldinasamplingcassette.Thefilter
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. is extracted ultrasonically with benzene. After filtration, an
aliquot of the total extract is evaporated to dryness and the
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard- residue weighed.
ization established in the Decision on Principles for the
5. Significance and Use
5.1 This test method provides a means of evaluating expo-
This test method is under the jurisdiction of ASTM Committee D22 on Air sures to benzene-soluble particulate matter in a concentration
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air
range that can be related to occupational exposures.
Quality.
Current edition approved March 1, 2022. Published June 2022. Originally
approved in 1986. Last previous edition approved in 2016 as D4600 – 95 (2016).
DOI: 10.1520/D4600-22. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
“Benzene-Soluble Compounds in Air, P&CAM 217,” NIOSH Manual of contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Analytical Methods, 2nd Ed., DHEW (NIOSH) Pub. No. 77-157-A, National Standards volume information, refer to the standard’s Document Summary page on
Institute of Occupational Safety and Health, Cincinnati, OH 1977. the ASTM website.
3 5
“Appendix B—Industrial Hygiene and Medical Surveillance Guidelines,” Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
20CFR 1910.1029 Coke Oven Emissions. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4600 − 22
6. Interferences 7.9 Weighing Cups, aluminum or PTFE of suitable capacity
with a weight not to exceed 500 mg.
6.1 This test method is, by definition, free of interferences.
7.10 Vacuum Oven.
However, this test method is nonspecific. It supplies no
information on the composition of the soluble material. It
8. Reagent
measures all those substances in the sample that are soluble in
8.1 Benzene—The benzene used should be of sufficient
benzene. The composition must be determined by some inde-
puritysothattheresidueweightfollowingevaporationof5mL
pendent means.
of the solvent is less than 10 µg.
6.2 The greatest errors most likely to be incurred in the use
9. Safety Precautions
of this test method are associated with the sample collection or
high blanks from solvent and filter. Avoid contamination from
9.1 To minimize the exposure hazard to benzene, analysts
extraneous material by using high-purity solvents for the final
should avoid inhalation of solvent vapors and, if indicated, be
cleaning of all apparatus. The use of plastic containers other
monitored to determine the magnitude of their exposures.
than polytetrafluoroethylene (PTFE) for any organic solvent is
Transferandevaporationofthesolventshouldbecarriedoutin
unacceptable, and the evaporation step should be conducted in
a properly ventilated fume hood (150-fpm face velocity).
a clean hood.
Protective gloves should be used to minimize the possibility of
absorbing benzene through the skin. See safety data sheets
7. Apparatus
(SDS) for additional hazard and handling information.
7.1 Personal Sampling Pumps, any pump capable of sam-
9.2 The extract must be handled with proper caution be-
pling at a rate of about 2 L/min for 8 h.
cause some polycyclic aromatic hydrocarbons are potential
carcinogens.
7.2 Flow Measuring Device, used in accordance with Prac-
tice D5337.
10. Sampling
7.3 Flexible Tubing, of a diameter suitable for making a
10.1 Refer to Practices D1357 for general information on
leak-proofconnectionfromthepersonalsamplingpumpstothe
sampling
samplers.
10.2 Adjust the personal sampling pumps to about 2 L/min
7.4 Glass-Fiber Filters, 37 mm, free of organic binder, held with an assembled cassette between the pump and the flow-
in a two- or three-piece polystyrene cassette having a rigid measuring device, using a flexible tubing, in accordance to
filter support. Filters should be pre-extracted or preheated at Practice D5337. After the sampling, perform a post sampling
400 °C for a minimum of 1 h. flow rate verification. Pre- and post-sampling flow rates are
expected to be within 65 % of a nominal value, in which case
7.4.1 There exists the possibility that sample may enter the
the nominal value can be used, or within 65 % of each other,
sampling cassette and be collected on the inner surfaces of the
when the average value can be used. If the difference between
sampler rather than on the filter. The use of conductive plastic
the two measurements is greater than 65 % then the sample
cassettes rather than polystyrene should reduce the amount of
shall be flagged and the two separate results recorded, or th
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4600 − 95 (Reapproved 2016) D4600 − 22
Standard Test Method for
Determination of Benzene-Soluble Particulate Matter in
Workplace Atmospheres
This standard is issued under the fixed designation D4600; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes the sampling and gravimetric determination of benzene-soluble particulate matter that has become
airborne as a result of certain industrial processes. This test method can be used to determine the total weight of benzene-soluble
materials and to provide a sample that may be used for specific and detailed analyses of the soluble components.
3 3
1.2 The limit of detection is 0.05 mg/m by sampling a 1-m1 m volume of air.
NOTE 1—Other volatile organic solvents have been used for this determination and whereas a less toxic solvent for this analysis might be desirable, the
substitution of a solvent other than benzene is unwise at this time. A tremendous volume of environmental sampling data based on benzene-soluble
determinations has been accumulated over many years in several industries. Some of the determinations have been used in epidemiological studies.
Furthermore, the use of benzene is specified in existing United States federal standards. As a result, it appears imprudent to use a different solvent until
the qualitative and quantitative relationship of analyses derived from benzene and a substitute solvent is established. With proper care, benzene can be
safely used in the laboratory.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D1357 Practice for Planning the Sampling of the Ambient Atmosphere
D4840 Guide for Sample Chain-of-Custody Procedures
D5337 Practice for Flow Rate Adjustment of Personal Sampling Pumps
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality.
Current edition approved May 15, 2016March 1, 2022. Published May 2016June 2022. Originally approved in 1986. Last previous edition approved in 20102016 as
D4600 – 95 (2010).(2016). DOI: 10.1520/D4600-95R16.10.1520/D4600-22.
“Benzene-Soluble Compounds in Air, P&CAM 217,” NIOSH Manual of Analytical Methods, 2nd Ed., DHEW (NIOSH) Pub. No. 77-157-A, National Institute of
Occupational Safety and Health, Cincinnati, OH 1977.
“Appendix B—Industrial Hygiene and Medical Surveillance Guidelines,” 20CFR 1910.1029 Coke Oven Emissions.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4600 − 22
D8358 Guide for Assessment and Inclusion of Wall Deposits in the Analysis of Single-Stage Samplers for Airborne Particulate
Matter
2.2 Other Documents:
ISO/IEC 17025 General requirements for the competence of testing and calibration laboratories
3. Terminology
3.1 Definitions: For definitions of terms used in this test method, refer to Terminology D1356.
4. Summary of Test Method
4.1 By the use of a personal sampling pump, air is pulled through a glass-fiber filter held in a sampling cassette. The filter is
extracted ultrasonically with benzene. After filtration, an aliquot of the total extract is evaporated to dryness and the residue
weighed.
5. Significance and Use
5.1 This test method provides a means of evaluating exposures to benzene-soluble particulate matter in a concentration range that
can be related to occupational exposures.
6. Interferences
6.1 This test method is, by definition, free of interferences. However, this test method is nonspecific. It supplies no information
on the composition of the soluble material. It measures all those substances in the sample that are soluble in benzene. The
composition must be determined by some independent means.
6.2 The greatest errors most likely to be incurred in the use of this test method are associated with the sample collection or high
blanks from solvent and filter. Avoid contamination from extraneous material by using high-purity solvents for the final cleaning
of all apparatus. The use of plastic containers other than TFE-fluorocarbon polytetrafluoroethylene (PTFE) for any organic solvent
is unacceptable, and the evaporation step should be conducted in a clean hood.
7. Apparatus
7.1 Personal Sampling Pumps, any pump capable of sampling at a calibration rate of about 2 L/min for 8 h.
7.2 Flow Measuring Device, used in accordance with Practice D5337.
7.3 Flexible Tubing, of a diameter suitable for making a leak-proof connection from the personal sampling pumps to the samplers.
7.4 Glass-Fiber Filters, 37-mm,37 mm, free of organic binder, held in a two- or three-piece polystyrene cassette having a rigid
filter support. Filters should be pre-extracted or preheated at 400°C400 °C for a minimum of 1 h.
7.4.1 There exists the possibility that sample may enter the sampling cassette and be collected on the inner surfaces of the sampler
rather than on the filter. The use of conductive plastic cassettes rather than polystyrene should reduce the amount of fine particulate
electrostatically attracted to the inner walls of the cassette, but may not eliminate the issue entirely. See Guide D8358 for additional
guidance on including non-filter sampler deposits for analysis
7.5 Extraction Vessel, 25-mL25 mL Erlenmeyer flask, 8-dram vial or any glass container of 1010 mL to 25-mL25 mL capacity
having a TFE-fluorocarbon-linedPTFE-lined screw cap (a 50-mL50 mL beaker is suitable if entire sample is to be used for the
benzene-soluble determination).
7.6 Ultrasonic Bath, 100100 W to 500 W, sufficient to disperse the particulate without destroying the glass-fiber matrix.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
D4600 − 22
7.7 Filtration Apparatus—AllihnAllign tubes with fine porosity fritted glass, 30 mL; Gelman Acrodisc CR disposable syringe
filter (0.45(0.45 μm to 1.0 μm 1.0 μm pore size) attached to a 55 mL to 10-mL10 mL syringe having a Luer tip; or other equivalent
suitable media.
NOTE 2—When using a disposable syringe filter, prewash with 10 mL of acetonitrile.
NOTE 3—Placing a pre-extracted filter (37-mm(37 mm glass fiber) ahead of the fritted glass in the Allihn tube will increase the life of the frit.
7.8 Microbalance, capable of weighing to 1 μg. with a resolution of 10 μg. (If entire sample is to be used for the benzene-soluble
determination, a five-placefive-decimal balance is acceptable.)
7.9 Weighing Cups, aluminum or TFE-fluorocarbonPTFE of suitable capacity with a weight not to exceed 500 mg.
7.10 Vacuum Oven.
8. Reagent
8.1 Benzene—The benzene used should be of sufficient purity so that the residue weight following evaporation of 5 mL of the
solvent is less than 10 μg.
9. Safety Precautions
9.1 To minimize the e
...