ASTM D7771-17a

Standard Test Method for Determination of Benzo-α-Pyrene (BaP) Content in Carbon Black

SIGNIFICANCE AND USE
5.1 This test procedure is used to determine the concentration of BaP extracted from carbon black by the means of a Soxhlet extraction apparatus with toluene.
SCOPE
1.1 This test method covers the qualitative and quantitative determination of only benzo-α-pyrene (BaP), a specific polycyclic aromatic hydrocarbon (PAH), on carbon black. The procedure involves Soxhlet extraction with toluene and analysis by gas chromatography with mass spectrometry (GC/MS). This method is not intended to test for U.S. Food and Drug Administration (FDA 21 CFR 178.3297) compliance of carbon blacks used for indirect food contact applications.  
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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: Historical
• Publication Date: 30-Sep-2017
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.66 - Environment, Health, and Safety

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7771 − 17a
Standard Test Method for
Determination of Benzo-α-Pyrene (BaP) Content in Carbon
1
Black
This standard is issued under the fixed designation D7771; 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.
3
1. Scope 2.2 EPA Standard:
Method 8270D Semivolatile Organic Compounds by Gas
1.1 This test method covers the qualitative and quantitative
Chromatography/Mass Spectrometry (GC/MS)
determination of only benzo-α-pyrene (BaP), a specific poly-
2.3 Federal Standard:
cyclic aromatic hydrocarbon (PAH), on carbon black. The
21 CFR 178.3297 Indirect Food Additives: Adjuvants, Pro-
procedure involves Soxhlet extraction with toluene and analy-
4
ductions Aids, and Sanitizers, Colorants for Polymers
sis by gas chromatography with mass spectrometry (GC/MS).
This method is not intended to test for U.S. Food and Drug
3. Terminology
Administration (FDA21 CFR 178.3297) compliance of carbon
3.1 Definitions of Terms Specific to This Standard:
blacks used for indirect food contact applications.
3.1.1 benzo-α-pyrene, BaP, n—also known as 3,4-
1.2 Units—The values stated in SI units are to be regarded
benzopyrene or benzo-a-pyrene is a specific polycyclic aro-
as the standard. No other units of measurement are included in
matic hydrocarbon (PAH) or polynuclear aromatic hydrocar-
this standard.
bon that consists of fused aromatic rings with no heteroatom or
substituent.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1.1.1 Discussion—PAHs naturally occur in oil, coal, and
tar deposits; are produced by the incomplete combustion of
responsibility of the user of this standard to establish appro-
hydrocarbons;andoccurinmanyotherproductsandprocesses.
priate safety, health, and environmental practices and deter-
BaP is a pentacyclic PAH with the formula C H , related to
mine the applicability of regulatory limitations prior to use.
20 12
pyrene by fusion of a phenylene group in the alpha position.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
4. Summary of Test Method
ization established in the Decision on Principles for the
4.1 A portion of carbon black is Soxhlet-extracted with
Development of International Standards, Guides and Recom-
toluene for 16 h. The extract is concentrated and subsequently
mendations issued by the World Trade Organization Technical
analyzed for BaPby gas chromatography with mass spectrom-
Barriers to Trade (TBT) Committee.
etry (GC/MS). The BaP quantification is performed by the
2. Referenced Documents
means of an internal standard.
2
2.1 ASTM Standards:
5. Significance and Use
D4483 Practice for Evaluating Precision for Test Method
5.1 This test procedure is used to determine the concentra-
Standards in the Rubber and Carbon Black Manufacturing
tion of BaP extracted from carbon black by the means of a
Industries
Soxhlet extraction apparatus with toluene.
6. Apparatus
1
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
Black and is the direct responsibility of Subcommittee D24.66 on Environment,
6.1 Soxhlet Extractor with Reflux Condenser, 50- or 100-
3
Health, and Safety.
cm capacity.
Current edition approved Oct. 1, 2017. Published November 2017. Originally
approved in 2011. Last previous edition approved in 2017 as D7771 – 17. DOI:
3
10.1520/D7771-17A. Available from United States Environmental Protection Agency (EPA), Ariel
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20004, http://
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.epa.gov/epaoswer/hazwaste/test/new-meth.htm#8270D.
4
Standards volume information, refer to the standard’s Document Summary page on Available from the U.S. Government Printing Office, Superintendent of
the ASTM website. Documents, 732 N. Capital St., NW., Washington, DC 20402-0001.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7771 − 17a
TABLE 1 Native and Deuterated BaP Compounds
C13 Labeled
Native PAH CAS# Deuterated PAH CAS# CAS#
PAH
Benzo-α-pyrene 50-32-8 d -Benzo-α-pyrene 63466-71-7 13C -Benzo-α- Not Available
12 4
pyrene
6.2 Extraction Thimbles, glass or cellulose, approximately 6.17 Drying Oven, gravity convection type, capable of
3
50- to 70-cm capacity. For instance, glass extraction thimble maintaining 40 6 10°C, used for slowing down the cooli
...

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: D7771 − 17 D7771 − 17a
Standard Test Method for
Determination of Benzo-α-Pyrene (BaP) Content in Carbon
1
Black
This standard is issued under the fixed designation D7771; 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 covers the qualitative and quantitative determination of only benzo-α-pyrene (BaP), a specific polycyclic
aromatic hydrocarbon (PAH), on carbon black. The procedure involves Soxhlet extraction with toluene and analysis by gas
chromatography with mass spectrometry (GC/MS). This method is not intended to test for U.S. Food and Drug Administration
(FDA 21 CFR 178.3297) compliance of carbon blacks used for indirect food contact applications.
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this
standard.
1.3 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.
1.4 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
2.1 ASTM Standards:
D4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
3
2.2 EPA Standard:
Method 8270D Semivolatile Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS)
2.3 Federal Standard:
4
21 CFR 178.3297 Indirect Food Additives: Adjuvants, Productions Aids, and Sanitizers, Colorants for Polymers
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 benzo-α-pyrene, BaP, n—also known as 3,4-benzopyrene or benzo-a-pyrene is a specific polycyclic aromatic hydrocarbon
(PAH) or polynuclear aromatic hydrocarbon that consists of fused aromatic rings with no heteroatom or substituent.
3.1.1.1 Discussion—
PAHs naturally occur in oil, coal, and tar deposits; are produced by the incomplete combustion of hydrocarbons; and occur in many
other products and processes. BaP is a pentacyclic PAH with the formula C H , related to pyrene by fusion of a phenylene group
20 12
in the alpha position.
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.66 on Environment, Health,
and Safety.
Current edition approved Jan. 1, 2017Oct. 1, 2017. Published January 2017November 2017. Originally approved in 2011. Last previous edition approved in 20152017
as D7771 – 15.D7771 – 17. DOI: 10.1520/D7771-17.10.1520/D7771-17A.
2
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.
3
Available from United States Environmental Protection Agency (EPA), Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20004, http://www.epa.gov/
epaoswer/hazwaste/test/new-meth.htm#8270D.
4
Available from the U.S. Government Printing Office, Superintendent of Documents, 732 N. Capital St., NW., Washington, DC 20402-0001.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7771 − 17a
4. Summary of Test Method
4.1 A portion of carbon black is Soxhlet-extracted with toluene for 16 h. The extract is concentrated and subsequently analyzed
for BaP by gas chromatography with mass spectrometry (GC/MS). The BaP quantification is performed by the means of an internal
standard.
5. Significance and Use
5.1 This test procedure is used to determine the concentration of BaP extracted from carbon black by the means of a Soxhlet
extraction apparatus with toluene.
6. Apparatus
3
6.1 Soxhlet Extractor with Reflux Condenser, 50- or 100-cm capacity.
3
6.2 Extraction Thimbles, glass or cellulose, approximately 50- to 70-cm capac
...