ASTM D7771-17

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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Dec-2016
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.66 - Environment, Health, and Safety

Relations

• Replaces: ASTM D7771-15 - Standard Test Method for Determination of Benzo-α-Pyrene (BaP) Content in Carbon Black
• Effective Date: 01-Jan-2017
• Referred By: ASTM D8466-22 - Standard Guide for Recovered Carbon Black—Carbon Black Test Methods for Testing rCB
• Effective Date: 01-Jan-2017

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 17
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 2.3 Federal Standard:
21 CFR 178.3297 Indirect Food Additives: Adjuvants, Pro-
1.1 This test method covers the qualitative and quantitative
4
ductions Aids, and Sanitizers, Colorants for Polymers
determination of only benzo-α-pyrene (BaP), a specific poly-
cyclic aromatic hydrocarbon (PAH), on carbon black. The
3. Terminology
procedure involves Soxhlet extraction with toluene and analy-
3.1 Definitions of Terms Specific to This Standard:
sis by gas chromatography with mass spectrometry (GC/MS).
3.1.1 benzo-α-pyrene, BaP, n—also known as 3,4-
This method is not intended to test for U.S. Food and Drug
benzopyrene or benzo-a-pyrene is a specific polycyclic aro-
Administration (FDA21 CFR 178.3297) compliance of carbon
matic hydrocarbon (PAH) or polynuclear aromatic hydrocar-
blacks used for indirect food contact applications.
bon that consists of fused aromatic rings with no heteroatom or
1.2 Units—The values stated in SI units are to be regarded
substituent.
as the standard. No other units of measurement are included in
3.1.1.1 Discussion—PAHs naturally occur in oil, coal, and
this standard.
tar deposits; are produced by the incomplete combustion of
1.3 This standard does not purport to address all of the hydrocarbons;andoccurinmanyotherproductsandprocesses.
safety concerns, if any, associated with its use. It is the BaP is a pentacyclic PAH with the formula C H , related to
20 12
responsibility of the user of this standard to establish appro- pyrene by fusion of a phenylene group in the alpha position.
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 A portion of carbon black is Soxhlet-extracted with
2. Referenced Documents
toluene for 16 h. The extract is concentrated and subsequently
2
analyzed for BaPby gas chromatography with mass spectrom-
2.1 ASTM Standards:
etry (GC/MS). The BaP quantification is performed by the
D4483 Practice for Evaluating Precision for Test Method
means of an internal standard.
Standards in the Rubber and Carbon Black Manufacturing
Industries
5. Significance and Use
3
2.2 EPA Standard:
5.1 This test procedure is used to determine the concentra-
Method 8270D Semivolatile Organic Compounds by Gas
tion of BaP extracted from carbon black by the means of a
Chromatography/Mass Spectrometry (GC/MS)
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-
Health, and Safety.
3
cm capacity.
Current edition approved Jan. 1, 2017. Published January 2017. Originally
approved in 2011. Last previous edition approved in 2015 as D7771 – 15. DOI:
6.2 Extraction Thimbles, glass or cellulose, approximately
10.1520/D7771-17.
3
50- to 70-cm capacity. For instance, glass extraction thimble
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 of 35-mm diameter by 90-mm height with course porosity (70
Standards volume information, refer to the standard’s Document Summary page on
to 100 µm similar to Ace Glass Size C, Porosity B, Code-14).
the ASTM website.
3
Available from United States Environmental Protection Agency (EPA), Ariel
4
Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20004, http:// Available from the U.S. Government Printing Office, Superintendent of
www.epa.gov/epaoswer/hazwaste/test/new-meth.htm#8270D. 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 − 17
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
6.3 Heating Mantle,compatiblewithboilingflaskdescribed 6.18 Furnace, capable of temperature regulation of 500 6
in 6.4. 25°C, used to burn off organic contamination from glass
3 surfaces.
6.4 Boiling Flasks for Soxhlet, for example, 250 cm .
6.19 Manometer, capable of pressure readings in the range
6.5 Glass Beads, approximately 180 to
...

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 − 15 D7771 − 17
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 and health practices and determine the applicability of regulatory
limitations prior to use.
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 consistconsists of fused aromatic rings with no heteroatom or substituent.
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, 2015Jan. 1, 2017. Published February 2015January 2017. Originally approved in 2011. Last previous edition approved in 20132015 as
D7771 – 13.D7771 – 15. DOI: 10.1520/D7771-15.10.1520/D7771-17.
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.
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.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7771 − 17
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 capacity. For instance, glass extraction thimble of
35-mm diameter by 90-mm height with course porosity (70 to 100 μm similar to Ace Glass Size C, Porosity B, Code-14).
6.3 Heating Mantle, compatible with boiling flask described in 6.4.
3
6.4 Boiling Flasks for Soxhlet, for example, 250 cm .
6.5 Glass Beads, approximately 180 to 250 μm (60/80 mesh) if
...