ASTM D8143-17(2022)

Standard Test Method for Determination of the EU-8 List of PAH Compounds in Carbon Black

SIGNIFICANCE AND USE
5.1 This test procedure is used to determine the individual concentrations of the PAH compounds in the EU-8 list 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 the EU-8 list of polycyclic aromatic hydrocarbons (PAH) on carbon black. The EU-8 list of PAH compounds is given in Table 1. The procedure involves Soxhlet extraction with toluene followed by extract analysis using 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: Published
• Publication Date: 31-May-2022
• ICS: 13.100 - Occupational safety. Industrial hygiene
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.66 - Environment, Health, and Safety

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: D8143 − 17 (Reapproved 2022)
Standard Test Method for
Determination of the EU-8 List of PAH Compounds in
Carbon Black
This standard is issued under the fixed designation D8143; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 polycyclic aromatic hydrocarbon, PAH, n—organic
compound(s) that consist of chemical structures of alternating
1.1 This test method covers the qualitative and quantitative
single and double bonds of a ring like nature (for example,
determination of the EU-8 list of polycyclic aromatic hydro-
benzene), with no heteroatom or other substituents; frequently
carbons (PAH) on carbon black. The EU-8 list of PAH
the rings are fused to make larger chemical structures.
compoundsisgiveninTable1.TheprocedureinvolvesSoxhlet
3.1.1.1 Discussion—PAHnaturallyoccurinoil,coal,andtar
extraction with toluene followed by extract analysis using gas
deposits; are produced by the incomplete combustion of
chromatography with mass spectrometry (GC/MS). This
hydrocarbons;andoccurinmanyotherproductsandprocesses.
method is not intended to test for U.S. Food and Drug
Administration(FDA21CFR178.3297)complianceofcarbon
3.1.2 EU-8 PAH compound list, n—a list of eight polycyclic
blacks used for indirect food contact applications.
aromatic hydrocarbons that are specified by the Commission
Regulation (EU) 1272/2013 (December 6, 2013) amending
1.2 Units—The values stated in SI units are to be regarded
Annex XVII to Regulation (EC) 1907/2006 of the European
as the standard. No other units of measurement are included in
Parliament and of the Council on the Registration, Evaluation,
this standard.
Authorisation and Restriction of Chemicals (REACH) as
1.3 This standard does not purport to address all of the
regards polycyclic aromatic hydrocarbons (2013) OJ L328/69.
safety concerns, if any, associated with its use. It is the
3.1.2.1 Discussion—Regulation (EU) No. 1272/2013 sets
responsibility of the user of this standard to establish appro-
PAH concentration limits on finished products specified by
priate safety, health, and environmental practices and deter-
their application. The regulation does not refer directly to
mine the applicability of regulatory limitations prior to use.
carbon black, though in many instances and for formulation
1.4 This international standard was developed in accor-
purposes there is a need to know the quantitative, extractable
dance with internationally recognized principles on standard-
PAH content present in carbon black that will become part of
ization established in the Decision on Principles for the
the finished product. In addition, no specific test method has
Development of International Standards, Guides and Recom-
been defined by the regulation for testing finished products or
mendations issued by the World Trade Organization Technical
raw materials used in the finished products.
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
2. Referenced Documents
4.1 A portion of carbon black is Soxhlet-extracted with
2.1 Federal Standard:
toluene for 48 h. The extract is concentrated and subsequently
21 CFR 178.3297Indirect Food Additives: Adjuvants, Pro-
analyzed for specific PAH compounds by gas chromatography
ductions Aids, and Sanitizers, Colorants for Polymers
with mass spectrometry (GC/MS). Each PAH compound is
quantified individually using internal and external standards.
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
5. Significance and Use
5.1 This test procedure is used to determine the individual
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
concentrations of the PAH compounds in the EU-8 list ex-
Black and is the direct responsibility of Subcommittee D24.66 on Environment,
tractedfromcarbonblackbythemeansofaSoxhletextraction
Health, and Safety.
apparatus with toluene.
CurrenteditionapprovedJune1,2022.PublishedJuly2022.Originallyapproved
in 2017. Last previous edition approved in 2017 as D8143–17. DOI: 10.1520/
D8143-17R22.
Available from U.S. Government Printing Office, Superintendent of
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:// Commission Regulation (EU) No 1272/2013 of 6 December 2013.Available at
www.access.gpo.gov. http://eur-lex.europa.eu/eli/reg/2013/1272/oj.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8143 − 17 (2022)
TABLE 1 EU-8 PAH Compounds and Internal Standards
Native PAH CAS# Deuterated Internal Standard CAS#
Benz[a]anthracene 56-55-3 Chrysene-d12 1719-03-5
Chrysene 218-01-9 Benzo[a]pyrene-d12 63466-71-7
Benzo[b]fluoranthene 205-99-2 1,12-Benzoperylene-d12 93951-66-7
Benzo[j]fluoranthene 205-82-3 Perylene-d12 1520-96-3
Benzo[k]fluoranthene 207-08-9
Benzo[e]pyrene 192-97-2
Benzo[a]pyrene 50-32-8
Dibenz[a,h]anthracene 53-70-3
6. Apparatus 6.12 Adjustable Micropipettes, for example 1000, 200, and
3 20 µL, or similar analytical-grade volume measuring equip-
6.1 Soxhlet Extractor with Reflux Condenser, 50 or 100 cm
ment.
capacity.
6.13 Microliter Syringes of Different Volumes, for example,
6.2 Extraction Thimbles, glass or cellulose, approximately
10 and 100 µL.
50to70cm capacity.Forinstance,glassextractionthimbleof
35 mm diameter by 90 mm height with course porosity (70 to 6.14 Volumetric Flasks, for example 10 and 100 cm .
100 µm similar to Ace Glass Size C, Porosity B, Code-14).
6.15 Analytical Balance, with an accuracy of 0.1 mg.
6.3 Heating Mantle,compatiblewithboilingflaskdescribed
6.16 Furnace, capable of temperature regulation of 500 6
in 6.4.
25°C, used to burn off organic contamination from glass
6.4 Boiling Flasks for Soxhlet, for example, 250 cm . surfaces.
6.5 Glass Beads, approximately 180 to 250 µm (60/80 6.17 Manometer, capable of pressure readings in the range
mesh) if glass thimbles are used. Need to be very clean or of 5 6 0.3 kPa for controlling vacuum evaporators.
toluene extracted.
7. Reagents and Materials
6.6 Glass Boiling Beads, approximately 3 mm.
7.1 Purity of Reagents—Reagent-grade chemicals shall be
6.7 Glass Wool, need to be very clean or toluene extracted.
used in all tests. Unless otherwise indicated, it is intended that
6.8 Rotary Evaporator, with temperature-controlled water
all reagents conform to the specifications of the Committee on
bath, automatic pressure regulation, and solvent-proof mem-
Analytical Reagents of theAmerican Chemical Society where
brane vacuum pump. Other evaporators may be used if they
such specifications are available. Other grades may be used,
produce acceptable results.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
6.9 Nitrogen Blow-Down Apparatus, equipped with a con-
the determination.
trolled water bath and nitrogen pressure control.
7.2 Stock solutions or mixtures of the native PAH standards
6.10 Pear-Shaped Flasks for Rotary Evaporator, for
and of the internal standard (deuterated PAH compounds) can
example, 25, 50, and 100 cm .
be purchased as premade solutions or prepared from solid
6.11 GC/MS, with autosampler.
materials (Table 1).
6.11.1 Mass Spectrometer (MS), with electron impact capa- 3
7.2.1 Aconcentration range of 80 to 100 µg/cm for each of
bility and Selected Ion Monitoring (SIM) mode.
the native PAH analytes is recommended for a stock solution
6.11.2 GC Capillary Column, usually a nonpolar GC col-
mixture.
umn composed of 5 % diphenyl/95 % dimethyl polysiloxane
7.2.2 Asimilar concentration range of 80 to 100 µg/cm for
coating is used for PAH analysis. Other similar column phases
each of the deuterated internal standard compounds is recom-
may be used if they provide acceptable peak resolutions.
mended for the internal standard (IS) stock solution.
6.11.3 Deactivated Straight Borosilicate Liner with Small
7.2.3 Allpurchasedstandardmaterialsshallbe98%pureor
Piece of Deactivated Glass Wool—This liner may be used as
better and certified with respect to their purity and concentra-
long as peak resolution is satisfactory.
tion by the manufacturer. Follow the manufacturer’s recom-
6.11.4 Alternative liner is a split/splitless nondeactivated
mendation on how to store the standard solutions and their
liner with glass wool (4 mm internal diameter, straight liner).
recommended expiration date. Typically, the stock solutions
This shall be deactivated with a silanizing agent before use.
are protected from light and stored at room temperature. They
Another alternative is a split/splitless liner with fluorocarbon
shouldbecheckedforsignsofdegradationorevaporation.The
liner seals. Such a liner will already contain conditioned
silanized glass wool. Other liners can be used if they produce
acceptable results.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
6.11.5 Gold-Plated Seal, for GC injector port or similar
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
nonreactive seal.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
6.11.6 GC/MS Amber Autosampler Vials, with polytetra-
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
fluoroethylene (PTFE)-coated caps. copeial Convention, Inc. (USPC), Rockville, MD.
D8143 − 17 (2022)
standard stock solutions shall be replaced/recertified on a properties. Solvents used are flammable.Appropriate personal
yearlybasisorsoonerifcomparisonswithqualitycontrol(QC) protection equipment (PPE) shall be used.
samples indicate a problem.
9. Preparation of Standard Solutions
7.3 Toluene, suitable for high resolution gas chromatogra-
9.1 TheGC/MSinstrumentiscalibratedusingfivesolutions
phy analysis (99.99 % pure).
of the PAH mixture in which internal standards (IS) have also
7.4 Cyclohexane, suitable for high resolution gas chroma-
been added. The recommended external standard concentra-
tography analysis (99.99 % pure). 3
tions are to cover a range of 0.0125 to 1.0 µg/cm . Other
7.5 Helium, GC/MS purity grade. concentrations may be used as needed for the application. The
IS concentration is kept constant within the calibration range.
7.6 Nitrogen, analytical purity grade.
Preferably the IS concentration is in the middle of the selected
7.7 Silica gel columns for Solid Phase Extraction (SPE)
calibration range (for example, 0.3 to 0.6 µg/cm ). A lower
removal of polar compounds.
PAH concentration range can be used for high-purity carbon
7.7.1 SilicaSPECartridges,single-useapplication,havinga
blacks. However, the IS concentration should maintain an S/N
3 5
volume capacity of approximately 1 to 10 cm .
ratio of at least 15/1 for routine instrument performance.
7.7.1.1 Preparation of Silica SPE Cartridge—Follow the
Subsections 9.2 – 9.4 describe the preparation of the various
manufacturer’s instruction for preparation and use.The typical
solutions required.
method of preparation is to wet the cartridge with approxi-
3 9.2 Preparation of PAH Standard Solutions for
mately 10 cm of the elution solvent. Discard the wetting
Calibration—Using the native PAH standard stock solution
solvent.
described in 7.2, prepare at least 10 cm of five toluene
7.7.2 Alternative SPE Method: Silica Gel/13 % H O Grav-
solutions at the concentrations suggested in the following list.
ity Column:
Other concentrations may be used but the difference between
7.7.2.1 Preparation of a Silica Gel/13 % H O Adsorbent—
any two concentration levels shall not exceed a factor of four.
Pour 200 g silica gel (high purity grade, type 60, particle size
Before diluting to the final solution volume, spike each
0.063 to 0.200 mm) into a screw cap glass bottle and add 30 g
3 standard with the appropriate volume (for example, 100 µLIS
ofdeionizedwaterinsmallportions(forexample,2cm )using
solution described in 9.3 into 10 cm volumetric flask to give
a suitable pipette. After addition of each portion of water, the
a final IS concentration of 0.500 µg/cm ). Other aliquot
silica gel bottle is shaken to evenly distribute the wetted silica
volumes and final volumes may be used to obtain the desired
gel. No aggregation should occur during this process. If so,
concentrations. Cap the standard solutions securely, mix thor-
shaking must be continued until a homogeneous material is
oughly and label. Store all standard solutions in the dark.
obtained. Finally, the closed bottle is shaken for8hby means
Native PAH Standard 5 1.00 µg/cm
of an overhead shaker. If properly closed and stored, the
Native PAH Standard 4 0.500 µg/cm
adsorbent should be viable for at least 6 months. 3
Native PAH Standard 3 0.200 µg/cm
7.7.2.2 Preparation of a Silica Gel/13 % H O Gravity
Native PAH Standard 2 0.0500 µg/cm
Native PAH Standard 1 0.0125 µg/cm
Column—Insert a glass wool plug into the bottom of a pipette
tip (for example, 8 to 10 mm inner diameter and 5 cm 9.3 Preparation of Diluted IS Solution—Using the IS stock
capacity). Place1gofthe silica gel/13 % H O in the column
solution described in 7.2, prepare at least 10 cm of diluted
and tap the column gently to settle the silica gel. Cover the internalstandardsolutionforaddingtosamplesandcalibration
adsorbent layer with a glass wool plug and pre-elute the standards. A concentration of 50 µg/cm is suggested for this
column with 5 cm of cyclohexane. Discard the cyclohexane solution but other concentrations can be used. For example,
3 3
eluate. when adding 100 µL of a 50 µg/cm IS solution to a 10 cm
finalextractvolume,theISconcentrationwillbe0.500µg/cm .
8. Hazards
9.4 All standard solutions shall be stored in a refrigerator
8.1 This test involves hazardous materials, operations, and
(<6°C) when not in use. Care has to be taken not to exceed
equipment. This procedure does not attempt to address the
their shelf life. If any indication of degradation is perceived,
safety problems associated with this test. A hazards review
then new standards have to be prepared.
shallbeconductedbyallpersonnelperformingthetest.Itisthe
10. Carbon Black Sample Preparation and Extraction
responsibility of the user to review all material safety data
sheets(MSDS),manuals,andhazardsproceduresandestablish
10.1 All glassware coming into contact with the sample
the appropriate safety measures. Some PAH
...