ASTM D6563-00
(Test Method)Test Method for Benzene, Toluene, Xylene, (BTX) Concentrates Analysis by Capillary Column Gas Chromatography
Test Method for Benzene, Toluene, Xylene, (BTX) Concentrates Analysis by Capillary Column Gas Chromatography
SCOPE
1.1 This test method covers the determination of the total nonaromatic hydrocarbons, benzene, toluene, ethylbenzene, xylenes, and C9 + aromatic hydrocarbons in BTX concentrates by capillary column gas chromatography. This test method is applicable ot materials with a final boiling point below 215oC.
Individual components can be determined fro 0.01 to 90%.
1.3 The following applies to all specified limits in this standard; for purpose of determining conformance with this standard, an observed value or a calculated value shall be rounded off "to the nearest unit" in the right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.4 This standard does not purport to address all of the safety concerns, if any, asociated 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. For a specific precautionary statement, see Section 9.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D6563–00
Test Method for
Benzene, Toluene, Xylene, (BTX) Concentrates Analysis by
Capillary Column Gas Chromatography
This standard is issued under the fixed designation D 6563; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
1.1 This test method covers the determination of the total
2.2 Other Documents:
nonaromatic hydrocarbons, benzene, toluene, ethylbenzene,
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
xylenes, and C + aromatic hydrocarbons in BTX concentrates
1910.1200
by capillary column gas chromatography. This test method is
applicable to materials with a final boiling point below 215°C.
3. Terminology
1.2 Individual components can be determined from 0.01 to
3.1 Definitions of Terms Specific to This Standard:
90 %.
3.1.1 extracted reformate—An aromatic concentrate ob-
1.3 The following applies to all specified limits in this
tained by solvent extraction of reformate.
standard: for purpose of determining conformance with this
3.1.2 reformate—The product of a catalytic process that
standard, an observed value or a calculated value shall be
increases the concentration of aromatic hydrocarbons.
rounded off “to the nearest unit” in the right-hand digit used in
3.1.3 pyrolysis gasoline—Depentanized by-product recov-
expressing the specification limit, in accordance with the
ered from ethylene manufacture.
rounding-off method of PracticeE29.
3.1.4 synthetic blend—Blend of reagent hydrocarbons that
1.4 This standard does not purport to address all of the
simulate a process product.
safety concerns, if any, associated with its use. It is the
3.1.5 hydrogenated pyrolysis gasoline—Pyrolysis gasoline
responsibility of the user of this standard to establish appro-
that has been treated with hydrogen to reduce the olefins
priate safety and health practices and determine the applica-
content.
bility of regulatory limitations prior to use. For a specific
3.1.6 crude ethylbenzene—Product produced from the reac-
precautionary statement, see Section 9.
tion of impure fluid cat cracking, (FCC) ethylene and benzene.
2. Referenced Documents 3.1.6.1 Discussion—It typically contains greater than 40 %
of ethylbenzene and benzene.
2.1 ASTM Standards:
3.1.7 light blending aromatics feedstock—Light aromatics
D 3437 Practice for sampling and Handling Liquid Cyclic
fraction (with high amounts of benzene and toluene) typically
Products
recovered from the isomerization of a p-xylene or m-xylene
E29 Practice for Using Significant Digits in Test Data to
depleted C aromatics stream.
Determine Conformance with Specifications
E 355 Practice for Gas Chromatography Terms and Rela-
4. Summary of Test Method
tionships
4.1 The specimen to be analyzed is injected into a gas
E 691 Practice for Conducting an Interlaboratory Study to
3 chromatographequippedwithaflameionizationdetector(FID)
Determine the Precision of a Test Method
and a capillary column. The peak area of each component is
measured and adjusted using effective carbon number (ECN)
This test method is under the jurisdiction of ASTM Committee D16 on response factors. The concentration of each component is
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
calculated based on its relative percentages of total adjusted
Subcommittee D16.01 on Benzene, Toluene, Xylenes, Cyclohexane, and Their
Derivatives.
Current edition approved June 10, 2000. Published August 2000.
2 4
Annual Book of ASTM Standards, Vol 06.04. Available from the Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D6563–00
TABLE 1 Instrument Parameters
peak area and normalized to 100.00. Results can be reported as
either volume or weight percent. Column Size of 60 m by 0.25 mm ID µm-
bonded polyethylene glycol-fused silica
4.2 Volumetric results can be derived by dividing each
capillary, internally coated to a 0.25-µm
component’s weight percent by its relative density and re- thickness
Carrier gas helium
normalizing to 100 %.
Flow, linear velocity at 70°C, cm/s 20
Split ratio 200:1
5. Significance and Use Detector gas
Hydrogen flow rate, mL/min 30
5.1 This test method was primarily developed to determine Air flow rate, mL/min 300
Make-up flow rate, mL/min 30
benzene, toluene, and xylenes in chemical intermediate and
Sample size, µL 0.5
solvent streams such as reformate, BTX extracts, pyrolysis
Temperatures
Injector, °C 250
gasoline, hydrogenated pyrolysis gasoline, crude benzene,
Detector, °C 300
crude ethylbenzene, commercial toluene, and light blending
Column
aromatic feedstocks. This test method may not detect all
Initial, °C 70
Hold, min 10
components and there may be unknown components that
Rate, °C/min 5
would be assigned inappropriate response factors and thus, the
Final, °C 200
results may not be absolute.
Hold, min 24
6. Interferences
9. Hazards
6.1 Nonaromatic hydrocarbons may interfere with the de-
9.1 Consult current OSHA regulations, supplier’s Material
termination of benzene and toluene when certain columns are
Safety Data Sheets, and local regulations for all material used
used.
in this test method.
6.2 Styrene may be present in some samples. It will elute
10. Sampling
with C + aromatics.
10.1 Sample material in accordance with Practice D 3437.
7. Apparatus
11. Preparation of Apparatus
7.1 Gas Chromatograph—Any gas chromatograph having a
11.1 Chromatograph—Follow manufacturer’s instructions
flame ionization detector and a splitter injector suitable for use
for mounting and conditioning the column in the chromato-
with a fused silica capillary column may be used, provided the
graph and adjusting the instrument to the conditions as
system has sufficient sensitivity to obtain a minimum peak
described in Table 1 to give the desired separation. Allow
height response of 0.1 mV for 0.01 % of any component of
sufficient time for the instrument to reach equilibrium as
interest in the sample being analyzed or in the system blend
indicatedbyastablerecorder/electronicbaseline.SeePractices
when operated at the stated conditions. Background noise
E 355 and E 1510 for additional information on gas chroma-
should not exceed 0.01 mV. Largest component of interest
tography practices and terminology.
should not exceed 90 % full scale of the electronic integration
12. Procedure
device.
12.1 Bring the sample to ambient room temperature.
7.2 Column—Capillary columns have found to be satisfac-
tory. For example, a 60 m by 0.25 mm inside diameter fused 12.2 Inject an appropriate amount of sample into the chro-
matograph that meets the criteria outlined in 7.1. See Practices
silica capillary, internally coated to a 0.25-µm thickness with a
E 355 and E 1510 for additional information on gas chroma-
bonded (cross-linked) polyethylene glycol can be used (see
tography practices and terminology.
Table1forparameters).Othercolumnsmaybeusedafterithas
12.3 Sample chromatograms are illustrated in Figs. 1-3.
been established that such a column is capable of separating all
12.4 Measure the area of all peaks. The nonaromatics
majorimpuritiesunderoperatingconditionsappropriateforthe
fraction includes all peaks up to ethylbenzene (except for the
column.
peaks assigned to benzene and toluene). Sum together all the
7.3 Recorder/Electronic Integration—Electronicintegration
nonaromatic peaks as a total area. The C + aromatics fraction
with tangent capabilities is recommended.
includes cumene and all peaks eluting after o-xylene. Sum
together all the C + aromatic peaks as a total a
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