ASTM D4367-02(2007)
(Test Method)Standard Test Method for Benzene in Hydrocarbon Solvents by Gas Chromatography
Standard Test Method for Benzene in Hydrocarbon Solvents by Gas Chromatography
SIGNIFICANCE AND USE
Benzene is classed as a toxic and carcinogenic material. A knowledge of the concentration of this compound may be an aid in evaluating the possible health hazards to persons handling and using hydrocarbon solvents, but this test method is not intended to evaluate such hazards.
SCOPE
1.1 This test method covers the determination by gas chromatography of benzene at levels from 0.01 to 1 volume % in hydrocarbon solvents.Note 1
For benzene levels lower than 0.01 volume %, use Test Method D 6229.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 For purposes of determining conformance of an observed or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
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.
1.4 For hazard information and guidance, see the supplier's Material Safety Data Sheet. For specific hazard statements, see Section 7.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4367 − 02 (Reapproved 2007)
StandardTest Method for
Benzene in Hydrocarbon Solvents by Gas Chromatography
This standard is issued under the fixed designation D4367; 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* 3. Summary of Test Method
3.1 An internal standard, methyl ethyl ketone (MEK), is
1.1 This test method covers the determination by gas
added to the material and then introduced into a gas chromato-
chromatography of benzene at levels from 0.01 to 1 volume %
graph equipped with two columns connected in series. The
in hydrocarbon solvents.
specimen passes first through a column packed with the
NOTE 1—For benzene levels lower than 0.01 volume %, use Test
nonpolar phase, methyl silicone, which separates the compo-
Method D6229.
nents by boiling point. After octane has eluted, the flow
1.2 The values stated in SI units are to be regarded as the through the nonpolar column is reversed, flushing out the
standard. The values given in parentheses are for information
components heavier than octane. The octane and lighter
only. components then pass through a column with the highly polar
phase, 1,2,3-tris(2-cyanoethoxy)propane, that separates the
1.3 For purposes of determining conformance of an ob-
aromatic and nonaromatic compounds. The eluted components
served or a calculated value using this test method to relevant
are detected by a conventional detector and recorded on a strip
specifications, test result(s) shall be rounded off “to the nearest
chart. The peak areas are measured and the concentration of
unit” in the last right-hand digit used in expressing the
each component is calculated by reference to the internal
specification limit, in accordance with the rounding-off method
standard.
of Practice E29.
4. Significance and Use
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 Benzene is classed as a toxic and carcinogenic material.
responsibility of the user of this standard to establish appro-
Aknowledge of the concentration of this compound may be an
priate safety and health practices and determine the applica-
aid in evaluating the possible health hazards to persons
bility of regulatory limitations prior to use.
handling and using hydrocarbon solvents, but this test method
1.5 For hazard information and guidance, see the supplier’s
is not intended to evaluate such hazards.
Material Safety Data Sheet. For specific hazard statements, see
5. Apparatus
Section 7.
5.1 Chromatograph—Any gas chromatographic instrument
2. Referenced Documents
that has a backflush system and flame ionization detector and
that can be operated at the conditions given in Table 1. The
2.1 ASTM Standards:
detector-recordercombinationmustproducea4-mmdeflection
D6229 Test Method for Trace Benzene in Hydrocarbon
for a 1-µL specimen containing 0.05 volume % MEK when
Solvents by Capillary Gas Chromatography
operated at maximum sensitivity.
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications 5.2 Columns, one 0.8-m (2.5-ft) length of 3.2-mm ( ⁄8-in.)
E300 Practice for Sampling Industrial Chemicals outside diameter stainless steel tubing and one 4.6-m (15-ft)
length of 3.2-mm ( ⁄8-in.) outsider diameter stainless steel
tubing.
This test method is under the jurisdiction of ASTM Committee D01 on Paint 5.3 Recorder, Strip Chart—Potentiometer with a full-scale
and Related Coatings, Materials, andApplications and is the direct responsibility of
deflection of 1 mV, a full-scale response time of2sor less, and
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
a maximum noise level of 60.3 % of full scale.
Current edition approved June 1, 2007. Published June 2007. Originally
approved in 1984. Last previous edition approved in 2002 as D4367 – 02. DOI:
5.4 Microsyringe, 5-µL capacity.
10.1520/D4367-02R07.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.5 Pipets, measuring 1 and 2 mL, graduated in 0.01 mL; 5,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
10, and 20-mL capacity.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.6 Flasks, volumetric, 25 and 100-mL capacity.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4367 − 02 (Reapproved 2007)
TABLE 1 Instrument Conditions Found Satisfactory for
6.6 Methanol.
Measuring Low Concentrations of Benzene in
6.7 Methylene Chloride.
Hydrocarbon Solvents (Note 2)
Detector flame ionization
6.8 Methyl Ethyl Ketone (MEK), 99.9 mol %.
Columns two, stainless steel
Length, m (A) 0.8; (B) 4.6
6.9 Methyl Silicone.
Outside diameter, mm 3.2
Stationary phases (A) methyl silicone, 10 weight %
6.10 1,2,3-Tris(2-Cyanoethoxy) Propane (TCEP).
(B) TCEP, 25 weight %
Support (A) acid-washed calcined diatomite, 60 to 6.11 Calibration Standards.
+
80-mesh
6.11.1 Benzene, 99 mol %.
(B) acid-washed pink diatomaceous
+
6.11.2 Isooctane, 99 mol %.
earth, 80 to 100-mesh
+
Reference column any column or restriction may be used
6.11.3 n-Nonane, 99 mol %.
Temperature, °C
Injection port 150
Column, isothermal 100
7. Hazards
Detector block 150
Carrier gas helium 7.1 Many hydrocarbon solvents are flammable and hazard-
Flow rate, mL/min approximately 30
ous; use special precautions when handling them. Of the
Recorder range, mV 0 to 1
reagents used in this procedure, methanol, chloroform, meth-
Chart speed, mm/min 10
Specimen size, µL 1.0 ylenechloride,acetone,methylethylketone,benzene(see4.1),
Time to backflush, min approximately 2
and n-nonane are hazardous.
Total cycle time, min approximately 30
7.2 Benzene is volatile and highly flammable. Exercise care
to prevent accidental ignition. Benzene is also carcinogenic
and toxic; acute or chronic poisoning may result from inhala-
5.7 Vibrator, electric.
tion of benzene vapor, absorption of benzene through the skin,
5.8 Vacuum Source.
or drinking benzene.
5.9 Evaporator, vacuum, rotary.
8. Sampling
5.10 Flask, boiling, round-bottom, short-neck, with 24/40 T
joint, 500-mL capacity. Suitable for use with the evaporator
8.1 Take samples of solvents to be analyzed by this test
(see 5.9).
method using the procedures described in Practice E300.
5.11 Lamp, infrared.
9. Preparation of Columns
5.12 Burets, automatic, with integral reservoir, 25-mL ca-
pacity. 9.1 Column Packing Preparation—Prepare the two packing
materials, one containing 10 % methyl silicone and the other
NOTE 2—Suppliers of stationary phases and supports can be found in
25 % TCEP, as follows:
Research Report RR:D01-1038, available from ASTM International
Headquarters. 9.1.1 Weigh 45 g of the acid-washed calcined diatomite
support60to80mesh,intoa500-mLflask(see5.10).Dissolve
6. Reagents and Materials
5 g of the methyl silicone in approximately 50 mL of
6.1 Purity of Reagents—Reagent grade chemicals shall be chloroform. (Warning—Chloroform is a toxic material and
inhalation must be avoided.) Pour the methyl silicone–chloro-
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit- form solution into the flask containing the support. Attach the
flask to the evaporator (see 5.9), connect the vacuum, and start
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be the motor. Turn on the infrared lamp and allow the packing to
used, provided it is first ascertained that the reagent is of mix thoroughly until dry.
sufficiently high purity to permit its use without lessening the
9.1.2 Weigh 75 g of acid-washed pink diatomaceous earth,
accuracy of the determination.
80 to 100 mesh, into a 500-mL flask (see 5.10). Dissolve 25 g
of TCEP in 200 mL of methanol and pour into the flask
6.2 Acetone.
containing the support. Attach the flask to the evaporator (see
6.3 Chloroform.
5.9), connect the vacuum, and start the motor. Turn on the
6.4 Diatomaceous Earth —Acid-washed, 60 to 80 mesh infrared lamp and allow the packing to mix thoroughly until
and 80 to 100 mesh.
dry, but do not heat the packing above 180°C.
6.5 Helium, 99.99 % pure.
9.2 Column Preparation:
9.2.1 Clean the stainless steel tubing as follows: Attach a
3 metal funnel to one end of the steel tubing. Hold or mount the
Reagent Chemicals, American Chemical Society Specifications, American
stainless steel tubing in an upright position and place a beaker
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
under the outlet end of the tubing. Pour about 50 mL of
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
methylenechlorideintothefunnelandallowittodrainthrough
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
thesteeltubingintothebeaker.Repeatthewashingwith50mL
MD.
See Note 2. of acetone. Remove the funnel and connect the steel tubing to
D4367 − 02 (Reapproved 2007)
an air line, by means of vinyl tubing. Remove all solvent from 10.2 Connect the outlet of Column B to the detector port.
the steel tubing by blowing filtered, oil-free air through or Adjust the operating conditions to those listed in Table 1, but
applying a vacuum. do not turn on the detector circuits. Check the system for leaks.
9.2.2 Pack the 0.8-m (2.5-ft) tubing (Column A) with the
10.3 Adjust the flow rate as follows:
methylsiliconepacking(see9.1.1)andthe4.6-m(15-ft)tubing
10.3.1 Set the value in the forward flow mode (Fig. 2(a))
(Column B) with the TCEP packing (see 9.1.2) as follows:
and adjust Flow Controller A to give the required flow rate
Preform Columns A and B separately to fit the chromato-
(Table 1). Measure the flow rate at the detector vent, specimen
graphic instrument. Close one end of each tubing with a small,
side.
gla
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