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ASTM D6142-03

(Test Method)

Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography

Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography

SIGNIFICANCE AND USE
This test method is suitable for setting specifications on phenol and for use as an internal quality control tool where phenol is produced or is used in a manufacturing process. It may also be used in development or research work involving phenol. It is generally applied to determining those commonly occurring impurities such as mesityl oxide, cumene, hydroxyacetone, acetone, alpha-methylstyrene, 2-methylbenzofuran, acetophenone, o-cresol, and m & p-cresol.
Purity is commonly reported by subtracting the determined expected impurities from 100.00. However, a gas chromatographic analysis cannot determine absolute purity if unknown components are contained within the material being examined.
SCOPE
1.1 This test method covers the determination of known impurities in phenol by gas chromatography (GC). It is generally meant for the analysis of phenol of 99.9% or greater purity.  
1.2 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or calculated value 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. Precision data is based on impurity concentrations of 15 to 70 mg/kg. Users of this test method believe it is linear over a wider range.  
1.3 This Test Method 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. For specific hazard statements, see Section 9.

General Information

Status
Historical
Publication Date
09-Feb-2003
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
D16 - Aromatic, Industrial, Specialty and Related Chemicals
Drafting Committee
D16.02 - Oxygenated Aromatics
Current Stage
Ref Project

Relations

Replaces
ASTM D6142-97 - Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography
Effective Date
10-Feb-2003
Replaced By
ASTM D6142-08 - Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography
Effective Date
01-Dec-2008

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ASTM D6142-03 - Standard Test Method for Analysis of Phenol by Capillary Gas ChromatographyASTM D6142-03 - Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography
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ASTM D6142-03 - Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography
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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: D 6142 – 03
Standard Test Method for
1
Analysis of Phenol by Capillary Gas Chromatography
This standard is issued under the fixed designation D 6142; 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* E 1510 Practice for Installing Fused Silica Open Tubular
4
Capillary Columns in Gas Chromatographs
1.1 This test method covers the determination of known
2.2 Other Document:
impurities in phenol by gas chromatography (GC). It is
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
generally meant for the analysis of phenol of 99.9 % or greater
5
1910.1200
purity.
1.2 The following applies to all specified limits in this test
3. Terminology
method: for purposes of determining conformance with this
3.1 See Terminology D 4790 for definition of terms used in
test method, an observed value or calculated value shall be
this method.
rounded off “to the nearest unit” in the last right-hand digit
used in expressing the specification limit in accordance with
4. Summary of Test Method
the rounding-off method of Practice E29. Precision data is
4.1 A known amount of an internal standard is added to a
based on impurity concentrations of 15 to 70 mg/kg. Users of
sample of phenol. The prepared sample is mixed and analyzed
this test method believe it is linear over a wider range.
by a gas chromatograph equipped with a flame ionization
1.3 This standard does not purport to address all of the
detector (FID).The peak area of each impurity and the internal
safety concerns, if any, associated with its use. It is the
standard is measured. The amount of each impurity is calcu-
responsibility of the user of this standard to establish appro-
lated from the ratio of the peak area of the internal standard
priate safety and health practices and determine the applica-
versus the peak area of the impurity. Results are reported in
bility of regulatory limitations prior to use. For specific hazard
milligrams per kilogram.
statements, see Section 9.
5. Significance and Use
2. Referenced Documents
5.1 This test method is suitable for setting specifications on
2.1 ASTM Standards:
phenol and for use as an internal quality control tool where
D 3852 Practice for Sampling and Handling Phenol,
phenol is produced or is used in a manufacturing process. It
2
Cresols, and Cresylic Acid
may also be used in development or research work involving
D 4790 Terminology of Aromatic Hydrocarbons and Re-
phenol. It is generally applied to determining those commonly
2
lated Chemicals
occurring impurities such as mesityl oxide, cumene, hydroxy-
E29 Practice for Using Significant Digits in Test Data to
acetone, acetone, alpha-methylstyrene, 2-methylbenzofuran,
3
Determine Conformance with Specifications
acetophenone, o-cresol, and m & p-cresol.
E 355 Practice for Gas Chromatography Terms and Rela-
5.2 Purity is commonly reported by subtracting the deter-
4
tionships
mined expected impurities from 100.00. However, a gas
E 691 Practice for Conducting an Interlaboratory Study to
chromatographic analysis cannot determine absolute purity if
3
Determine the Precision of a Test Method
unknown components are contained within the material being
examined.
1
6. Interferences
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
6.1 The internal standard chosen must be sufficiently re-
Subcommittee D16.02 on Oxygenated Aromatics.
solved from any impurity and the phenol peak.
Current edition approved Feb. 10, 2003. Published April 2003. Originally
approved in 1997. Last previous edition approved in 1997 as D 6142 - 97.
2
Annual Book of ASTM Standards, Vol 06.04.
3 5
Annual Book of ASTM Standards, Vol 14.02. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
4
Annual Book of ASTM Standards, Vol 03.06. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
*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.
1

---------------------- Page: 1 ----------------------
D6142–03
TABLE 1 Instrument Conditions for Phenol Analysis
Column: To use for identification of all but cresols To use for identification of all components
Tubing fused silica fused silica
Stationary phase polyethylene glycol-acid modified (5 % Phenyl)-methylpolysiloxane
Solid support crosslinked bonded and crosslinked
Film thickness, µ 0.5 1.0
Length, m 50 60
Inside diameter, m 0.32 0.32
Flow rate mL/min 1.3 1.3
Temperature, °C
Injector 180 200
Detector 230 22
...

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4.1 Knowledge of the UV transmittance of MEG is required to establish whether the product meets the requirements of its quality specifications.  
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1.1 This test method covers a procedure for the determination of the transmittance of monoethylene glycol (1,2-ethanediol; MEG) at wavelengths in the region 220 nm to 350 nm. The results provide a measure of the purity of the sample with respect to ultraviolet (UV) absorbing compounds.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D6144-22(Test Method)
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5.1 This test method is suitable for setting specifications on the materials referenced in 1.2 and for use as an internal quality control tool where AMS is produced or is used in a manufacturing process. It may also be used in development or research work involving AMS.  
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1.1 This test method covers the determination of the purity of AMS (α-methylstyrene) by gas chromatography. Calibration of the gas chromatography system is done by the external standard calibration technique.  
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Standard Test Method for Analysis of Phenol by Capillary Gas Chromatography

SIGNIFICANCE AND USE
5.1 This test method is suitable for setting specifications on phenol and for use as an internal quality control tool where phenol is produced or is used in a manufacturing process. It may also be used in development or research work involving phenol. It is generally applied to determining those commonly occurring impurities such as mesityl oxide, cumene, hydroxyacetone, acetone, α-methylstyrene, 2-methylbenzofuran, and acetophenone.  
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1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.  
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4.1 This test method is suitable for setting specifications and for use as an internal quality control tool where these products are produced or are used. Typical impurities are: 1,3-dioxolane-2-methanol, diethylene glycol, and triethylene glycol.  
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1.1 This test method covers the gas chromatographic determination of impurities in monoethylene glycol including 1,3-dioxolane-2-methanol, diethylene glycol (DEG) and triethylene glycol (TEG). The purity of monoethylene glycol (MEG) is also calculated. A similar test method, using the internal standard calibration technique and the external standard calibration technique, is Test Method E2409.  
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4.1 pH is, within the limits described in 1.1, an accurate measurement of the hydrogen ion concentration and thus is widely used for the characterization of aqueous solutions.  
4.2 pH measurement is one of the main process control variables in the chemical industry and has a prominent place in pollution control.
SCOPE
1.1 This test method specifies the apparatus and procedures for the electrometric measurement of pH values of aqueous solutions with the glass electrode. It does not deal with the manner in which the solutions are prepared. pH measurements of good precision can be made in aqueous solutions containing high concentrations of electrolytes or water-soluble organic compounds, or both. It should be understood, however, that pH measurements in such solutions are only a semiquantitative indication of hydrogen ion concentration or activity. The measured pH will yield an accurate result for these quantities only when the composition of the medium matches approximately that of the standard reference solutions. In general, this test method will not give an accurate measure of hydrogen ion activity unless the pH lies between 2 and 12 and the concentration of neither electrolytes nor nonelectrolytes exceeds 0.1 mol/L (M).  
1.2 The values stated in SI units are to be regarded as standard. The values in parentheses are for information only.  
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ASTM D5917-15(2019)(Test Method)
Standard Test Method for Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and External Calibration

SIGNIFICANCE AND USE
5.1 Determining the type and amount of hydrocarbon impurities remaining from the manufacture of toluene, mixed xylenes, and p-xylenes used as chemical intermediates and solvents is often required. This test method is suitable for setting specifications and for use as an internal quality control tool where these products are produced or are used. Typical impurities are: alkanes containing 1 to 10 carbons atoms, benzene, toluene, ethylbenzene (EB), xylenes, and aromatic hydrocarbons containing nine carbon atoms.  
5.2 Purity is commonly reported by subtracting the determined expected impurities from 100.00. However, a gas chromatographic analysis cannot determine absolute purity if unknown or undetected components are contained within the material being examined.  
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1.1 This test method covers the determination of the total nonaromatic hydrocarbons and trace monocyclic aromatic hydrocarbons in toluene, mixed xylenes, and p-xylene by gas chromatography. The purity of toluene, mixed xylenes, or p-xylene can also be calculated. Calibration of the gas chromatographic system is done by the external standard calibration technique. A similar test method, using the internal standard calibration technique, is Test Method D2360.  
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1.2.1 A small amount of benzene in mixed xylenes or p-xylenes may not be distinguished from the nonaromatics and the concentrations are determined as a composite (see 6.1).  
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1.4 In determining the conformance of the test results to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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. For specific hazard statement, see Section 9.  
1.7 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.

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