ASTM D5310-00

Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography

SCOPE
1.1 This test method covers the quantitative determination of phenol and certain homologues of phenol in tar acid and cresylic acid mixtures using capillary gas chromatography. It is a normalization test method that determines homolog distribution but is not an absolute assay since it does not account for water or other compounds not detected by a flame ionization detector.
1.2 The following applies to all specified limits in this standard: for purposes of determining conformance with this standard, an observed value or a 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 E29.
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. For specific hazard statements, see Section 7.

General Information

• Status: Historical
• Publication Date: 09-Jan-2000
• ICS: 71.080.40 - Organic acids
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.02 - Oxygenated Aromatics

Relations

• Replaced By: ASTM D5310-00(2004) - Standard Test Method for Tar Acid Composition by Capillary Gas Chromatography
• Effective Date: 01-Jun-2004

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5310 – 00
Standard Test Method for
Tar Acid Composition by Capillary Gas Chromatography
This standard is issued under the fixed designation D 5310; 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 3. Terminology
1.1 This test method covers the quantitative determination 3.1 For definition of terms used in this test method see
of phenol and certain homologues of phenol in tar acid and Terminology D 4790.
cresylic acid mixtures using capillary gas chromatography. It is
4. Summary of Test Method
a normalization test method that determines homolog distribu-
tion but is not an absolute assay since it does not account for 4.1 The sample composition is determined by capillary gas
chromatography. The weight percent composition is calculated
water or other compounds not detected by a flame ionization
detector. from the ratio of the individual peak areas to the total area of
all peaks using appropriate response factors determined for
1.2 The following applies to all specified limits in this
standard: for purposes of determining conformance with this each component by means of a calibration sample.
standard, an observed value or a calculated value shall be
5. Significance and Use
rounded off “to the nearest unit” in the last right-hand digit
5.1 This test method is suitable for the general quantitative
used in expressing the specification limit, in accordance with
analysis of commercial tar acid mixtures. It may be used as a
the rounding-off method of Practice E 29.
tool for quality control and specification purposes by producers
1.3 This standard does not purport to address all of the
and users.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Chromatograph—A gas chromatograph compatible
bility of regulatory limitations prior to use. For specific hazard
with capillary columns, equipped with inlet splitter and high
statements, see Section 8.
temperature flame ionization detector. Typical Operating Con-
2. Referenced Documents
ditions are given in Table 1.
6.2 Peak Integrator—Electronic integration is recom-
2.1 ASTM Standards:
mended.
D 3852 Practice for Sampling and Handling Phenol and
6.3 Recorder, with full scale response time of1sor less.
Cresylic Acid
6.4 Microsyringe, capacity of 1 μL.
D 4790 Terminology of Aromatic Hydrocarbons and Re-
6.5 Capillary Column—Any column capable of resolving
lated Chemicals
all components of interest. Prepared columns are commercially
E 29 Practice for Using Significant Digits in Test Data to
available from chromatography supply houses. Chromato-
Determine Conformance with Specifications
grams from three columns are presented in Fig. 1, Fig. 2, and
2.2 Other Documents:
Fig. 3. Peak identification is given in Table 2.
OSHA Regulations, 29 CFR, paragraphs 1910.1000, and
1910.1200
7. Reagents and Materials
7.1 Calibration Standards—Samples of known composition
This test method is under the jurisdiction of ASTM Committee D16 on
representative of samples to be analyzed.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.02 on Oxygenated Aromatics.
8. Hazards
Current edition approved Jan. 10, 2000. Published March 2000. Originally
e1
published as D 5310 – 94. Last previous edition D 5310 – 94 . 8.1 Consult current OSHA regulations and suppliers’ mate-
Annual Book of ASTM Standards, Vol 06.04.
rial safety data sheets, and local regulations for all materials
Annual Book of ASTM Standards, Vol 14.02.
used in this test method.
Available from Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5310
TABLE 1 Typical Chromatographic Operating Conditions
Cyanopropyl 25 %, Phenyl 25 %, Dimethyl 95 %, Diphenylpolysiloxane
Column Liquid Phase Diisodecyl Phthalate
Methylpolysiloxane 50 %, Bonded Phase 5 %, Bonded Phase
Column Fused Silica Fused Silica Fused Silica
Column length, m 30 25 30
Column ID, mm 0.25 0.22 0.25
Film thickness,μ m 0.2 0.2 0.25
Column temperature,° C 100 100 105
Detector temperature,° C 200–275 200–275 200–275
Injection block temperature, °C 200–275 200–275 200–275
Carrier gas H or He H or He H or He
2 2 2
Carrier flow, linear velocity, cm/s 40–80 40–80 40–80
Hydrogen flow to flame, mL/min 30–40 (optimize) 30–40 (optimize) 30–40 (optimize)
Air flow to flame ;10·H flow (optimize) ;10·H flow (optimize) ;10·H flow (optimize)
2 2 2
A
Make up gas N or He N or He N or He
2 2 2
Sample size, μL 0.05–0.1 0.05–0.1 0.05–0.1
Split ratio 100:1 to 250:1 100:1 to 250:1 100:1 to 250:1
A
Inert gas added to hydrogen fuel gas as coolant to prevent overheating and thermal emissions for optimal detector operations; each instrument should be optimized
according to manufacturer’s recommendations.
FIG. 1 Typical Chromatogram of Cresylic Acid on Column of
Diisodecyl Phthalate on Fused Silica
FIG. 3 Typical Chromatogram of Cresylic Acid on Column of 95 %
Dimethyl, 5 % Diphenyl Polysiloxane Bonded on Fused Silica
(DB-5)
preparation is of known purity. Even when purchased as
reagent grade, it is prudent to verify impuritie
...