ASTM D8311-20

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: D8311 − 20
Standard Test Method for
Impurities in Monoethylene Glycol by Gas Chromatography
with Normalization
This standard is issued under the fixed designation D8311; 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 2. Referenced Documents
1.1 This test method covers the gas chromatographic deter- 2.1 ASTM Standards:
mination of impurities in monoethylene glycol including 1,3- D6809 Guide for Quality Control and Quality Assurance
dioxolane-2-methanol, diethylene glycol (DEG) and triethyl- Procedures for Aromatic Hydrocarbons and Related Ma-
ene glycol (TEG). The purity of monoethylene glycol (MEG) terials
is also calculated. A similar test method, using the internal E29 Practice for Using Significant Digits in Test Data to
standard calibration technique and the external standard cali- Determine Conformance with Specifications
bration technique, is Test Method E2409. E300 Practice for Sampling Industrial Chemicals
E355 Practice for Gas Chromatography Terms and Relation-
1.2 This test method is applicable for monoethylene glycol
ships
purities of 98.0 mass % or higher.
E691 Practice for Conducting an Interlaboratory Study to
1.3 The limit of detection (LOD) for 1,3-dioxolane-2-
Determine the Precision of a Test Method
methanol, DEG and TEG is 0.0002 mass %.
E1064 Test Method for Water in Organic Liquids by Coulo-
metric Karl Fischer Titration
1.4 In determining the conformance of the test results using
this method to applicable specifications, results shall be E1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
rounded off in accordance with the rounding-off method of
Practice E29. E2409 TestMethodforGlycolImpuritiesinMono-,Di-,Tri-
and Tetraethylene Glycol and in Mono- and Dipropylene
1.5 The values stated in SI units are to be regarded as
Glycol(Gas Chromatographic Method)
standard. No other units of measurement are included in this
2.2 Other Document:
standard.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
1.6 This standard does not purport to address all of the 3
1910.1200
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3. Summary of Test Method
priate safety, health, and environmental practices and deter-
3.1 The specimen to be analyzed is injected into a gas
mine the applicability of regulatory limitations prior to use.
chromatographequippedwithaflameionizationdetector(FID)
1.7 This international standard was developed in accor-
and a capillary column.
dance with internationally recognized principles on standard-
3.2 The peak area of each component is measured and
ization established in the Decision on Principles for the
adjustedusingrelativecalibrationfactors.Theconcentrationof
Development of International Standards, Guides and Recom-
each component is calculated based on its relative percentages
mendations issued by the World Trade Organization Technical
of total adjusted peak area and normalized to 100.0000 %.
Barriers to Trade (TBT) Committee.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D16 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- Standards volume information, refer to the standard’s Document Summary page on
bility of Subcommittee D16.14 on Alcohols & Glycols. the ASTM website.
Current edition approved April 1, 2020. Published May 2020. DOI: 10.1520/ Available from Occupational Safety and Health Administration (OSHA), 200
D8311-20. Constitution Ave., NW, Washington, DC 20210, http://www.osha.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8311 − 20
4. Significance and Use 6. Reagents and Materials
4.1 Thistestmethodissuitableforsettingspecificationsand 6.1 Purity of Reagent—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
for use as an internal quality control tool where these products
are produced or are used. Typical impurities are: 1,3- all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
dioxolane-2-methanol, diethylene glycol, and triethylene gly-
col. where such specifications are available. Reagents with an
establish purity greater than ACS reagent grade may be used.
4.2 This method may not detect all components and there
6.2 Calibration Standards:
may be unknown components that would be assigned inappro-
6.2.1 Mono-ethylene Glycol (MEG), minimum GC purity
priate relative calibration factors and thus, the results may not
99.95 mass %. As a blank MEG sample, the concentrations of
be absolute.
each component of interest should not be higher than 0.005
mass %.
5. Apparatus
6.2.2 Di-ethylene Glycol (DEG), minimum purity 99.5
5.1 Gas Chromatograph—Any instrument having a flame
mass %.
ionization detector and a splitter injector suitable for use with
6.2.3 Tri-ethylene Glycol (TEG), minimum purity 99.5
a fused silica capillary column may be used, provided the
mass %.
system has sufficient sensitivity, linearity, and range to deter-
6.2.4 1,3-Dioxolane-2-methanol, minimum purity 95 mass
mine 0.0001 mass %, while not exceeding the full scale of
%.
either the detector or the electronic integration for the major
6.3 Carrier gas (helium, nitrogen, or hydrogen), makeup gas
component. It shall have a split injection system that will not
and detector gases 99.999 % (v/v) pure or better. Oxygen in
discriminate over the boiling range of the samples analyzed.
carrier gas less than 1 ppm, less than 0.5 ppm is preferred.
The system should be capable of operating at conditions given
Purify carrier, makeup and detector gases to remove oxygen,
in Table 1.
water, and hydrocarbons.
5.2 Columns—The choice of column is based on resolution
6.4 Air for the FID should contain less than 0.1 ppm total
requirements. Any column may be used that is capable of
hydrocarbon.
resolving all significant impurities from the major component.
The column and conditions described in Table 1 have been
7. Hazards
used successfully and shall be used as a referee in cases of
7.1 Consult current OSHA regulations and supplier’s Safety
dispute.
Data Sheets and local regulations for all materials used in this
5.3 Injector—The specimen must be precisely and repeat-
test method.
edly injected into the gas chromatograph. An autoinjector is
7.2 Monoethylene Glycol—Although monoethylene glycol,
required.
in general, is not classified as dangerous or flammable and is
5.4 Syringe—Chromatographic, capable of delivering ap-
not expected to impose a health hazard when used under
propriate µL volumes.
normal conditions, it is recommended to avoid inhalation and
contact with skin and eyes. Wear suitable protective clothing
5.5 Electronic Integrator chromatography data system is
required. and gloves. Do not breathe gas, fumes, vapor, or spray. Use
only in well-ventilated areas. In cases of contact with eyes,
rinse with plenty of water and seek medical advice.
8. Sampling
TABLE 1 Recommended Method Parameters
8.1 Followtherelevantinstructionsforsamplingasgivenin
Inlet Split
Temperature, °C 300
Practice E300.
Column
Material fused silica
9. Preparation of Apparatus
Stationary Phase 6 % Cyanopropyl-phenyl - 94 % dimethyl
polysiloxane
9.1 Follow manufacturer’s instructions for mounting and
Length, m 30
conditioning the column into the chromatograph and adjusting
Internal diameter, mm 0.32
Fi
...