ASTM E2409-13
(Test Method)Standard Test Method for Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol and in Mono- and Dipropylene Glycol(Gas Chromatographic Method)
Standard Test Method for Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol and in Mono- and Dipropylene Glycol<brk/>(Gas Chromatographic Method)
SIGNIFICANCE AND USE
4.1 Knowledge of the impurities is required to establish whether the product meets the requirements of its specifications.
SCOPE
1.1 This test method describes the gas chromatographic determination of glycol impurities in Mono-, Di- Tri- and Tetraethylene Glycol (MEG, DEG, TEG and TeEG) in the range of 5 to 3000 mg/kg, and in Mono- and Dipropylene Glycol (MPG and DPG) in the range 0.01 to 2.5 % (m/m).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Review the current Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.
1.4 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.
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Designation: E2409 − 13
Standard Test Method for
Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol
and in Mono- and Dipropylene Glycol
1
(Gas Chromatographic Method)
This standard is issued under the fixed designation E2409; 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
1.1 This test method describes the gas chromatographic 3.1 Aportion of the test sample is analyzed by temperature-
determination of glycol impurities in Mono-, Di- Tri- and programmed, capillary gas chromatography over a polyethyl-
Tetraethylene Glycol (MEG, DEG, TEG and TeEG) in the ene glycol column, using flame ionization detection. For
range of 5 to 3000 mg/kg, and in Mono- and Dipropylene quantification, the External Standard Technique or the Internal
Glycol (MPG and DPG) in the range 0.01 to 2.5 % (m/m). Standard (Marker) Technique are applied. When applying the
Internal StandardTechnique, the standard addition technique is
1.2 The values stated in SI units are to be regarded as
used to eliminate the effect of other impurities present in the
standard. No other units of measurement are included in this
glycols. For this purpose, a blank glycol is used, as 100 % pure
standard.
glycol samples are not available.
1.3 ReviewthecurrentMaterialSafetyDataSheets(MSDS)
for detailed information concerning toxicity, first aid 4. Significance and Use
procedures, and safety precautions.
4.1 Knowledge of the impurities is required to establish
1.4 This standard does not purport to address all of the
whether the product meets the requirements of its specifica-
safety concerns, if any, associated with its use. It is the
tions.
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5.1 Gas Chromatograph(s), provided with a sample splitter
or on-column injection, flame ionization detector and
2. Referenced Documents
temperature-programming facilities. Optional are pressure pro-
2
2.1 ASTM Standards:
gramming and auto sampler facilities. The instrument must be
E180 Practice for Determining the Precision of ASTM
suitable for analysis according to the operating instructions
Methods for Analysis and Testing of Industrial and Spe-
given in Table 1 or Table 2.
3
cialty Chemicals (Withdrawn 2009)
5.1.1 Columns—The analytical column (chemically bonded
E300 Practice for Sampling Industrial Chemicals
cross-linked polyethylene glycol) used must completely sepa-
E1064 Test Method for Water in Organic Liquids by Coulo-
rate
metric Karl Fischer Titration
MEG, DEG, TEG, TeEG, PentaEG (Penta-ethylene Gly-
2.2 Other Document: col) and 1,4-butanediol, or
Manufacturers’ instruction manuals of gas chromatograph MPG, DPG, TPG, and TePG
and digital integration system used. Figs. A1.1 through A1.5 show examples of chromatograms
conforming to the requirements.
1
5.2 Digital Integration Equipment.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
5.3 Analytical Balance, readability 0.1 mg, calibrated. Re-
bility of Subcommittee D16.14 on Alcohols & Glycols.
calibrate or verify at regular intervals.
Current edition approved June 1, 2013. Published August 2013. Originally
approved in 2004. Last previous edition approved in 2008 as E2409 – 08. DOI:
5.4 Crimp Top Vials, 1 mL and 5 mL.
10.1520/E2409-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.5 Crimper/De-capper, for capping and de-capping the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
vials.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
5.6 Micro Syringes, 10 µL.
3
The last approved version of this historical standard is referenced on
www.astm.org. 5.7 Bottles, 50 mL, with screw cap.
*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 ----------------------
E2409 − 13
TABLE 1 Typical Operating Parameters for the GC Analysis of
6. Reagents and Materials
Glycol Impurities in MEG, DEG, TEG or TeEG
6.1 Purity of Reagents—Unless otherwise indicated, it is
A
Column
intended that all reagents shall conform to the specifications of
Type Capillary wide-bore
Material Fused silica
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
4
Length × I.D. 15m×0.53mm
cal Society where such spec
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E2409 − 08 E2409 − 13
Standard Test Method for
Glycol Impurities in Mono-, Di-, Tri- and Tetraethylene Glycol
and in Mono- and Dipropylene Glycol
1
(Gas Chromatographic Method)
This standard is issued under the fixed designation E2409; 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*
1.1 This test method describes the gas chromatographic determination of glycol impurities in Mono-, Di- Tri- and Tetraethylene
Glycol (MEG, DEG, TEG and TeEG) in the range of 5 to 3000 mg/kg.mg/kg, and in Mono- and Dipropylene Glycol (MPG and
DPG) in the range 0.01 to 2.5 % (m/m).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Review the current Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures,
and safety precautions.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E300 Practice for Sampling Industrial Chemicals
E1064 Test Method for Water in Organic Liquids by Coulometric Karl Fischer Titration
2.2 Other Document:
Manufacturers’ instruction manuals of gas chromatograph and digital integration system used.
3. Summary of Test Method
3.1 A portion of the test sample is analyzed by temperature-programmed, capillary gas chromatography over a DB-wax
polyethylene glycol column, using flame ionization detection. For quantification, the External Standard Technique or the Internal
Standard (Marker) Technique, using 1,4-butanediol as marker, Technique are applied. When applying the Internal Standard
Technique, the standard addition technique is used to eliminate the effect of other impurities present in the glycols. For this
purpose, a blank glycol is used, as 100 % pure glycol samples are not available.
4. Significance and Use
4.1 Knowledge of the impurities is required to establish whether the product meets the requirements of its specifications.
5. Apparatus
5.1 Gas Chromatograph(s), provided with a sample splitter or on-column injection, flame ionization detector and temperature-
programming facilities. Optional are pressure programming and autosampler auto sampler facilities. The instrument must be
suitable for analysis according to the operating instructions given in Table 1 or Table 2.
1
This test method is under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and is the direct responsibility of Subcommittee E15.02 on
Product Standards.
Current edition approved April 1, 2008June 1, 2013. Published May 2008August 2013. Originally approved in 2004. Last previous edition approved in 20042008 as
E2409 – 04.E2409 – 08. DOI: 10.1520/E2409-08.10.1520/E2409-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
*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 ----------------------
E2409 − 13
TABLE 1 Typical Operating Parameters for the GC Analysis of
Glycol Impurities in MEG, DEG, TEG or TeEG
A
Column
Type Capillary wide-bore
Material Fused silica
Length × I.D. 15 m × 0.53 mm
Stationary Phase Polyethylene glycol, for example, DB-
Wax
Film Thickness 1 μm
Detector System
Type FID
Sensitivity The ratio of the signal to the noise level
must be at least
2:1 at a concentration of 5 mg/kg
DEG in MEG
Temperatures
Column Oven 0.05 min at 70°C
Programmed from 70 to 230°C at 25°C/
min
10 min at 230°C
Detector 250°C
Carrier Gas Helium or Nitrogen
Calibration see Section 9
Injected Volume 0.2 μL (on-column injection), or
0.5 μL
...
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