ASTM D7515-19(2023)
(Test Method)Standard Test Method for Purity of 1,3-Propanediol (Gas Chromatographic Method)
Standard Test Method for Purity of 1,3-Propanediol (Gas Chromatographic Method)
SIGNIFICANCE AND USE
4.1 Knowledge of an approved method is required to establish whether the product meets the requirements of its specifications. The use of glycols in the reference sample is not intended to suggest the presence of glycol (EG, PG and DPG) impurities, but to demonstrate and quantify the separation of commonly used Engine Coolant glycols from PDO.
SCOPE
1.1 This test method describes the gas chromatographic determination of purity for 1,3-propanediol (PDO). This test method was originally developed to determine the purity of 1,3-propanediol used for the application as the freeze point depressant base fluid in formulated PDO engine coolants. Use of the method for purity of PDO for other applications may be viable.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exception—Inch-pound units (psi) are used in Table 1, Pressure Program, Options A and B.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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.
General Information
Relations
Standards Content (Sample)
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: D7515 − 19 (Reapproved 2023)
Standard Test Method for
Purity of 1,3-Propanediol (Gas Chromatographic Method)
This standard is issued under the fixed designation D7515; 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 D1123 Test Methods for Water in Engine Coolant Concen-
trate by the Karl Fischer Reagent Method
1.1 This test method describes the gas chromatographic
E177 Practice for Use of the Terms Precision and Bias in
determination of purity for 1,3-propanediol (PDO). This test
ASTM Test Methods
method was originally developed to determine the purity of
E300 Practice for Sampling Industrial Chemicals
1,3-propanediol used for the application as the freeze point
E691 Practice for Conducting an Interlaboratory Study to
depressant base fluid in formulated PDO engine coolants. Use
Determine the Precision of a Test Method
of the method for purity of PDO for other applications may be
E2409 Test Method for Glycol Impurities in Mono-, Di-, Tri-
viable.
and Tetraethylene Glycol and in Mono- and Dipropylene
1.2 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
standard.
3. Summary of Test Method
1.2.1 Exception—Inch-pound units (psi) are used in Table 1,
3.1 The sample is analyzed by a temperature-programmed
Pressure Program, Options A and B.
gas chromatograph, equipped with a capillary column and
1.3 Review the current Material Safety Data Sheets (MSDS)
flame ionization detector (FID), and quantification is per-
for detailed information concerning toxicity, first aid
formed by direct area normalization.
procedures, and safety precautions.
3.2 Additionally, the use of a reference sample using
1.4 This standard does not purport to address all of the
Ethylene, Propylene, or Dipropylene Glycol (EG, PG or DPG)
safety concerns, if any, associated with its use. It is the
in 1,3-PDO (minimum purity 99.5 %) should be used as a
responsibility of the user of this standard to establish appro-
performance check (see Section 8).
priate safety, health, and environmental practices and deter-
NOTE 1—The application of this reference sample is also used to
mine the applicability of regulatory limitations prior to use.
demonstrate the separation of commonly used glycols (EG, PG and DPG)
1.5 This international standard was developed in accor- in engine coolants, from PDO. Solutions of EG, PG, or DPG in
concentrations of 0.1 to not more than 1 % may be used.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Significance and Use
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4.1 Knowledge of an approved method is required to
Barriers to Trade (TBT) Committee.
establish whether the product meets the requirements of its
specifications. The use of glycols in the reference sample is not
2. Referenced Documents
intended to suggest the presence of glycol (EG, PG and DPG)
2.1 ASTM Standards: impurities, but to demonstrate and quantify the separation of
commonly used Engine Coolant glycols from PDO.
This test method is under the jurisdiction of ASTM Committee D15 on Engine
5. Apparatus
Coolants and Related Fluids and is the direct responsibility of Subcommittee
D15.04 on Chemical Properties.
5.1 Gas Chromatograph(s)—provided with a sample splitter
Current edition approved Sept. 1, 2023. Published September 2023. Originally
or on-column injection, flame ionization detector and
approved in 2009. Last previous edition approved in 2019 as D7515 – 19. DOI:
10.1520/D7515–19R23.
temperature-programming facilities. The instrument must be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
suitable for analysis according to the operating instructions
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
given in Table 1. To account for differences among laboratory
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. equipment, the two most common column choices are listed.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7515 − 19 (2023)
TABLE 1 Typical Operating Parameters for the GC Analysis of PDO
A B
Column Option A Option B Option C
Type Capillary Capillary Capillary
Material Fused Silica PEG PEG
Length × I.D. 10 m × 0.1 mm 30 m × 0.25 mm 30 m × 0.32 mm
Stationary Phase DB-5 ZB-Wax ZB-Wax
Film Thickness 0.17 μm 0.25 μm 1 μm
Detector System
Type FID FID FID
Sensitivity The ratio of the signal to the The ratio of the signal to the noise The ratio of the signal to the noise level
noise level must be at least 2:1 at level must be at least 2:1 at a must be at least 2:1 at a concentration of
a concentration of 5 mg/kg concentration of 5 mg/kg glycols in 5 mg/kg glycols in PDO
glycols in PDO PDO
Temperatures
Column Oven
Initial 0.5 min at 35 °C 0 min at 50 °C 0 min at 100 °C retention time 0.5 min
Ramp 1 35 °C to 85 °C at 50 °C ⁄min 50 °C to 200 °C at 15 °C ⁄min 100 °C to 180 °C at 15 °C ⁄min; 5.83 min
Ramp 2 85 °C to 325 °C at 100 °C ⁄min 200 °C to 250 °C at 40 °C ⁄min 180 °C to 225 °C at 30 °C ⁄min; 0 min
Ramp 3 2 min at 325 °C 17 min at 250 °C Hold 3.7 min at 225 °C
Detector 325 °C 250 °C 250 °C
Carrier Gas Helium Helium Helium or Nitrogen
Calibration This method employs straight This method employs straight area Calibration
area normalization so no normalization so no calibration is
calibration is required required
Injected Volume 01. μL 0.2 μL 1.0 μL
Pressure Program 0.5 min at 30 psi Pressure: 13.2 psi at 50 °C Constant flow at 5 mL/min
30 psi to 100 psi at 100 psi/min Flow: 1.1 mL/min
8 min at 100 psi Velocity: 28 cm/s
Gas saver on at 0.5 min
Split Ratio 1:250 or appropriate split ratio to 1:18 or appropriate split ratio to Inlet temperature 235 °C
allow adequate sensitivity as allow adequate sensitivity as defined Split flow 300 mL/min
defined under Detector System under Detector System (only if split Split ratio 60
injection technique is used)
A
The columns are available commercially. Some column suppliers market alternative stationary phases. The chromatogram obtained must be identical, with regard to
separation of PDO and other glycol components, to those illustrated in Fig. A1.1 and Fig. A1.2.
B
Option C instrument method is for reference only; due to instrument operational variations, temperature ramp, gas flow, and split flow/ratio may need adjustment to
achieve separation of analyzed glycols.
NOTE 2—Other column suppliers market alternative stationary phases,
cal Society where such specifications are available. Other
therefore, it is permissible to use a different column from an alternative
grades may be used, provided it is first ascertained that the
supplier. However, the chromatogram obtained must be identical, with
reagent is of sufficiently high purity to permit its use without
regard to separation of PDO and other glycol components, to those
lessening the accuracy of the determination.
illustrated in Fig. A1.1 and Fig. A1.2.
6.2 Reagents:
5.1.1 Columns—The analytical column used must com-
6.2.1 1,3-Propanediol (PDO), minimum purity 99.5 % mass
pletely separate EG, PG or DPG from PDO. Fig. A1.1 and Fig.
(m/m).
A1.2 show examples of chormatograms conforming to the
6.2.2 Ethylene Glycol (EG), minimum purity 99.5 % mass
requirements.
(m/m).
5.2 Digital Integration Equipment—A computer with data
6.2.3 Propylene Glycol (PG), minimum purity 99.5 % mass
collection software.
(m/m).
6.2.4 Dipropylene Glycol (DPG), minimum purity 99.0 %
5.3 Analytical Balance, readability 0.1 mg, calibrated. Cali-
mass (m/m).
brate and verify at regular intervals.
6.3 Water or Methanol, HPLC grade.
5.4 Crimp Top Vials, 1 mL and 5 mL.
6.4 Internal Reference Sample.
5.5 Crimper/De-capper, for capping and de-capping the
vials. 7. Sampling, Test Specimens and Test Units
7.1 Follow the relevant instructions for sampling as given in
5.6 Micro Syringes, 5 μL or 10 μL.
Practice E300.
5.7 Bottles, 100 mL, with screw cap.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
6. Reagents and Materials
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
6.1 Purity of Reagents—Unless otherwise indicated, it is
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
intended that all reagents shall conform to the specifications of
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the Committee on Analytical Reagents of the American Chemi- copeial Convention, Inc. (USPC), Rockville, MD.
D7515 − 19 (2023)
8. Preparation of Apparatus 8.3 Sample Preparation:
8.3.1 Weigh 0.1 g 1,3 PDO sample to the nearest 0.1 mg in
8.1 Met
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