ASTM D7515-09(2014)
(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.
1.3 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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7515 − 09 (Reapproved 2014)
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 3.2 Additionally, the use of a reference sample using
Ethylene, Propylene or Dipropylene Glycol (EG, PG or DPG)
1.1 This test method describes the gas chromatographic
in 1,3-PDO (minimum purity 99.5 %) should be used as a
determination of purity for 1,3-propanediol (PDO). This test
performance check (see Section 8).
method was originally developed to determine the purity of
NOTE 1—The application of this reference sample is also used to
1,3-propanediol used for the application as the freeze point
demonstrate the separation of commonly used glycols (EG, PG and DPG)
depressant base fluid in formulated PDO engine coolants. Use
in engine coolants, from PDO. Solutions of EG, PG, or DPG in
of the method for purity of PDO for other applications may be concentrations of 0.1 to not more than 1 % may be used.
viable.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 4.1 Knowledge of an approved method is required to
standard. establish whether the product meets the requirements of its
specifications.The use of glycols in the reference sample is not
1.3 ReviewthecurrentMaterialSafetyDataSheets(MSDS)
intended to suggest the presence of glycol (EG, PG and DPG)
for detailed information concerning toxicity, first aid
impurities, but to demonstrate and quantify the separation of
procedures, and safety precautions.
commonly used Engine Coolant glycols from PDO.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Gas Chromatograph(s)—providedwithasamplesplitter
priate safety and health practices and determine the applica-
or on-column injection, flame ionization detector and
bility of regulatory limitations prior to use.
temperature-programming facilities. The instrument must be
2. Referenced Documents suitable for analysis according to the operating instructions
given in Table 1. To account for differences among laboratory
2.1 ASTM Standards:
equipment, the two most common column choices are listed.
E177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
NOTE 2—Other column suppliers market alternative stationary phases,
therefore, it is permissible to use a different column from an alternative
E300 Practice for Sampling Industrial Chemicals
supplier. However, the chromatogram obtained must be identical, with
E691 Practice for Conducting an Interlaboratory Study to
regard to separation of PDO and other glycol components, to those
Determine the Precision of a Test Method
illustrated in Fig. A1.1 and Fig. A1.2.
5.1.1 Columns—The analytical column used must com-
3. Summary of Test Method
pletely separate EG, PG or DPG from PDO. Fig.A1.1 and Fig.
3.1 The neat sample is analyzed by a temperature-
A1.2 show examples of chormatograms conforming to the
programmed gas chromatograph, equipped with a capillary
requirements.
column and flame ionization detector (FID), and quantification
5.2 Digital Integration Equipment—A computer with data
is performed by direct area normalization.
collection software.
5.3 Analytical Balance, readability 0.1 mg, calibrated. Cali-
This test method is under the jurisdiction ofASTM Committee D15 on Engine
brate and verify at regular intervals.
Coolants and Related Fluids and is the direct responsibility of Subcommittee
D15.07 on Specifications.
5.4 Crimp Top Vials, 1 mL and 5 mL.
Current edition approved Feb. 1, 2014. Published March 2014. Originally
approved in 2009. Last previous edition approved in 2009 as D7515-09. DOI:
5.5 Crimper/De-capper, for capping and de-capping the
10.1520/D7515-09R14.
vials.
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
5.6 Micro Syringes,5µLor10µL.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.7 Bottles, 100 mL, with screw cap.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7515 − 09 (2014)
TABLE 1 Typical Operating Parameters for the GC Analysis of
PDO
A
Column Option A Option B
Type Capillary Capillary
Material Fused Silica PEG
Length × I.D. 10m×0.1 mm 30m×0.25mm
Stationary Phase DB-5 ZB-Wax
Film Thickness 0.17 µm 0.25 µm
Detector System
Type FID FID
Sensitivity The ratio of the signal to the The ratio of the signal to the noise
noise level must be at least 2:1 atlevel must be at last 2:1 at a
a concentration of 5 mg/kg concentration of 5 mg/kg glycols in
glycols in PDO PDO
Temperatures
Column Oven
Initial 0.5 min at 35°C 0 min at 50°C
Ramp 1 35 to 85°C at 50°C/min 50 to 200°C at 15°C/min
Ramp 2 85 to 325°C at 100°C/min 200 to 250°C at 40°C/min
Ramp 3 2 min at 325°C 17 min at 250°C
Detector 325°C 250°C
Carrier Gas Helium Helium
Calibration This method employs straight This method employs straight area
area normalization so no normalization so no calibration is
calibration is required required
Injected Volume 01. µL 0.2 µL
Pressure Program 0.5 min 30 psi Pressure: 13.2 psi at 50°C
30 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 allow
allow adequate sensitivity as adequate sensitivity as defined under
defined under Detector System Detector System (only if split
injection technique is used)
A
The columns are available commercially. Some column suppliers market alter-
native 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.
6. Reagents and Materials 7. Sampling, Test Specimens and Test Units
6.1 Purity of Reagents—Unless otherwise indicated, it is 7.1 Followtherelevantinstructionsforsamplingasgivenin
intended that all reagents shall conform to the specifications of Practice E300.
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
8. Preparation of Apparatus
cal Society where such specifications are available. Other
8.1 Gas Chromatograph(s) and Column(s)—Check the per-
grades may be used, provided it is first ascertained that the
formance of the gas chromatograph and column as follows:
reagent is of sufficiently high purity to permit its use without
lessening the accuracy of the determi
...
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