ASTM D4773-02(2007)
(Test Method)Standard Test Method for Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene Glycol Monomethyl Ether Acetate
Standard Test Method for Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene Glycol Monomethyl Ether Acetate
SIGNIFICANCE AND USE
This test method is used to determine the purity of PM, DPM, and PMA by subtracting calculated total impurities from 100 %.
This test method is used to determine the quantity of residual glycol ether present in PMA.
This test method is used for identifying various impurities in PM, DPM, and PMA.
SCOPE
1.1 This test method covers the determination by gas chromatography of propylene glycol monomethyl ether (PM), dipropylene glycol monomethyl ether (DPM), and propylene glycol monomethyl ether acetate (PMA). Propylene glycol monomethyl ether (PM) is a mixture of two isomers: 1-methoxy-2-propanol and 2-methoxy-1-propanol. Dipropylene glycol monomethyl ether (DPM) is a mixture of four isomers: 1-(2-methoxy-1-methylethoxy)-2-propanol is one of the major isomers. Propylene glycol monomethyl ether acetate (PMA) is a mixture of two isomers: 1-methoxy-2-acetoxypropane and 2-methoxy-1-acetoxypropane.
1.1.1 This test method covers the determination of PM in the range from 98 to 100 %, and DPM in the range from 0.08 to 0.6 %.
1.1.2 This test method covers the determination of DPM in the range from 98 to 100 %, PM in the range from 0.05 to 0.3 %, and tripropylene glycol monomethyl ether (TPM) in the range from 0.06 to 0.3 %.
1.1.3 This test method covers the determination of PMA in the range from 99 to 100 %, and PM in the range from 0.03 to 1.0 %.
1.2 Water and acid cannot be determined by this test method and must be measured in accordance with Test Methods D 1364 and D 1613, and the results used to normalize the chromatographic data.
1.3 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 E 29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
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.
General Information
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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: D4773 − 02 (Reapproved 2007)
StandardTest Method for
Purity of Propylene Glycol Monomethyl Ether, Dipropylene
Glycol Monomethyl Ether, and Propylene Glycol
Monomethyl Ether Acetate
This standard is issued under the fixed designation D4773; 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* 1.5 For hazard information and guidance, see the supplier’s
Material Safety Data Sheet.
1.1 This test method covers the determination by gas
chromatography of propylene glycol monomethyl ether (PM), 1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
dipropylene glycol monomethyl ether (DPM), and propylene
glycol monomethyl ether acetate (PMA). responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
NOTE 1—Propylene glycol monomethyl ether (PM) is a mixture of two
bility of regulatory limitations prior to use.
isomers: 1-methoxy-2-propanol and 2-methoxy-1-propanol.
Dipropylene glycol monomethyl ether (DPM) is a mixture of four
isomers: 1-(2-methoxy-1-methylethoxy)-2-propanol is one of the major
2. Referenced Documents
isomers.
2.1 ASTM Standards:
Propylene glycol monomethyl ether acetate (PMA) is a mixture of two
isomers: 1-methoxy-2-acetoxypropane and 2-methoxy-1-acetoxypropane. D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
1.1.1 This test method covers the determination of PM in
D1613 Test Method for Acidity in Volatile Solvents and
the range from 98 to 100 %, and DPM in the range from 0.08
Chemical Intermediates Used in Paint, Varnish, Lacquer,
to 0.6 %.
and Related Products
1.1.2 This test method covers the determination of DPM in
E29 Practice for Using Significant Digits in Test Data to
the range from 98 to 100 %, PM in the range from 0.05 to
Determine Conformance with Specifications
0.3 %, and tripropylene glycol monomethyl ether (TPM) in the
range from 0.06 to 0.3 %.
3. Summary of Test Method
1.1.3 This test method covers the determination of PMA in
the range from 99 to 100 %, and PM in the range from 0.03 to
3.1 Arepresentative sample of PM, DPM, or PMAcontain-
1.0 %.
ing the appropriate internal standard is injected into a capillary
gas chromatograph and the components are detected with a
1.2 Waterandacidcannotbedeterminedbythistestmethod
flame ionization detector. Quantification is made by peak area
andmustbemeasuredinaccordancewithTestMethodsD1364
measurement using internal standardization and a computing
and D1613, and the results used to normalize the chromato-
integrator.
graphic data.
1.3 The following applies to all specified limits in this
4. Significance and Use
standard; for purposes of determining conformance with this
4.1 This test method is used to determine the purity of PM,
standard, an observed value or a calculated value shall be
DPM, and PMAby subtracting calculated total impurities from
rounded off “to the nearest unit” in the last right-hand digit
100 %.
used in expressing the specification limit, in accordance with
the rounding-off method of Practice E29.
4.2 This test method is used to determine the quantity of
1.4 The values stated in SI units are to be regarded as residual glycol ether present in PMA.
standard. No other units of measurement are included in this
4.3 This test method is used for identifying various impu-
standard.
rities in PM, DPM, and PMA.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2007. Published June 2007. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1988. Last previous edition approved in 2002 as D4773 – 02. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4773-02R07. the ASTM website.
*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
D4773 − 02 (Reapproved 2007)
5. Apparatus (see 6.3.4) and 0.02 g of DPM. Check these reagents for purity
under the conditions used in the procedures and, if interfering
5.1 Chromatograph—Any programmed temperature gas
compounds are present, adjustment must be made in preparing
chromatograph designed or modified for use with capillary
the standard.
columns. The chromatograph must also be equipped with a
7.1.2 Dipropylene Glycol Monomethyl Ether (DPM)—
flame ionization detector.
Weigh into a vial to within 0.1 mg, 10.00 g of DPM calibration
5.2 Column—Capillary, 5 µm thick film, 10 m by 0.32 mm
standard (see 6.3.3), 0.02 g of PM calibration standard (see
inside diameter, fused silica coated, with 5 % phenyl methyl
6.3.4), and 0.02 g ofTPM (see 6.3.6). Check these reagents for
silicon liquid phase.
purity under the conditions used in the procedure and, if
5.3 Syringe—10 µL or equivalent to introduce a representa-
interferingcompoundsarepresent,adjustmentmustbemadein
tive sample onto the column.
preparing the standard.
7.1.3 Propylene Glycol Monomethyl Ether Acetate (PMA)—
5.4 Computing Integator, capable of peak summation and a
Weigh into a vial to within 0.1 mg, 10.00 g of PMAcalibration
baseline construction.
standard(see6.3.5)and0.04gofPM.Checkthesereagentsfor
5.5 Analytical Balance, capable of measuring 0.1 mg.
purity under the conditions used in the procedure and, if
interferingcompoundsarepresent,adjustmentmustbemadein
6. Reagents and Materials
preparing the standard.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 7.2 Preparation of Standard:
all reagents shall conform to the specifications of the Commit-
7.2.1 Weighintoavialtowithin0.1mg,1.0gofthedesired
tee onAnalytical Reagents of theAmerican Chemical Society,
calibration standard solution (see 7.1.1 for PM, 7.1.2 for DPM
where such specifications are available. Other grades may be
and 7.1.3 for PMA).
used, provided it is first ascertained that the reagent is of
7.2.2 Into the respective vials for PM and DPM, weigh to
sufficiently high purity to permit its use without lessening the
within 0.1 mg, 1.0 g of monochlorobenzene internal standard
accuracy of the determination.
(see 6.3.2), tightly seal with a polyethylene-lined cap, and mix
thoroughly.
6.2 Gases:
6.2.1 Carrier Gas—Helium, with a minimum purity of
7.2.3 Into the vial containing PMA, weigh to within 0.1 mg,
99.95 mol % for use with a flame ionization detector. 1.0gof n-butyl acetate internal standard (see 6.3.1), tightly
6.2.2 Detector Gas—Hydrogen with a minimum purity and
seal with a polyethylene lined cap, and mix thoroughly.
air for use with the flame ionization detector.
7.3 Chromatographic Conditions:
6.3 Standards for Calibration and Identification:
Column: capillary fused silica
6.3.1 N-Butyl Acetate—Distilled-in-glass purity for use as
Length, m 10
an internal standard in determination of PMA.
Inside diameter, mm 0.32
Film thickness, µm 5
6.3.2 Monochlorobenzene—Distilled-in-glass purity for use
Injection temperature, °C 300
as an internal standard in determination of PM and DPM.
Detector temperature, °C 300
6.3.3 Dipropylene Glycol Monomethyl Ether (DPM)— Split: 30:1
Specimen size,µ L 0.5 needle flash
Purity should be determined and the standard solution adjusted
Oven temperature, °C at 8°C/min 80–260
for this purity.
Column flow, mL/min (He) 1.2
6.3.4 Propylene Glycol Monomethyl Ether (PM)—Purity
Makeup flow, mL/min (He) 24
Internal standard:
should be determined and the standard solution adjusted for
PM DPM PMA
this purity.
Monochlorobenzene monochlorobenzene n-butyl acetate
6.3.5 Propylene Glycol Monomethyl Ether Acetate (PMA)—
7.4 Calibration for Propylene Glycol Monomethyl Ether
Purity should be determined and the standard solution adjusted
(PM):
for this purity.
6.3.6 Tripropylene Glycol Monomethyl Ether (TPM)—
7.4.1 Make a needle-flash injection of the standard into the
Purity should be determined and the standard solution adjusted
chromatograph and separate according to the chromatographic
for this purity. conditions in 7.3. At the end of the run, set the peak summing
windows to sum the isomer peaks as shown in Areas I and II
7. Calibration and Standardization
of Fig. 1.
7.1 Preparation of Calibration Standard Solution:
7.4.2 Program the integrator to set the baseline at the same
7.1.1 Propylene Glycol Monomethyl Ether (PM)—Weigh
time peak summation begins for the PM isomers. Force the
into a vial to within 0.1 mg, 10.00 g of PM calibration standard
integrator to extend a baseline horizontally from the set
baseline.
7.4.3 Make another needle-flash injection of the standard
“Reagent Chemicals, American Chemical Society Specifications,” American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
and calibrate the integrator according to the manufacturer’s
listed by the American Chemical Society, see “Analar Standards for Laboratory
operating instruction for an internal standard method. Re-
...
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