ASTM D4773-93(1998)

Standard Test Method for Purity of Propylene Glycol Monomethyl Ether, Dipropylene Glycol Monomethyl Ether, and Propylene Glycol Monomethyl Ether Acetate

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).
Note 1—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 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
1.5 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

• Status: Historical
• Publication Date: 09-May-2002
• ICS: 71.080.60 - Alcohols. Ethers
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

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NOTICE: This standard has either been superseded and replaced by a new version or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 – 93 (Reapproved 1998)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Fischer Reagent Titration Method)
D 1613 Test Method for Acidity in Volatile Solvents and
1.1 This test method covers the determination by gas
Chemical Intermediates Used in Paint, Varnish, Lacquer,
chromatography of propylene glycol monomethyl ether (PM),
and Related Products
dipropylene glycol monomethyl ether (DPM), and propylene
glycol monomethyl ether acetate (PMA).
3. Summary of Test Method
NOTE 1—Propylene glycol monomethyl ether (PM) is a mixture of two
3.1 A representative sample of PM, DPM, or PMA contain-
isomers: 1-methoxy-2-propanol and 2-methoxy-1-propanol.
ing the appropriate internal standard is injected into a capillary
Dipropylene glycol monomethyl ether (DPM) is a mixture of four
gas chromatograph and the components are detected with a
isomers: 1-(2-methoxy-1-methylethoxy)-2-propanol is one of the major
flame ionization detector. Quantification is made by peak area
isomers.
measurement using internal standardization and a computing
Propylene glycol monomethyl ether acetate (PMA) is a mixture of two
isomers: 1-methoxy-2-acetoxypropane and 2-methoxy-1-acetoxypropane.
integrator.
1.1.1 This test method covers the determination of PM in
4. Significance and Use
the range from 98 to 100 %, and DPM in the range from 0.08
4.1 This test method is used to determine the purity of PM,
to 0.6 %.
DPM, and PMA by subtracting calculated total impurities from
1.1.2 This test method covers the determination of DPM in
100 %.
the range from 98 to 100 %, PM in the range from 0.05 to
4.2 This test method is used to determine the quantity of
0.3 %, and tripropylene glycol monomethyl ether (TPM) in the
residual glycol ether present in PMA.
range from 0.06 to 0.3 %.
4.3 This test method is used for identifying various impu-
1.1.3 This test method covers the determination of PMA in
rities in PM, DPM, and PMA.
the range from 99 to 100 %, and PM in the range from 0.03 to
1.0 %.
5. Apparatus
1.2 Water and acid cannot be determined by this test method
5.1 Chromatograph—Any programmed temperature gas
and must be measured in accordance with Test Methods
chromatograph designed or modified for use with capillary
D 1364 and D 1613, and the results used to normalize the
columns. The chromatograph must also be equipped with a
chromatographic data.
flame ionization detector.
1.3 This standard does not purport to address all of the
5.2 Column—Capillary, 5 μm thick film, 10 m by 0.32 mm
safety concerns, if any, associated with its use. It is the
inside diameter, fused silica coated, with 5 % phenyl methyl
responsibility of the user of this standard to establish appro-
silicon liquid phase.
priate safety and health practices and determine the applica-
5.3 Syringe—10 μL or equivalent to introduce a represen-
bility of regulatory limitations prior to use.
tative sample onto the column.
1.4 For hazard information and guidance, see the supplier’s
5.4 Computing Integator, capable of peak summation and a
Material Safety Data Sheet.
baseline construction.
2. Referenced Documents 5.5 Analytical Balance, capable of measuring 0.1 mg.
2.1 ASTM Standards:
6. Reagents and Materials
D 1364 Test Method for Water in Volatile Solvents (Karl
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
all reagents shall conform to the specifications of the Commit-
and Related Coatings, Materials, and Applications and is the direct responsibility of
tee on Analytical Reagents of the American Chemical Society,
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved May 15, 1993. Published July 1993. Originally
published as D 4773 – 88. Last previous edition D 4773 – 89.
Annual Book of ASTM Standards, Vol 06.04.
D4773
where such specifications are available. Other grades may be (see 6.3.2), tightly seal with a polyethylene-lined cap, and mix
used, provided it is first ascertained that the reagent is of thoroughly.
sufficiently high purity to permit its use without lessening the 7.2.3 Into the vial containing PMA, weigh to within 0.1 mg,
accuracy of the determination. 1.0gof n-butyl acetate internal standard (see 6.3.1), tightly
6.2 Gases: seal with a polyethylene lined cap, and mix thoroughly.
6.2.1 Carrier Gas—Helium, with a minimum purity of 7.3 Chromatographic Conditions:
99.95 mol % for use with a flame ionization detector. Column: capillary fused silica
6.2.2 Detector Gas—Hydrogen with a minimum purity and
Length, m 10
Inside diameter, mm 0.32
air for use with the flame ionization detector.
Film thickness, μm 5
6.3 Standards for Calibration and Identification:
Injection temperature, °C 300
6.3.1 N-Butyl Acetate—Distilled-in-glass purity for use as
Detector temperature, °C 300
Split: 30:1
an internal standard in determination of PMA.
Specimen size,μ L 0.5 needle flash
6.3.2 Monochlorobenzene—Distilled-in-glass purity for use
Oven temperature, °C at 8°C/min 80–260
as an internal standard in determination of PM and DPM. Column flow, mL/min (He) 1.2
Makeup flow, mL/min (He) 24
6.3.3 Dipropylene Glycol Monomethyl Ether (DPM)—
Internal standard:
Purity should be determined and the standard solution adjusted
PM DPM PMA
for this purity.
Monochlorobenzene monochlorobenzene n-butyl acetate
6.3.4 Propylene Glycol Monomethyl Ether (PM)—Purity
7.4 Calibration for Propylene Glycol Monomethyl Ether
should be determined and the standard solution adjusted for
(PM):
this purity.
7.4.1 Make a needle-flash injection of the standard into the
6.3.5 Propylene Glycol Monomethyl Ether Acetate
chromatograph and separate according to the chromatographic
(PMA)—Purity should be determined and the standard solution
conditions in 7.3. At the end of the run, set the peak summing
adjusted for this purity.
windows to sum the isomer peaks as shown in Areas I and II
6.3.6 Tripropylene Glycol Monomethyl Ether (TPM)—
of Fig. 1.
Purity should be determined and the standard solution adjusted
7.4.2 Program the integrator to set the baseline at the same
for this purity.
time peak summation begins for the PM isomers. Force the
7. Calibration and Standardization
integrator to extend a baseline horizontally from the set
baseline.
7.1 Preparation of Calibration Standard Solution:
7.1.1 Propylene Glycol Monomethyl Ether (PM)—Weigh 7.4.3 Make another needle-flash injection of the standard
and calibrate the integrator according to the manufacturer’s
into a vial to within 0.1 mg, 10.00 g of PM calibration standard
(see 6.3.4) and 0.02 g of DPM. Check these reagents for purity operating instruction for an internal standard method. Re-
sponse factors should agree within the precision of this test
under the conditions used in the procedures and, if interfering
compounds are present, adjustment must be made in preparing method. If not, recalibrate and repeat the analysis.
7.4.4 If manual calculations are used, calculate the response
the standard.
factors RF for each component as follows:
7.1.2 Dipropylene Glycol Monomethyl Ether (DPM)—
Weigh into a vial to within 0.1 mg, 10.00 g of DPM calibration
RF 5 ~A 3 B!/~C 3 D! (1)
standard (see 6.3.3), 0.02 g of PM calibration standard (see
where:
6.3.4), and 0.02 g of TPM (see 6.3.6). Check these reagents for
A 5 peak area of internal standard,
purity under the conditions used in the procedure and, if
B 5 component of interest in standard, g,
interfering compounds are present, adjustment must be made in
C 5 peak area for component of interest in standard, and
preparing the standard.
D 5 internal standard in standard mixture, g.
7.1.3 Propylene Glycol Monomethyl Ether Acetate
(PMA)—Weigh into a vial to within 0.1 mg, 10.00 g of PMA
calibration standard (see 6.3.5) and 0.04 g of PM. Check these
reagents for purity under the conditions used in the procedure
and, if interfering compounds are present, adjustment must be
m
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