ASTM D3133-96
(Test Method)Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry
Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry
SCOPE
1.1 This test method covers the quantitative determination of the content of cellulose nitrate (also known as nitrocellulose) in lacquers containing alkyd resins.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3This 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. For a specific hazard statement, see 7.1.1.
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Designation: D 3133 – 96
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
Quantitative Determination of Cellulose Nitrate in Alkyd
Modified Lacquers by Infrared Spectrophotometry
This standard is issued under the fixed designation D 3133; 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 quantitatively analyzed for the cellulosic derivative without
isolating it. The test method is applicable to lacquers for which
1.1 This test method covers the quantitative determination
the grade of nitrocellulose is known and available. Other
of the content of cellulose nitrate (also known as nitrocellulose)
cellulosics, alkyd resins, many vinyl resins, and solvents do not
in lacquers containing alkyd resins.
interfere. Components, such as acrylic resins and some vinyl
1.2 The values stated in inch-pound units are to be regarded
−1
polymers, that absorb infrared near 848 cm (11.8 μm) inter-
as the standard. The values given in parentheses are for
fere with the determination. High boiling ester solvents, in
information only.
particular methyl cellosolve acetate, may also interfere with the
1.3 This standard does not purport to address all of the
determination if not removed in the evaporation procedure (see
safety concerns, if any, associated with its use. It is the
8.3).
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. For a specific
5.1 Infrared Spectrophotometer, automatic recording,
hazard statement, see Note 1.
double-beam. Most infrared spectrophotometers operate from
−1
2. Referenced Documents 4000 to 650 cm (2.5 to 15 μm), but in this test method only
−1
the range between 1000 and 750 cm (10 to 14 μm) is used.
2.1 ASTM Standards:
2 See Practices E 168.
D 1644 Test Methods for Nonvolatile Content of Varnishes
5.2 Absorption Cells, sealed, with sodium chloride (NaCl)
D 2372 Practice for Separation of Vehicle from Solvent-
windows, 0.1-mm path length, one pair approximately
Reducible Paints
matched.
E 168 Practices for General Techniques of Infrared Quanti-
5.3 Film Vacuum Evaporator, rotary thin or equivalent
tative Analysis
apparatus, to obtain redissolvable lacquer solids without de-
E 275 Practice for Describing and Measuring Performance
composition of the cellulose nitrate.
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
5.4 Oven, vacuum drying, thermostatically controlled to
eters
operate at 65 6 2C.
3. Summary of Test Method
6. Reagents
3.1 The method of standard additions is employed. Incre-
6.1 Purity of Reagents— Reagent grade chemicals shall be
ments of cellulose nitrate, in solution, are added to aliquots of
used in all tests. Unless otherwise indicated, it is intended that
the sample. Absorbance measurements are made of the band at
−1
all reagents shall conform to the specifications of the Commit-
848 cm (11.8 μm) for each addition. The original content is
tee on Analytical Reagents of the American Chemical Society,
then calculated from absorbance versus concentration.
where such specifications are available. Other grades may be
4. Significance and Use used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
4.1 Coating compositions based on a mixture of synthetic
accuracy of the determination.
resins and cellulose nitrate dissolved in organic solvents are
6.2 Cellulose Nitrate, of the same grade as in the sample.
This method is under the jurisdiction of ASTM Committee D-1 on Paint and
Related Coatings, Materials, and Applications and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.55 on Factory-Applied Coatings on Preformed Products. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved Nov. 10, 1996. Published January 1997. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
e1
published as D 3133 – 72. Last previous edition D 3133 – 72 (1989) . Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 03.06. MD.
D 3133
6.3 N, N-Dimethylacetamide (DMA), spectrograde quality.
6.4 Nitrogen Gas, dry.
7. Standard Solution
7.1 Thoroughly dry a quantity of cellulose nitrate at 65°C,
in the vacuum oven (Note 1). Transfer 4000 g, weighed to 0.1
mg, to a 200-mL volumetric flask. Add DMA, shake to dissolve
the cellulose nitrate, and dilute to volume with DMA. One
millilitre of solution is equivalent to 20 m
...
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