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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09-May-2001
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ASTM D3133-01 - Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 3133 – 01
Standard Test Method for
Quantitative Determination of Cellulose Nitrate in Alkyd
1
Modified Lacquers by Infrared Spectrophotometry
This standard is issued under the fixed designation D3133; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope isolatingit.Thetestmethodisapplicabletolacquersforwhich
the grade of nitrocellulose is known and available. Other
1.1 This test method covers the quantitative determination
cellulosics,alkydresins,manyvinylresins,andsolventsdonot
ofthecontentofcellulosenitrate(alsoknownasnitrocellulose)
interfere. Components, such as acrylic resins and some vinyl
in lacquers containing alkyd resins.
−1
polymers, that absorb infrared near 11.8 µm (848 cm )
1.2 The values stated in SI units are to be regarded as the
interferewiththedetermination.Highboilingestersolvents,in
standard. The values given in parentheses are for information
particularmethylcellosolveacetate,mayalsointerferewiththe
only.
determinationifnotremovedintheevaporationprocedure(see
1.3 This standard does not purport to address all of the
8.3).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Infrared Spectrophotometer, automatic recording,
bility of regulatory limitations prior to use. For a specific
double-beam. Most infrared spectrophotometers operate from
hazard statement, see 7.1.1.
−1
2.5 to 15 µm (4000 to 650 cm ) , but in this test method only
−1
2. Referenced Documents the range between 10 to 14 µm (1000 and 750 cm ) is used.
See Practices E168.
2.1 ASTM Standards:
2
5.2 Absorption Cells, sealed, with sodium chloride (NaCl)
D1644 TestMethodsforNonvolatileContentofVarnishes
windows, 0.1-mm path length, one pair approximately
D2372 Practice for Separation of Vehicle from Solvent-
2
matched.
Reducible Paints
5.3 Film Vacuum Evaporator, rotary thin or equivalent
E168 Practices for General Techniques of Infrared Quanti-
3
apparatus, to obtain redissolvable lacquer solids without de-
tative Analysis
composition of the cellulose nitrate.
E275 Practice for Describing and Measuring Performance
5.4 Oven, vacuum drying, thermostatically controlled to
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
3 operate at 65 62C.
eters
6. Reagents
3. Summary of Test Method
6.1 Purity of Reagents— Reagent grade chemicals shall be
3.1 The method of standard additions is employed. Incre-
used in all tests. Unless otherwise indicated, it is intended that
ments of cellulose nitrate, in solution, are added to aliquots of
all reagents shall conform to the specifications of the Commit-
thesample.Absorbancemeasurementsaremadeofthebandat
−1
tee onAnalytical Reagents of theAmerican Chemical Society,
848 cm (11.8 µm) for each addition. The original content is
4
where such specifications are available. Other grades may be
then calculated from absorbance versus concentration.
used, provided it is first ascertained that the reagent is of
4. Significance and Use sufficiently high purity to permit its use without lessening the
accuracy of the determination.
4.1 Coating compositions based on a mixture of synthetic
6.2 Cellulose Nitrate, of the same grade as in the sample.
resins and cellulose nitrate dissolved in organic solvents are
6.3 N, N-Dimethylacetamide (DMA), spectrograde quality.
quantitatively analyzed for the cellulosic derivative without
6.4 Nitrogen Gas, dry.
1
This method is under the jurisdiction of ASTM Committee D01 on Paint and
4
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 May 10, 2001. Published July 2001. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D3133–72. Last previous edition D3133–96. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
2
Annual Book of ASTM Standards, Vol 06.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
3
Annual Book of ASTM Standards, Vol 03.06. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D 3133
7. Standard Solution
7.1 Thoroughly dry a quantity of cellulose nitrate at 65°C,
in the vacuum
...

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