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ASTM D3133-01(2005)

(Test Method)

Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry (Withdrawn 2008)

Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry (Withdrawn 2008)

SIGNIFICANCE AND USE
Coating compositions based on a mixture of synthetic resins and cellulose nitrate dissolved in organic solvents are quantitatively analyzed for the cellulosic derivative without isolating it. The test method is applicable to lacquers for which the grade of nitrocellulose is known and available. Other cellulosics, alkyd resins, many vinyl resins, and solvents do not interfere. Components, such as acrylic resins and some vinyl polymers, that absorb infrared near 11.8 μm (848 cm−1) interfere with the determination. High boiling ester solvents, in particular methyl cellosolve acetate, may also interfere with the determination if not removed in the evaporation procedure (see 8.3).
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.
1.3 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. For a specific hazard statement, see 7.1.1.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in June 2008. This standard is being withdrawn without replacement due to its limited use by industry.

General Information

Status
Withdrawn
Publication Date
14-May-2005
Withdrawal Date
10-Jun-2008
ICS
87.040 - Paints and varnishes
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.55 - Factory Applied Coatings on Preformed Products
Current Stage
Ref Project

Relations

Replaces
ASTM D3133-01 - Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry
Effective Date
15-May-2005

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ASTM D3133-01(2005) - Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry (Withdrawn 2008)ASTM D3133-01(2005) - Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry (Withdrawn 2008)
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ASTM D3133-01(2005) - Standard Test Method for Quantitative Determination of Cellulose Nitrate in Alkyd Modified Lacquers by Infrared Spectrophotometry (Withdrawn 2008)
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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: D 3133 – 01 (Reapproved 2005)
Standard Test Method for
Quantitative Determination of Cellulose Nitrate in Alkyd
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
1. Scope 11.8 µm (848 cm ) for each addition. The original content is
then calculated from absorbance versus concentration.
1.1 This test method covers the quantitative determination
ofthecontentofcellulosenitrate(alsoknownasnitrocellulose)
4. Significance and Use
in lacquers containing alkyd resins.
4.1 Coating compositions based on a mixture of synthetic
1.2 The values stated in SI units are to be regarded as the
resins and cellulose nitrate dissolved in organic solvents are
standard. The values given in parentheses are for information
quantitatively analyzed for the cellulosic derivative without
only.
isolatingit.Thetestmethodisapplicabletolacquersforwhich
1.3 This standard does not purport to address all of the
the grade of nitrocellulose is known and available. Other
safety concerns, if any, associated with its use. It is the
cellulosics,alkydresins,manyvinylresins,andsolventsdonot
responsibility of the user of this standard to establish appro-
interfere. Components, such as acrylic resins and some vinyl
priate safety and health practices and determine the applica-
−1
polymers, that absorb infrared near 11.8 µm (848 cm )
bility of regulatory limitations prior to use. For a specific
interferewiththedetermination.Highboilingestersolvents,in
hazard statement, see 7.1.1.
particularmethylcellosolveacetate,mayalsointerferewiththe
2. Referenced Documents determinationifnotremovedintheevaporationprocedure(see
8.3).
2.1 ASTM Standards:
D1644 Test Methods for Nonvolatile Content of Varnishes
5. Apparatus
D2372 Practice for Separation of Vehicle from Solvent-
5.1 Infrared Spectrophotometer, automatic recording,
Reducible Paints
double-beam. Most infrared spectrophotometers operate from
E168 Practices for General Techniques of Infrared Quanti-
−1
2.5 to 15 µm (4000 to 650 cm ), but in this test method only
tative Analysis
−1
the range between 10 to 14 µm (1000 and 750 cm ) is used.
E275 Practice for Describing and Measuring Performance
See Practices E168.
of Ultraviolet, Visible, and Near-Infrared Spectrophotom-
5.2 Absorption Cells, sealed, with sodium chloride (NaCl)
eters
windows, 0.1-mm path length, one pair approximately
3. Summary of Test Method matched.
5.3 Film Vacuum Evaporator, rotary thin or equivalent
3.1 The method of standard additions is employed. Incre-
apparatus, to obtain redissolvable lacquer solids without de-
ments of cellulose nitrate, in solution, are added to aliquots of
composition of the cellulose nitrate.
thesample.Absorbancemeasurementsaremadeofthebandat
5.4 Oven, vacuum drying, thermostatically controlled to
operate at 65 62C.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
andRelatedCoatings,Materials,andApplicationsandisthedirectresponsibilityof 6. Reagents
Subcommittee D01.55 on Factory Applied Coatings on Preformed Products.
6.1 Purity of Reagents—Reagent grade chemicals shall be
Current edition approved May 15, 2005. Published June 2005. Originally
used in all tests. Unless otherwise indicated, it is intended that
approved in 1972. Last previous edition approved in 2001 as D3133–01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
all reagents shall conform to the specifications of the Commit-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tee onAnalytical Reagents of theAmerican Chemical Society,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3133 – 01 (2005)
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
6.2 Cellulose Nitrate, of the same grade as in the sample.
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 (7.1.1). Transfer 4000 g, weighed to 0.1
mg,toa200-mLvolumetricflask.AddDMA,shaketodissolve
the cellulose nitrate, and dilute to volume with DMA. One
millilitreofsolutionisequivalentto20mgofcellulosenitrate.
7.1.1 Warning; Every precaution must be exercised in the FIG.1PlotofDA verses Cellulose Nitrate Additions
handling and drying of cellulose nitrate because of its explo-
sivenature.Nomorethan15gshouldbedriedatanyonetime.
−1
minimum at 12.3 µm (813 cm ). Determine the mean DA for
8. Procedure
the three runs on each solution.
8.1 If the material is pigmented, remove the pigment quan-
9. Calculation
titativelyinaccordancewithPracticeD2372,andproceedwith
the determination on the vehicle.
9.1 Plottheabsorbancedifference, D A,versusthecellulose
8.2 Determine the nonvolatile content o
...

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