ASTM D4795-94(2008)
(Test Method)Standard Test Method for Nitrogen Content of Soluble Nitrocellulose—Alternative Method (Withdrawn 2017)
Standard Test Method for Nitrogen Content of Soluble Nitrocellulose<span class='unicode'>—</span>Alternative Method (Withdrawn 2017)
SIGNIFICANCE AND USE
This test method provides a simpler means for measuring the nitrogen content of nitrocellulose than the nitrometer described in Test Methods D 301. Under controlled conditions, the procedure described is capable of results equivalent to those obtained by the nitrometer.
SCOPE
1.1 Test Methods D 301 for measuring nitrogen content in nitrocellulose by nitrometer are the accepted standard. However, the glassware is specialized and the precision is dependent on the development of a high level of skill by the operator. The ferrous-sulfate titration of nitrate is a classical procedure. By controlling critical variables and automating the actual titration, precision equivalent to the nitrometer can be achieved with nitrocellulose. This test method describes such a procedure.
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 specific hazard statements, see Section 8.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in January 2017 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4795 − 94 (Reapproved 2008)
Standard Test Method for
Nitrogen Content of Soluble Nitrocellulose—Alternative
Method
This standard is issued under the fixed designation D4795; 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 4. Significance and Use
1.1 Test Methods D301 for measuring nitrogen content in
4.1 This test method provides a simpler means for measur-
nitrocellulose by nitrometer are the accepted standard.
ing the nitrogen content of nitrocellulose than the nitrometer
However, the glassware is specialized and the precision is
described in Test Methods D301. Under controlled conditions,
dependent on the development of a high level of skill by the
the procedure described is capable of results equivalent to
operator. The ferrous-sulfate titration of nitrate is a classical
those obtained by the nitrometer.
procedure. By controlling critical variables and automating the
actual titration, precision equivalent to the nitrometer can be
5. Interferences
achieved with nitrocellulose.This test method describes such a
5.1 The presence of moisture (or other volatile components)
procedure.
in the specimen will affect results. It is recommended that only
1.2 The values stated in SI units are to be regarded as the
thoroughly dry specimens be used.
standard. The values given in parentheses are for information
5.2 Temperature rise must be controlled during the titration.
only.
The cooling bath provides that control. However, if the rate of
1.3 This standard does not purport to address all of the
titrant addition is too fast, temperature may rise out of control.
safety concerns, if any, associated with its use. It is the
Results may then be erratic. Adherence to the procedure will
responsibility of the user of this standard to establish appro-
avoid temperature excursions. For optimum system efficiency,
priate safety and health practices and determine the applica-
room temperature should be maintained at 23 6 2°C.
bility of regulatory limitations prior to use. For specific hazard
5.3 The strength of the sulfuric acid used to dissolve the
statements, see Section 8.
specimen is very important.Too low an acid strength slows the
2. Referenced Documents
rate of solution which, in turn, causes titrations to be abnor-
mally slow. Results then become erratic.
2.1 ASTM Standards:
D301 Test Methods for Soluble Cellulose Nitrate (With-
drawn 2011) 6. Apparatus
D1193 Specification for Reagent Water
6.1 Acid Bottle Safety Dispenser.
3. Summary of Test Method
6.2 Brinkman 20 Titration System, or equivalent, with 25
mL amber buret:
3.1 A weighed specimen of nitrocellulose is dissolved in
sulfuric acid and titrated automatically with ferrous sulfate. 6.2.1 Electrode, platinum.
The nitrogen content of the specimen is calculated using the
6.2.2 Electrode, glass.
equivalence factor of the ferrous sulfate.
6.3 Desiccator, with drying agent.
6.4 Weighing bottles, 12-mLcapacity, aluminum (preferred)
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of or glass.
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
6.5 Analytical Balance, accurate to 60.1 mg.
Current edition approved June 1, 2008. Published June 2008. Originally
approved in 1988. Last previous edition approved in 2003 as D4795 – 94 (2003).
6.6 Ovens—135°C, for drying standards, and 100°C, for
DOI: 10.1520/D4795-94R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or drying specimens, having unexposed heating elements and the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
door latch removed.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
6.7 Circulating Unit, for chilled water, 5 6 2°C.
The last approved version of this historical standard is referenced on
www.astm.org. 6.8 Blender, with 0.25-L (8-oz) blender jar.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4795 − 94 (2008)
7. Reagents 10.2 Place the magnetic stirring bar into a dry 250-mL
beaker and fill the beaker with 150 mL of H SO (20 6 2°C).
2 4
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
10.3 Place the beaker in the cooling bath on the stirrer unit.
all reagents shall conform to the specifications of the Commit- Start the stirrer and adjust the speed for a slight vortex. Too
tee onAnalytical Reagents of theAmerican Chemical Society,
vigorous a vortex can cause the nitrocellulose to splash onto
where such specifications are available. Other grades may be the sides of the beaker.
used, provided it is first ascertained that the reagent is of
10.4 With the stirrer operating and the electrodes up in the
sufficiently high purity to permit its use without lessening the
air away from the acid, slowly pour the specimen into the
accuracy of the determination.
vortex of the swirl. Be careful not to touch the dispensing tip
7.2 Purity of Water—Unless otherwise indicated, references
or electrodes with the weighing bottle. Reweigh the weighing
to water shall be understood to mean reagent water as defined
bottle to find the weight of the standard by difference.
by Type III of Specification D1193.
10.5 Allow most of the KNO to dissolve. Visually inspect
7.3 Sulfuric Acid (H SO)95to98%.
2 4 the solution until no more chunks or chips of KNO remain.
The solution may be cloudy.
7.4 Ferrous Sulfate Solution—Dissolve 350 g of ferrous
sulfate crystals (FeSO ) in 1000 mL of distilled water. Add
10.6 Lower the electrodes and the dispensing tip into the
1000 mL of 1+1 H SO solution. Makes 2 L.
2 4 H SO .
2 4
7.5 Potassium Nitrate (KNO ) Standard or an equivalent
10.7 Set the controls to the desired settings.
nitrate primary standard.
10.8 As the KNO dissolves and HNO is formed by the
3 3
7.6 Nitrocellulose Standard—Asample with a known nitro-
reaction of H SO and the specimen, a millivolt potential
2 4
gen value or other known organic nitrate.
change is evident by a rising recorder pen.
10.8.1 When the pen shows a leveling off, it is an indication
8. Hazards
that the majority of the KNO is in solution. Visually inspect
8.1 Since the sample of nitrocellulose must be dried, it is
the solution to verify the fact that chips are no longer present.
imperative that care be exercised in storage, handling, and
10.9 Settheburetcontroltoarateofabout5mL/min.Allow
disposal. Dry nitrocellu
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