ASTM D4589-96

Standard Test Method for Nitrobenzene in Aniline (Withdrawn 2002)

SCOPE
1.1 This test method covers a polarographic procedure for the determination of nitrobenzene in aniline.
1.2 This test method has been found applicable to the determination of nitrobenzene in aniline containing concentrations of not more than 25 mg/kg nitrobenzene.
1.3 This standard does not purport to address all of the safety problems, 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 9 and Note 3.

General Information

• Status: Withdrawn
• Publication Date: 09-Dec-1996
• Withdrawal Date: 09-Jan-2002
• ICS: 71.080.30 - Organic nitrogen compounds
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4589 – 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
Nitrobenzene in Aniline
This standard is issued under the fixed designation D 4589; 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 3. Terminology
1.1 This test method covers a polarographic procedure for 3.1 See Terminology D 4790 for definition of terms used in
the determination of nitrobenzene in aniline. this test method.
1.2 This test method has been found applicable to the
4. Summary of Test Method
determination of nitrobenzene in aniline containing concentra-
tions of not more than 25 mg/kg nitrobenzene. 4.1 Polarography is an electrochemical method of analysis.
A quantitative evaluation of an electro-reducible material such
1.3 The following applies to all specified limits in this test
method: for purposes of determining conformance with this as nitrobenzene can be determined by measuring the charac-
teristic current flow, as a function of an increasingly applied
test method, an observed value or a calculated value shall be
rounded off “to the nearest unit” in the last right-hand digit voltage, resulting from the solution undergoing electrolysis.
4.2 The current flowing through the specimen during the
used in expressing the specification limit, in accordance with
the rounding-off method of Practice E 29. analysis is in the microampere range so several polarograms
can be obtained on the same specimen solution without
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the significant differences.
4.3 The nitrobenzene content is determined by mixing four
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- volumes of aniline with one volume of concentrated hydro-
bility of regulatory limitations prior to use. For specific hazard chloric acid. The diffusion current of nitrobenzene is then
measured by polarographic technique. A standard calibration
statements, see Section 10 and Note 3.
graph is developed with various concentrations of nitrobenzene
2. Referenced Documents
in aniline versus their diffusion currents. A reading of the
2.1 ASTM Standards: diffusion current level of the test specimen from the calibration
D 1193 Specification for Reagent Water graph determines its nitrobenzene content.
D 1549 Test Method for Zinc in Lubricating Oils and
3 5. Significance and Use
Additives (Polarographic Method)
5.1 This test method gives a quantitative means of detection
D 3436 Practice for Sampling and Handling Aniline
D 4790 Terminology of Aromatic Hydrocarbons and Re- of nitrobenzene in industrial grade aniline both for quality
control and quality assurance of the product.
lated Chemicals
E 29 Practice for Using Significant Digits in Test Data to
5 6. Interferences
Determine Conformance with Specifications
6.1 Since the diffusion coefficient for solutions of organic
E 50 Practices for Apparatus, Reagents, and Safety Precau-
molecules can possibly increase up to 2 % per degree rise in
tions for Chemical Analysis of Metals
temperature, the polarographic cell temperature should be
2.2 Other Document:
relatively the same when comparing specimen analyses with
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
standard calibration analyses.
1910.1200
6.2 The sensitivity of an analysis is affected by the dimen-
sions of the dropping mercury electrode (DME) capillary and
This test method is under the jurisdiction of ASTM Committee D-16 on
also by the height of the mercury column above the electrode.
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
It is advisable to use the same DME capillary with a constant
Subcommittee D16.0D on Organic Nitrogen Compounds.
head of mercury that will yield a uniform dropping rate during
Current edition approved Dec. 10, 1996. Published February 1997. Originally
published as part of D 3264 – 73 T. Last previous edition D 3264 – 91.
a series of analyses. Recalibrate when the DME is changed.
Annual Book of ASTM Standards, Vol 11.01.
6.3 Sudden or severe vibrations of the DME system can
Discontinued 1984: see 1984 Annual Book of ASTM Standards, Part 23.
cause interferences in the resulting polarogram.
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 14.02. 6.4 Residual dissolved oxygen in the specimen solution will
Annual Book of ASTM Standards, Vol 03.05.
interfere with the analysis. This test method includes a nitrogen
Available from Superintendent of Documents, U.S. Government Printing
purge to remove dissolved oxygen.
Office, Washington, DC 20402.
D 4589
7. Apparatus handling, and the immediate cleaning of mercury spills.
10.2 Consult current OSHA regulations, suppliers’ Material
7.1 Recording Polarograph—However, a nonrecording po-
Safety Data Sheets, and local regulations for all materials used
larograph may be adapted for this test method.
in this test method.
7.2 Electrodes:
7.2.1 Dropping Mercury Electrode Capillary.
11. Sampling and Handling
7.2.2 Electrolysis Vessel, with a mercury pool reference
11.1 Sample the material in accordance with Practice
electrode.
D 3436.
NOTE 1—Suitable electrolysis assemblies are shown in Test Method
12. Calibration and Standardization
D 1549 and Practices E 50. Any other cell that will perform similarly may
12.1 The DME capillary has an average length of approxi-
be used.
mately 80 mm and a bore of approximately 0.04 mm. The
7.3 Nitrogen Bubbler System and Purification Assembly.
height of the mercury column and reservoir will normally vary
NOTE 2—If the nitrogen being used contains enough oxygen to interfere
from 400 to 800 mm. The exact length of the capillary and the
with the polarogram, it must be purified by passing the gas over copper
height of the mercury column are determined by trial and error
turnings at 450°C.
to give a mercury drop-time from 3 to 5 s/drop when it is
7.4 Tubing, flexible, vinyl for connections. Rubber tubing
immersed in a solution of the type to be tested.
should be avoided due to the possibility of oxygen permeation.
12.2 Operate the polarograph in accordance with th
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