Standard Test Method for Determination of Titanium in Nickel Alloys by Diantipyrylmethane Molecular Absorption Spectrometric Method

SIGNIFICANCE AND USE
This practice is used for the analysis of nickel and nickel base alloy samples by molecular absorption spectrometry to check compliance with compositional specifications. It is assumed that all who use the procedure will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described in Guide E 882.
SCOPE
1.1 This test method covers the determination of titanium in nickel alloys in the 0.3 through 5.0 % range. With appropriate reference materials the test method may be extended down to 0.05 %.
1.2 Molybdenum, if present, may cause a high bias to the extent of 0.001 % Ti for every 1 % Mo.
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 hazards associated with the use of this test method see Practices E 50.

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Publication Date
09-Oct-2002
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ASTM E1938-02 - Standard Test Method for Determination of Titanium in Nickel Alloys by Diantipyrylmethane Molecular Absorption Spectrometric Method
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Designation:E1938–02
Standard Test Method for
Determination of Titanium in Nickel Alloys by the
Diantipyrylmethane Molecular Absorption Spectrometric
1
Method
This standard is issued under the fixed designation E 1938; 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 ISO 11433:1993(E) - Nickel Alloys - Determination of
Titanium Content - Diantipyrylmethane Molecular Ab-
1.1 This test method covers the determination of titanium in
3
sorption Spectrometric Method
nickel alloys in the 0.3 through 5.0 % range. With appropriate
reference materials the test method may be extended down to
3. Summary of Test Method
0.05 %.
3.1 This sample is dissolved in a mixture of hydrochloric
1.2 Molybdenum, if present, may cause a high bias to the
and nitric acid. The solution is evaporated to sulfuric acid
extent of 0.001 % Ti for every 1 % Mo.
fumes to remove the hydrochloric and nitric acids. Color is
1.3 This standard does not purport to address all of the
developed with diantipyrylmethane, and the absorbance is
safety concerns, if any, associated with its use. It is the
measured at 390 nm.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.Forspecifichazards
4.1 Thispracticeisusedfortheanalysisofnickelandnickel
associated with the use of this test method see PracticesE50.
base alloy samples by molecular absorption spectrometry to
2. Referenced Documents check compliance with compositional specifications. It is
2 assumed that all who use the procedure will be trained analysts
2.1 ASTM Standards:
capable of performing common laboratory procedures skill-
E50 Practices forApparatus, Reagents, and Safety Precau-
fully and safely. It is expected that the work will be performed
tions for Chemical Analysis of Metals
in a properly equipped laboratory and that proper waste
E 882 Guide for Accountability and Quality Control in the
disposal procedures will be followed. Appropriate quality
Chemical Analysis Laboratory
control practices must be followed such as those described in
E 1452 Practice for Preparation of Calibration Solutions for
Guide E 882.
Spectrophotometric and for Spectroscopic Atomic Analy-
sis
5. Apparatus
E 1601 Practice for Conducting an Interlaboratory Study to
5.1 Spectrophotometer, capable of measuring absorbance at
Evaluate the Performance of an Analytical Method
a wavelength of 390 nm.
2.2 ISO Standards:
5.2 Cells, to fit spectrophotometer, having an optical path of
ISO 5725:1986 - Precision of Test Methods – Determina-
1 cm.
tion of Repeatability and Reproducibility for a Standard
3
Test Method by Inter-Laboratory Tests
NOTE 1—Cells having other dimensions can be used, provided suitable
adjustments can be made in the amount of sample and reagents used.
1
This test method is under the jurisdiction of ASTM Committee E01 on
6. Reagents
Analytical Chemistry of Metals, Ores and Related Materials, and is the direct
6.1 Purity and Concentration of Reagents—The purity and
responsibility of Subcommittee E01.08 on Nickel, Cobalt and High Temperature
Alloys. concentration of common chemical reagents shall conform to
Current edition approved Oct 10, 2002. Published June 2003. Originally
PracticesE50. The reagents should be free of or contain only
approved in 1997. Last previous edition approved in 1997 as E 1938–97.
minimal amounts (< 0.1 µg/g) of titanium. Calibration solu-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tions shall be prepared in accordance with Practice E 1452.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
6.2 Potassium Hydrogen Sulfate (KHSO ).
4
the ASTM website.
6.3 Ascorbic Acid Solution—Dissolve 20 g ascorbic acid
3
Available from American National Standards Institute, 11 West 42nd Street,
(C H O ) in water, dilute to 200 mL and mix.
6 8 6
New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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E1938–02
TABLE 1 Weight of Sample to be Taken
6.4 Oxalic Acid Solution—Dissolve 10 g of oxalic acid
dihydrate [(COOH) 2H O] in water and dilute to 200 mL and Expected Ti Content, Weight of Test Portion,
2 2
% g
mix.
0.3 to 3.0 0.19 to 0.21
6.5 Diantipyrylmethane Solution—Dissolve4gof dian-
3.0 to 5.0 0.09 to 0.11
tipyrylmethane monohydrate (C H N O H O) in water con-
23 24 4 2 2
tain
...

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