ASTM E1917-13
(Test Method)Standard Test Method for Determination of Phosphorus in Nickel, Ferronickel, and Nickel Alloys by Phosphovanadomolybdate Spectrophotometry
Standard Test Method for Determination of Phosphorus in Nickel, Ferronickel, and Nickel Alloys by Phosphovanadomolybdate Spectrophotometry
SIGNIFICANCE AND USE
5.1 This test method is used for the determination of phosphorus in nickel, ferronickel, and nickel 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 E882.
SCOPE
1.1 This test method covers the determination of phosphorus in nickel, ferronickel, and nickel alloys in the range 0.0007 % to 0.05 %.
1.2 Arsenic, chromium, hafnium, niobium, silicon, tantalum, titanium, and tungsten interfere, but the interference can be avoided by complexation or volatilization (for chromium). The lowest phosphorus content (0.0007 %) can be reached only in samples with low contents of interfering elements.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 E50. Refer to specific warning notes given throughout this test method.
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Designation: E1917 − 13
Standard Test Method for
Determination of Phosphorus in Nickel, Ferronickel, and
Nickel Alloys by Phosphovanadomolybdate
1
Spectrophotometry
This standard is issued under the fixed designation E1917; 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 Chemical Analysis Laboratory
E1601 Practice for Conducting an Interlaboratory Study to
1.1 This test method covers the determination of phospho-
Evaluate the Performance of an Analytical Method
rus in nickel, ferronickel, and nickel alloys in the range
3
2.2 ISO Standards:
0.0007 % to 0.05 %.
ISO 5725:1986 Precision of Test Methods—Determination
1.2 Arsenic, chromium, hafnium, niobium, silicon,
of Repeatability and Reproducibility for a Standard Test
tantalum, titanium, and tungsten interfere, but the interference
Method by Inter-laboratory Tests
can be avoided by complexation or volatilization (for chro-
ISO 11400:1992(E) Nickel, Ferronickel, and Nickel
mium). The lowest phosphorus content (0.0007 %) can be
Alloys—Determination of Phosphorus Content—
reached only in samples with low contents of interfering
Phosphovanadomolybdate MolecularAbsorption Spectro-
elements.
metric Method
1.3 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
standard. 3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology E135.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 The sample is dissolved in a mixture of HCl and HNO .
priate safety and health practices and determine the applica- 3
HClO is added and the solution is evaporated to fumes of
bility of regulatory limitations prior to use.Forspecifichazards
4
HClO to remove chromium as volatile chromyl chloride.
associated with the use of this test method see Practices E50.
4
Silicon and refractory elements are complexed with fluoride
Refer to specific warning notes given throughout this test
ions through the addition of HF. Phosphorus is converted to
method.
phosphovanadomolybdicacidinanHClO andHNO solution.
4 3
2. Referenced Documents The phosphovanadomolybdic acid is extracted with 2-methyl-
2
2-pentanone in the presence of citric acid to complex arsenic.
2.1 ASTM Standards:
Absorbance is measured at 355 nm.
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
5. Significance and Use
Related Materials
5.1 This test method is used for the determination of
E135 Terminology Relating to Analytical Chemistry for
phosphorus in nickel, ferronickel, and nickel alloy samples by
Metals, Ores, and Related Materials
molecular absorption spectrometry to check compliance with
E882 Guide for Accountability and Quality Control in the
compositional specifications. It is assumed that all who use the
procedure will be trained analysts capable of performing
1 common laboratory procedures skillfully and safely. It is
This practice is under the jurisdiction of ASTM Committee E01 on Analytical
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of expected that the work will be performed in a properly
Subcommittee E01.08 on Ni and Co and High Temperature Alloys.
equipped laboratory and that proper waste disposal procedures
Current edition approved Oct. 1, 2013. Published October 2013. Originally
will be followed.Appropriate quality control practices must be
approved in 1997. Last previous edition approved in 2008 as E1917 – 08. DOI:
followed, such as those described in Guide E882.
10.1520/E1917-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1917 − 13
TABLE 1 Weight of Test Portion of the Sample
conform to Practices E50. The reagents should be free of or
Expected Maximum concentration of the interfering contain only minimal amounts (< 0.1 µg/g) of phosphorus.
Weight of Test
Phosphorus elements, %
7.1.1 Verify the absence of phosphorus in the reagents using
Portion,
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1917 − 08 E1917 − 13
Standard Test Method for
Determination of Phosphorus in Nickel, Ferronickel, and
Nickel Alloys by Phosphovanadomolybdate Molecular
1
Absorption SpectrometrySpectrophotometry
This standard is issued under the fixed designation E1917; 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
1.1 This test method covers the determination of phosphorus in nickel, ferronickel, and nickel alloys in the range 0.0007 % to
0.05 %.
1.2 Arsenic, chromium, hafnium, niobium, silicon, tantalum, titanium, and tungsten interfere, but the interference can be
avoided by complexation or volatilization (for chromium). The lowest phosphorus content (0.0007 %) can be reached only in
samples with low contents of interfering elements.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 E50. Refer to specific warning
notes given throughout this test method.
2. Referenced Documents
2
2.1 ASTM Standards:
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
3
2.2 ISO Standards:
ISO 5725:1986 Precision of Test Methods—Determination of Repeatability and Reproducibility for a Standard Test Method by
Inter-laboratory Tests
ISO 11400:1992(E) Nickel, Ferronickel, and Nickel Alloys—Determination of Phosphorus Content—Phosphovanadomolybdate
Molecular Absorption Spectrometric Method
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The sample is dissolved in a mixture of HCl and HNO . HClO is added and the solution is evaporated to fumes of HClO
3 4 4
to remove chromium as volatile chromyl chloride. Silicon and refractory elements are complexed with fluoride ions through the
addition of HF. Phosphorus is converted to phosphovanadomolybdic acid in an HClO and HNO solution. The phosphovana-
4 3
domolybdic acid is extracted with 2-methyl-2-pentanone in the presence of citric acid to complex arsenic. Absorbance is measured
at 355 nm.
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.08 on Ni and Co and High Temperature Alloys.
Current edition approved Dec. 15, 2008Oct. 1, 2013. Published January 2009October 2013. Originally approved in 1997. Last previous edition approved in 20022008 as
E1917 – 02.E1917 – 08. DOI: 10.1520/E1917-08.10.1520/E1917-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1917 − 13
5. Significance and Use
5.1 This test method is used for the determination of phosphorus in nickel, ferronickel, and nickel 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 practice
...
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