ASTM E1587-94(1998)
(Test Method)Standard Test Methods for Chemical Analysis of Refined Nickel
Standard Test Methods for Chemical Analysis of Refined Nickel
SCOPE
1.1 These test methods apply to the chemical analysis of refined nickel and other forms of metallic nickel having chemical compositions within the following limits: Element Weight % Antimony, less than 0.005 Arsenic, less than 0.005 Bismuth, less than 0.01 Cadmium, less than 0.0025 Carbon, max 0.03 Cobalt, max 1.00 Copper, max 1.00 Hydrogen, max 0.003 Iron, max 0.15 Lead, less than 0.01 Manganese, less than 0.20 Nickel, min 98.0 Nitrogen, less than 0.50 Oxygen, less than 0.03 Phosphorus, less than 0.005 Selenium, less than 0.0010 Silicon, less than 0.005 Silver, less than 0.01 Sulfur, max 0.01 Tellurium, less than 0.0010 Thallium, less than 0.0010 Tin, less than 0.005 Zinc, less than 0.015
1.2 These test methods may be used to determine the following elements in the sections indicated below: Sections Antimony, Arsenic, Bismuth, Cadmium, Lead, Selenium, 20 to 30 Silver, Tellurium, Tin, and Thallium by the Electrothermal Atomic Absorption Method Bismuth, Cadmium, Cobalt, Copper, Iron, Lead, Manganese, Silver, and Zinc by the Flame Atomic 8 to 19 Absorption Method Carbon, Total, by the Combustion-Instrumental Method 8 31 to 42 Nickel by the Dimethylglyoxime Gravimetric Method 12 91 to 99 Nitrogen by the Inert Gas Fusion Thermal Conductivity Method 8 66 to 77 Oxygen by the Inert Gas Fusion Method 8 78 to 90 Sulfur by the Infrared Absorption Method 8 43 to 54 Sulfur by the Methylene Blue Spectrophotometric Method After Generation of Hydrogen Sulfide 55 to 65
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 precautions, see Section 5.
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Designation: E 1587 – 94 (Reapproved 1998)
Standard Test Methods for
Chemical Analysis of Refined Nickel
This standard is issued under the fixed designation E 1587; 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 1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods apply to the chemical analysis of
responsibility of the user of this standard to establish appro-
refined nickel and other forms of metallic nickel having
priate safety and health practices and determine the applica-
chemical compositions within the following limits:
bility of regulatory limitations prior to use. For specific
Element Weight %
precautions, see Section 5.
Antimony, less than 0.005
Arsenic, less than 0.005
2. Referenced Documents
Bismuth, less than 0.01
2.1 ASTM Standards:
Cadmium, less than 0.0025
Carbon, max 0.03
D 1193 Specification for Reagent Water
Cobalt, max 1.00
E 29 Practice for Using Significant Digits in Test Data to
Copper, max 1.00
Determine Conformance with Specifications
Hydrogen, max 0.003
Iron, max 0.15
E 39 Methods for Chemical Analysis of Nickel
Lead, less than 0.01
E 50 Practices for Apparatus, Reagents, and Safety Precau-
Manganese, less than 0.20
tions for Chemical Analysis of Metals
Nickel, min 98.0
Nitrogen, less than 0.50
E 60 Practice for Photometric and Spectrophotometric
Oxygen, less than 0.03
Methods for Chemical Analysis of Metals
Phosphorus, less than 0.005
Selenium, less than 0.0010 E 107 Test Methods for Chemical Analysis of Electronic
Silicon, less than 0.005
Nickel
Silver, less than 0.01
E 173 Practice for Conducting Interlaboratory Studies of
Sulfur, max 0.01
Methods for Chemical Analysis of Metals
Tellurium, less than 0.0010
Thallium, less than 0.0010
E 354 Test Methods for Chemical Analysis of High-
Tin, less than 0.005
Temperature, Electrical, Magnetic, and Other Similar Iron,
Zinc, less than 0.015
Nickel, and Cobalt Alloys
1.2 These test methods may be used to determine the
E 882 Guide for Accountability and Quality Control in the
following elements in the sections indicated below: 8
Chemical Analysis Laboratory
Sections
E 1019 Test Methods for Determination of Carbon, Sulfur,
Nitrogen, Oxygen, and Hydrogen in Steel and in Iron,
Antimony, Arsenic, Bismuth, Cadmium, Lead, Selenium, 20 to 30
Silver, Tellurium, Tin, and Thallium by the Electrothermal Nickel, and Cobalt Alloys
Atomic Absorption Method
E 1024 Guide for Chemical Analysis of Metals and Metal
Bismuth, Cadmium, Cobalt, Copper, Iron, Lead, Manga- 8to19
Bearing Ores by Flame Absorption Spectrophotometry
nese, Silver, and Zinc by the Flame Atomic Absorption
Method 2.2 ISO Standard:
Carbon, Total, by the Combustion-Instrumental Method 31 to 42
ISO 5725 Precision of Test Methods—Determination of
Nickel by the Dimethylglyoxime Gravimetric Method 91 to 99
Repeatability and Reproducibility by Interlaboratory
Nitrogen by the Inert Gas Fusion Thermal Conductivity 66 to 77
3 9
Method
Tests
Oxygen by the Inert Gas Fusion Method 78 to 90
Sulfur by the Infrared Absorption Method 43 to 54
Sulfur by the Methylene Blue Spectrophotometric Method 55 to 65
After Generation of Hydrogen Sulfide This method appears in Test Methods E 1019 – 88, in the 1992 Annual Book of
ASTM Standards, Vol 03.05.
Supporting data are available from ASTM Headquarters. Request RR:E03-
1051.
1 5
These test methods are under the jurisdiction of ASTM Committee E-1 on Annual Book of ASTM Standards, Vol 11.01.
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct Annual Book of ASTM Standards, Vol 14.02.
responsibility of Subcommittee E01.08 on Ni and Co and High-TemperatureAlloys. Annual Book of ASTM Standards, Vol 03.05.
Current edition approved Jan. 15, 1994. Published March 1994. Annual Book of ASTM Standards, Vol 03.06.
2 9
These methods represent revisions of, and replacements for, methods covered Available from American National Standards Institute, 11 W. 42nd St., 13th
by Methods E 39 and E 107. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1587 – 94 (1998)
3. Significance and Use 6.4 If the laboratory sample contains particles or pieces of
widely varying sizes, the test sample should be obtained by
3.1 These test methods are primarily intended to test refined
riffling or coning and quartering techniques.
nickel metal for compliance with compositional specifications.
Itisassumedthatallwhousethesetestmethodswillbetrained
7. Rounding Calculated Values
analysts capable of performing common laboratory procedures
7.1 Calculated values shall be rounded to the desired num-
skillfully and safely. It is expected that the analytical work will
ber of places in accordance with the rounding method in
be performed in a properly equipped laboratory under appro-
Practice E 29.
priate quality control practices such as those described in
Guide E 882.
SILVER, BISMUTH, CADMIUM, COBALT, COPPER,
4. Apparatus, Reagents, and Instrumental Practices IRON, MANGANESE, LEAD, AND ZINC BY THE
FLAME ATOMIC ABSORPTION METHOD
4.1 Apparatus—Special apparatus and reagents required for
each determination are listed in the Apparatus section of each
8. Scope
testmethod.Insomecases,referenceismadetoPracticesE 50.
8.1 This test method applies to the determination of the
4.2 Reagents:
silver, bismuth, cadmium, cobalt, copper, iron, manganese,
4.2.1 Purity of Reagents—Unless otherwise indicated, all
lead, and zinc contents of refined, wrought, and cast nickel
reagents used in these test methods shall conform to the
metal within the following ranges.
specifications of the Committee on Analytical Reagents of the
Concentration Range, %
American Chemical Society. Other chemicals may be used,
Element Method A Method B
provided it is first ascertained that they are of sufficiently high
purity to permit their use without adversely affecting the
Ag 0.0002 to 0.01 .
Bi 0.0010 to 0.01 .
expected performance of the determination, as indicated in
Cd 0.0002 to 0.0025 .
each Precision and Bias section.
Co 0.0010 to 0.01 0.01 to 1.00
4.2.2 Purity of Water—Unless otherwise indicated, refer-
Cu 0.0005 to 0.01 0.01 to 1.00
Fe 0.0025 to 0.01 0.01 to 0.15
ences to water shall be understood to mean reagent water as
Mn 0.0005 to 0.01 0.01 to 0.20
defined by Type II of Specification D 1193.
Pb 0.0006 to 0.01 .
4.2.3 Reagents and their preparation are described in the
Zn 0.0005 to 0.0025 0.001 to 0.015
Reagents section in each test method.
8.2 This test method is applicable to the independent deter-
4.2.4 Instructions for the preparation of standard solutions
mination of any one or more of the elements listed without
used in these test methods frequently call for measuring exact
including all the elements specified in the standard solutions.
weights of substances of known composition so that the
8.3 The lower level for iron can be extended to less than
concentrations of the resulting standard solutions can be
0.0025 % provided nickel metal containing less than 0.0001 %
expressed using simple numbers. Small variations from these
iron is used for preparation of standards (12.8).
specified quantities are acceptable, provided that the true
8.4 The upper limit for the determination of cobalt and
weighed masses are used to calculate the concentration of the
copper can be raised to 2 % by a minor modification to the test
prepared solutions and then these calculated values are used
method. See Note 6.
throughout the test methods.
4.3 Instrumental Practices—Informationontheuseofsome
9. Summary of Test Method
instrumental techniques employed in these test methods are
9.1 The sample is dissolved in dilute nitric acid, excess acid
described in Practice E 60 and in Guide E 1024.
is evaporated, and the solution diluted to a known volume.The
test solution is aspirated into the air/acetylene flame of an
5. Hazards
atomic absorption spectrophotometer. The absorption of the
5.1 For precautions to be observed in the use of certain
resonance line energy from the spectrum of each element is
reagentsandequipmentinthesetestmethods,refertoPractices
measured and compared with that from a set of calibration
E 50.
solutions of the same element in a matched nickel matrix.
5.2 Where appropriate, specific precautionary information
is given in the Hazards sections and in special warning
10. Interferences
paragraphs.
10.1 Elements ordinarily present in nickel metal do not
6. Sampling
presentspectralinterferencesintheatomicabsorptionanalysis.
10.2 For the determination of silver, take care to avoid
6.1 Sampling shall be carried out by a mutually acceptable
contamination of the sample and calibration solutions with
method.
chloride.
6.2 The laboratory sample normally is in the form of a
10.3 Potential background absorption interference is elimi-
powder, granules, millings, or drillings and no further prepa-
nated by use of matched matrix standards prepared from
ration is necessary.
high-purity nickel metal. See Note 7.
6.3 If it is suspected that the laboratory sample is contami-
nated with oil or grease from the milling or drilling process, it
11. Apparatus
may be cleaned by washing with high-purity acetone and
drying in air. 11.1 Atomic Absorption Spectrophotometer:
E 1587 – 94 (1998)
11.1.1 The atomic absorption spectrophotometer used in mum), weighed to the nearest 0.001 g, to a 600-mL beaker.
this test method shall meet the instrument performance param- Proceed as directed in 12.1.2.
eters in accordance with Guide E 1024. 12.11 Working Solutions:
11.1.2 The instrument shall be equipped with a burner head 12.11.1 Mixed Analyte Standard Solution A (1 mL = 20 µg
capable of accepting a solution containing 25 g/L of nickel, as of Silver, Bismuth, Cadmium, Cobalt, Copper, Iron, Manga-
nitrate, and suitable for an air/acetylene flame. nese, and Lead and 10 µg of Zinc)—Using pipets, transfer 20.0
11.1.3 The instrument should be capable of using single- mLof each of the standard stock solutions for Silver, Bismuth,
element hollow cathode or electrodeless discharge lamps Cadmium, Cobalt, Copper, Iron, Manganese, and Lead and 10
operated at currents recommended by the instrument manufac- mL of the standard stock solution for Zinc to a 1-L volumetric
turer. flask containing 160 mL of HNO (1 + 1) (Note 1). Dilute to
volume with water and mix. Store in a glass container.
12. Reagents
12.11.2 Mixed Analyte Standard Solution B (1mL = 100µg
of Cobalt, Copper, Iron, and Manganese and 10 µg of Zinc)—
12.1 Bismuth, Standard Stock Solution (1 mL = 1 mg Bis-
Using pipets, transfer 50.0 mLof the Cobalt, Copper, Iron, and
muth):
Manganese standard stock solutions and 5.0 mL of the Zinc
12.1.1 Transfer a 1.00-g sample of bismuth metal (purity,
standard stock solution to a 500-mLvolumetric flask. Dilute to
99.9 %minimum),weighedtothenearest0.001g,toa600-mL
volume and mix. Store in a polyethylene bottle.
beaker.
12.1.2 Add40mLofHNO (1 + 1)(Note1)andheatgently
13. Calibration Solutions
until dissolution is complete. Boil gently to expel oxides of
13.1 Set A:
nitrogenandcool.Transfertoa1-Lvolumetricflaskcontaining
13.1.1 This set corresponds to 0, 0.2, 0.5, 1.0, 1.5, 2.0, and
160mLofHNO (1 + 1),dilutetovolumewithwater,andmix.
2.5µg/mLeachofsilver,bismuth,cadium,cobalt,copper,iron,
Store in a polyethylene bottle.
manganese, and lead and 0, 0.1, 0.25, 0.5, 0.75, 1.0, and 1.25
NOTE 1—Use the same batch of nitric acid throughout the entire
µg/L of Zinc.
procedure. Also see Note 4.
Analyte Concentration µg/mL
12.2 Cadmium, Standard Stock Solution (1 mL = 1 mg
Silver, Bismuth, Cadium, Co-
Cadmium)—Transfer a 1.00-g sample of cadmium metal
Aliquot of balt, Copper, Iron, Manga-
(purity, 99.9 % mininum), weighed to the nearest 0.001 g, to a No. Solution A, mL nese and Lead Zinc
10 0 0
600-mL beaker. Proceed as directed in 12.1.2.
2 2.0 0.2 0.1
12.3 Cobalt, Standard Stock Solution (1 mL = 1 mg
3 5.0 0.5 0.25
Cobalt)—Transfer a 1.00-g sample of cobalt metal (purity, 4 10.0 1.0 0.5
5 15.0 1.5 0.75
99.9 %minimum),weighedtothenearest0.001g,toa600-mL
6 20.0 2.0 1.0
beaker. Proceed as directed in 12.1.2.
7 25.0 2.5 1.25
12.4 Copper, Standard Stock Solution (1 mL = 1 mg
13.1.2 Weigh, to the nearest 0.01 g, seven separate 5.0-g
Copper)—Transfer a 1.00-g sample of copper metal (purity,
portions of high-purity nickel powder and transfer to 600-mL
99.9 %minimum),weighedtothenearest0.001g,toa600-mL
beakers. Treat as directed in 14.2
beaker. Proceed as directed in 12.1.2.
13.1.3 Add,usingaburetgraduatedin0.05-mLdivisions,0,
12.5 Iron, Standard Stock Solution (1 mL = 1 mg Iron)—
2.0, 5.0, 10.0, 15.0, 20.0, and 25.0 mL respectively of the
Transfer a 1.00-g sample of iron metal (purity, 99.9 % mini-
mixed Analyte Standard Solution A to the 200-mL volumetric
mum), weighed to the nearest 0.001 g, to a 600-mL beaker.
flasks. Dilute to volume with water and mix.
Proceed as directed in 12.1.2.
12.6 Lead, Standard Stock Solution (1 mg = 1 mg Lead)— NOTE 2—The solution with zero addition is the reagent blank. See 14.3
and Note 5.
Transfer a 1.00-g sample of lead metal (purity, 99.9 % mini-
mum), weighed to the nearest 0.001 g, to a 600-mL beaker.
13.2 Set B:
Proceed as directed in 12.1.2.
13.2.1 This set corresponds to 0, 2.5, 5.0, 10.0, 15.0, 20.0,
12.7 Manganese, Standard Stock Solution (1 mL = 1 mg
and 25.0 µg/mLof cobalt, copper, iron, and manganese, and 0,
Manganese)—Transfer a 1.00-g sample of manganese metal
0.25, 0.5, 1.0, 1.5, 2.0, and 2.5 µg/mL of Zinc.
(purity, 99.9 % minimum), weighed to the nearest 0.001 g, to
Analyte Concentration µg/mL
a 600-mL beaker. Proceed as directed in 12.1.2. Aliquot of Mixed Ana-
lyte Standard Colbalt, Copper, Iron,
12.8 Nickel Powder—High-purity, containing less than
No. Solution B, mL and Manganese Zinc
0.0005 % Iron and less than 0.0001 % each of silver, bismuth,
10 0 0
2 5.0 2.5 0.25
cadmium, cobalt, copper, manganese, lead, and zinc.
3 10.0 5.0 0.5
12.9 Silver, Standard Stock Solution(1mL = 1mgSilver)—
4 20.0 10.0 1.0
Transfer a 1.00-g sample of silver metal (purity, 99.9 %
5 30.0 15.0 1.5
6 40.0 20.0 2.0
minimum), weighed to the nearest 0.001-g, to a 600-mL
7 50.0 25.0 2.5
beaker. Proceed as directed in 12.1.2, except store in a glass
bottle. 13.2.2 Weigh, to the nearest 0.005 g, seven separate 2.00-g
12.10 Zinc, Standard Stock Solution (1 mL = 1 mg Zinc)— portions of high-purity nickel powder and transfer to 400-
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