ASTM E107-88(1998)
(Test Method)Standard Test Methods for Chemical Analysis of Electronic Nickel (Withdrawn 2003)
Standard Test Methods for Chemical Analysis of Electronic Nickel (Withdrawn 2003)
SCOPE
1.1 These test methods cover photometric procedures for the chemical analysis of nickel, intended primarily for use in electronic devices, having a chemical composition within the following limits: Element Concentration Range, % Nickel 94 to 100 Copper 0.005 to 0.3 Iron 0.0035 to 0.3 Cobalt 0.05 to 1.0 Manganese 0.02 to 0.5 Titanium 0.0005 to 0.5 Silicon 0.001 to 0.3 Aluminum 0.01 to 0.35 Carbon 0.001 to 0.10 Hydrogen 0.0001 to 0.01 Nitrogen 0.0001 to 0.01 Oxygen 0.001 to 0.10 Tungsten 3.0 to 5.0 Magnesium 0.005 to 0.2
1.2 The techniques and procedures covered in these test methods have been chosen so as to keep the consumption of sample to a minimum.
1.3 The analytical procedures appear in the following order: (This standard contains more than one test method for some elements. In some cases, the use of multiple test methods is needed to cover the concentration range of the scope of the standard; in others, multiple test methods are supplied to allow for variations in availability of instruments and other facilities among laboratories.) Sections Copper by the Hydrobromic Acid (Photometric) Method 8 to 15 Iron by the Thiocyanate (Photometric) Method 16 to 24 Cobalt by the Nitroso-R-Salt (Photometric) Method 25 to 32 Manganese by the Periodate (Photometric) Method 33 to 40 Titanium by the Tiron (Photometric) Method 41 to 48 Silicon by the Molybdenum Blue (Photometric) Method 49 to 56 Aluminum by the Aluminon (Photometric) Method 57 to 64 Carbon by the Low-Pressure Combustion Method 65 to 73 Hydrogen, Nitrogen, and Oxygen by the Vacuum Fusion Method 74 to 78 Copper by the Neocuproine (Photometric) Method 79 to 87 Tungsten by the Acid Digestion-Cinchonine (Gravimetric) Method 88 to 92 Magnesium by the 8-Hydroxyquinoline (Photometric) Method 93 to 102
1.4 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. Specific hazard statements are given in Section 5.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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Designation: E 107 – 88 (Reapproved 1998)
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 Methods for
Chemical Analysis of Electronic Nickel
This standard is issued under the fixed designation E 107; 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
Magnesium by the 8-Hydroxyquinoline (Photometric)
Method 93 to 102
1.1 These test methods cover photometric procedures for
1.4 This standard does not purport to address all of the
the chemical analysis of nickel, intended primarily for use in
safety concerns, if any, associated with its use. It is the
electronic devices, having a chemical composition within the
responsibility of the user of this standard to establish appro-
following limits:
priate safety and health practices and determine the applica-
Element Concentration Range, %
Nickel 94 to 100
bility of regulatory limitations prior to use. Specific hazard
Copper 0.005 to 0.3
statements are given in Section 5.
Iron 0.0035 to 0.3
Cobalt 0.05 to 1.0
2. Referenced Documents
Manganese 0.02 to 0.5
Titanium 0.0005 to 0.5
2.1 ASTM Standards:
Silicon 0.001 to 0.3
E 29 Practice for Using Significant Digits in Test Data to
Aluminum 0.01 to 0.35
Carbon 0.001 to 0.10
Determine Conformance With Specifications
Hydrogen 0.0001 to 0.01 3
E 39 Methods for Chemical Analysis of Nickel
Nitrogen 0.0001 to 0.01
E 50 Practices for Apparatus, Reagents, and Safety Precau-
Oxygen 0.001 to 0.10
Tungsten 3.0 to 5.0
tions for Chemical Analysis of Metals
Magnesium 0.005 to 0.2
E 55 Practice for Sampling Wrought Nonferrous Metals and
1.2 The techniques and procedures covered in these test Alloys for Determination of Chemical Composition
methods have been chosen so as to keep the consumption of E 60 Practice for Photometric and Spectrophotometric
sample to a minimum. Methods for Chemical Analysis of Metals
1.3 The analytical procedures appear in the following order:
3. Significance and Use
(This standard contains more than one test method for some
3.1 These test methods for the chemical analysis of metals
elements. In some cases, the use of multiple test methods is
and alloys are primarily intended to test such materials for
needed to cover the concentration range of the scope of the
standard; in others, multiple test methods are supplied to allow compliance with compositional specifications. It is assumed
that all who use these test methods will be trained analysts
for variations in availability of instruments and other facilities
among laboratories.) capable of performing common laboratory procedures skill-
fully and safely. It is expected that work will be performed in
Sections
Copper by the Hydrobromic Acid (Photometric) Method 8 to 15
a properly equipped laboratory.
Iron by the Thiocyanate (Photometric) Method 16 to 24
Cobalt by the Nitroso-R-Salt (Photometric) Method 25 to 32
4. Photometric Practice, Apparatus, and Reagents
Manganese by the Periodate (Photometric) Method 33 to 40
Titanium by the Tiron (Photometric) Method 41 to 48
4.1 Photometers and Photometric Practice—Photometers
Silicon by the Molybdenum Blue (Photometric) Method 49 to 56
and photometric practice prescribed in these test methods shall
Aluminum by the Aluminon (Photometric) Method 57 to 64
conform to Practice E 60.
Carbon by the Low-Pressure Combustion Method 65 to 73
Hydrogen, Nitrogen, and Oxygen by the Vacuum Fusion
4.2 Apparatus other than photometers, standard solutions,
Method 74 to 78
and certain other reagents used in more than one procedure are
Copper by the Neocuproine (Photometric) Method 79 to 87
referred to by number and shall conform to the requirements
Tungsten by the Acid Digestion-Cinchonine (Gravimetric)
Method 88 to 92
prescribed in Practices E 50.
5. Hazards
5.1 For precautions to be observed in the use of certain
These test methods are under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
reagents in these test methods, reference shall be made to
responsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.
Practices E 50.
Current edition approved Dec. 30, 1988. Published February 1989. Originally
published as E 107 – 54 T. Last previous edition E 107 – 83.
These test methods were developed in cooperation with ASTM Committee F-1 Annual Book of ASTM Standards, Vol 14.02.
on Electronics. Annual Book of ASTM Standards, Vol 03.05.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 107
6. Sampling 13. Preparation of Calibration Curve
6.1 The sample shall be selected so as to be representative 13.1 Calibration Solutions:
of the material to be analyzed. 13.1.1 Transfer 0.5, 1.0, 2.0, 3.0, 4.0, 6.0, and 8.0 mL of
6.2 For the determination of carbon, hydrogen, nitrogen, copper solution (1 mL 5 0.1 mg Cu) to 125-mL conical flasks.
and oxygen, wrought products shall be sampled in accordance Add 3 mL of HClO and dilute to 40 mL.
with Practice E 55, with the exception that for the determina- 13.1.2 Add1gof test lead, cover, and boil at a moderate
tion of hydrogen, nitrogen, and oxygen solid pieces are rate for 15 min to displace all the copper. Cool somewhat,
preferred to millings or drillings, if representative, so as to remove the solution by decantation, and wash once with water,
minimize the effect of surface area. decanting thoroughly. Heat the flask gently to remove mois-
ture.
7. Rounding Calculated Values
13.1.3 Add 10 mL of HBr − Br mixture to the flask, cover,
7.1 Calculated values shall be rounded to the desired num-
and heat gently to dissolve the metal. Boil to expel the excess
ber of places in accordance with the rounding method given in
bromine. Cool to room temperature. Transfer 10 mL of H PO
3 4
Section 3.4 and 3.5 of Practice E 29.
and 1 drop (0.05 mL) of HBr − Br mixture to a dry 25-mL
volumetric flask (Note 2). Transfer the sample solution to a
COPPER BY THE HYDROBROMIC ACID
volumetric flask, washing with a few millilitres of HBr. Dilute
(PHOTOMETRIC) TEST METHOD
to the mark with HBr and mix.
8. Summary of Test Method
NOTE 2—Partial reduction of the copper to the cuprous state may occur
8.1 Cupric copper in a mixture of HBr and H PO forms a
when a bromine-free HBr solution of cupric copper is boiled. For this
3 4
reason, it is necessary to add a small amount of bromine to oxidize any
red-violet colored complex. Photometric measurement is made
cuprous copper before photometric measurement is made. Bromine in
at approximately 600 nm.
small amounts does not absorb appreciably at 600 nm.
NOTE 1—By calibrating the system using a light band centered at
13.2 Reference Solution—Transfer 40 mL of water and 3
approximately 600 nm, this test method can be used to determine higher
mL of HClO to a 125-mL flask and proceed as directed in
concentrations of copper, if necessary. Under these conditions, the range 4
13.1.2 and 13.1.3.
is from 0.15 to 3.0 mg of copper in 25 mL of solution, using a cell depth
of 2 cm.
13.3 Photometry—Transfer a suitable portion of the refer-
ence solution to an absorption cell and adjust the photometer to
9. Concentration Range
the initial setting, using a light band centered at approximately
9.1 The recommended concentration range is from 0.05 to
600 nm. While maintaining this photometer adjustment, take
0.8 mg of copper per 25 mL of solution, using a cell depth of
the photometric readings of the calibration solutions.
2 cm.
13.4 Calibration Curve—Plot the photometric readings of
the calibration solutions against milligrams of copper per 25
10. Stability of Color
mL of solution.
10.1 The color develops immediately and is stable for
14. Procedure
several days.
14.1 Sample Solution:
11. Interfering Elements
14.1.1 Transfer 1.000 g of the sample to a 125-mL conical
11.1 Gold and the platinum group metals interfere if
flask and add 10 mL of HNO (1 + 1). Cover and warm gently
present. Provision is made in this test method to eliminate other
to dissolve the sample.
interfering elements that might be present in nickel.
14.1.2 When dissolution is as complete as possible, add 6
mL of HClO and heat while swirling over an open flame until
12. Reagents
the volume of the solution has been reduced to about 3 mL
12.1 Copper, Standard Solution (1 mL 5 0.1 mg Cu)—
(Note 3). Cool, add 10 mL of water plus 2 drops of H O (3 %),
2 3
Dissolve 0.1000 g of high-purity copper (99.9 % Cu and over)
and heat to boiling (Note 4). Dilute to 40 mL with water. If
in3mLofHNO by heating gently in a 125-mL conical flask.
necessary, filter through a fine paper into a 150-mL flask or
Add 10 mL of HClO and heat to copious fumes to expel
beaker (Note 5). Wash once or twice with water and discard the
HNO . Cool and add 10 mL of water. Transfer to a 1-L
paper and precipitate.
volumetric flask, dilute to the mark, and mix.
NOTE 3—It is essential that the fuming operation completely remove
12.2 Hydrobromic Acid - Bromine Mixture—Add 1 volume
the HNO , yet care should be used to avoid evaporation of too much
of bromine to 16 volumes of HBr and mix.
HClO , lest an insoluble nickel oxide be formed.
12.3 Hydrogen Peroxide (3 %)—Dilute 1 mL of H O
2 2
NOTE 4—The H O is added to destroy any MnO or HMnO that
2 2 2 4
(30 %) to 10 mL with water. Prepare fresh before use.
might be present.
12.4 Test Lead—Finely granulated test lead containing less
NOTE 5—If more than a small amount of tungsten is present, as
than 0.0001 % of copper and less than 0.001 % of iron or
indicated by a colored precipitate at this point, the subsequent method for
nickel. the determination of iron should not be used, as the precipitate tends to
hold iron. No apparent difficulties are encountered in the determination of
copper, cobalt, or manganese.
These procedures have been written for a cell having a 2-cm light path. Cells
14.1.3 Add1gof test lead to the flask or beaker. Cover and
having other dimensions may be used, provided suitable adjustments can be made
in the amount of sample and reagents used. boil gently for 15 min to collect the copper on the lead. Decant
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 107
the filtrate. Quickly wash the container and test lead twice by 20.2 Hydrogen Peroxide Solution (1.5 %)—Dilute 1 mL of
decantation with water. Cool the decanted solution and wash H O (30 %) to 20 mL with water. Prepare fresh before use.
2 2
water to room temperature, transfer to a 100-mL volumetric 20.3 Iron, Standard Solution (1 mL 5 0.025 mg Fe)—
flask, dilute to the mark, and mix. Reserve this solution for the Dissolve 0.1756 g of Fe(NH ) (SO ) 6HOin10mL of
4 2 4 2 2
determination of cobalt, iron, and manganese (see Note 5). HNO (1 + 1). Heat to gentle boiling to expel brown fumes.
14.1.4 Add 10 mL of HBr − Br mixture to the lead remain- Cool, dilute to 1 L in a volumetric flask, and mix.
ing in the flask or beaker, cover, and heat gently to dissolve. 20.4 Nickel Nitrate, Ni(NO ) ·6H O.
3 2 2
Proceed as directed in 13.1.3.
21. Preparation of Calibration Curve A
14.2 Reference Solution—Carry a reagent blank through the
21.1 Calibration Solutions:
entire procedure, using the same amount of all reagents, for use
21.1.1 Transfer 5.0 g of Ni(NO ) ·6H O to each of two
as a reference solution.
3 2 2
125-mL conical flasks. Add 3 mL of water and warm to
14.3 Photometry—Take the photometric reading of the
dissolve most of the sample. Add 6 mL of HClO and heat over
sample solution as described in 13.3.
an open flame until the volume of the solution has been
14.4 Calculation—Convert the photometric reading of the
reduced to 3 mL. Add 10 mL of water and heat to boiling.
sample solution to milligrams of copper by means of the
Combine the two solutions, transfer to a 200-mL volumetric
calibration curve. Calculate the percentage of copper as fol-
flask, dilute to the mark, and mix.
lows:
21.1.2 Transfer 5.0-mL portions of the nickel solution to
Copper, % 5 A/~B 3 10! (1)
seven 50-mL beakers, and add 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, and
6.0 mL of iron solution (1 mL 5 0.025 mg Fe).
where:
A 5 copper found, g, and 21.1.3 Add 5 mL of HNO (1 + 3) to each beaker and boil
B 5 sample used, g.
for 1 min to expel brown fumes. Cool, transfer to 50-mL
volumetric flasks, and dilute to approximately 35 mL. Add 1
15. Precision and Bias
mL of H O solution and then add 10 mL of NH CNS solution.
2 2 4
15.1 This test method was originally approved for publica-
Dilute to the mark and mix.
tion before the inclusion of precision and bias statements 21.2 Reference Solution—Transfer a 5-mL aliquot of the
within standards was mandated. The original interlaboratory
nickel solution (21.1.1) to a 50-mL beaker and proceed as
test data for this test method are no longer available. The user directed in 21.1.3.
is cautioned to verify by the use of reference materials, if 21.3 Photometry—Transfer a suitable portion of the refer-
available, that the precision and bias of this test method are ence solution to an absorption cell and adjust the photometer to
adequate for the contemplated use. the initial setting, using a light band centered at approximately
470 nm. While maintaining this photometer adjustment, take
IRON BY THE THIOCYANATE (PHOTOMETRIC)
the photometric readings of the calibration solutions.
TEST METHOD
21.4 Calibration Curve—Plot the photometric readings of
the calibration solutions against milligrams of iron per 50 mL
16. Summary of Test Method
of solution.
16.1 Ferric iron forms a red-brown soluble complex with
22. Preparation of Calibration Curve B
thiocyanate in acid solution. Photometric measurement is made
at approximately 470 nm.
22.1 Repeat the preparation of a calibration curve, as
directed in 21.1.2 to 21.4, except to use 20-mL portions of a
17. Concentration Range
nickel solution prepared as directed in 21.1.1.
17.1 The recommended concentration range is from 0.007
NOTE 6—The presence of varying amounts of nickel affects the ferric
to 0.14 mg of iron in 50 mL of solution, using a cell depth of
thiocyanate color, and necessitates the preparation of two calibration
2 cm.
curves to cover the analytical range indicated in 1.1.
18. Stability of Color
23. Procedure
18.1 The color develops immediately and is rea
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