ASTM E76-88(1998)
(Test Method)Standard Test Methods for Chemical Analysis of Nickel-Copper Alloys (Withdrawn 2003)
Standard Test Methods for Chemical Analysis of Nickel-Copper Alloys (Withdrawn 2003)
SCOPE
1.1 These test methods cover procedures for the chemical analysis of nickel-copper alloys having chemical compositions within the following limits: Element Concentration Range, % Nickel 40 to 90 Cobalt 0.01 to 1.0 Copper 10 to 50 Iron 0.1 to 5.0 Manganese 0.1 to 2.5 Carbon 0.01 to 1.0 Silicon 0.01 to 5.0 Sulfur 0.001 to 0.1 Aluminum 0.01 to 4.0
1.2 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: Perchloric Acid-Electrolytic Test Method 9 to 13 Sulfuric Acid-Electrolytic Test Method 14 to 18 Nickel: Dimethylglyoxime-Gravimetric Test Method 19 to 22 Dimethylglyoxime-Electrolytic Test Method 23 to 26 Cobalt: Alpha-Nitroso-beta-Naphthol Test Method 27 to 29 Nitroso-R-Salt-Photometric Test Method 30 to 37 Iron: Stannous-Chloride-Potassium Dichromate Test Method 38 to 40 Thiocyanate-Photometric Test Method 41 to 48 Manganese: Persulfate-Arsenite Test Method 49 to 52 Periodate-Photometric Test Method 53 to 60 Carbon, Total, by the Direct Combustion Test Method 61 to 63 Silicon: Perchloric Acid Test Method 64 to 66 Sulfuric Acid Test Method 67 to 68 Sulfur: Gravimetric Test Method 69 to 71 Direct Combustion-Iodate Test Method 72 to 75 Aluminum by the Mercury Cathode-Cupferron-8-Hydroxyquinoline Test Method 76 to 81
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 to determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 5.
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Standards Content (Sample)
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Designation: E 76 – 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 Nickel-Copper Alloys
This standard is issued under the fixed designation E 76; 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
Sections
Sulfuric Acid Test Method 67 to 68
1.1 These test methods cover procedures for the chemical
Sulfur:
analysis of nickel-copper alloys having chemical compositions
Gravimetric Test Method 69 to 71
Direct Combustion-Iodate Test Method 72 to 75
within the following limits:
Aluminum by the Mercury Cathode-Cupferron-8- Hydroxyquinoline
Element Concentration Range, %
Test Method 76 to 81
Nickel 40 to 90
Cobalt 0.01 to 1.0
1.3 This standard does not purport to address all of the
Copper 10 to 50
safety problems, if any, associated with its use. It is the
Iron 0.1 to 5.0
responsibility of the user of this standard to establish appro-
Manganese 0.1 to 2.5
Carbon 0.01 to 1.0
priate safety and health practices and to determine the
Silicon 0.01 to 5.0
applicability of regulatory limitations prior to use. Specific
Sulfur 0.001 to 0.1
precautionary statements are given in Section 5.
Aluminum 0.01 to 4.0
1.2 The analytical procedures appear in the following order:
2. Referenced Documents
(This standard contains more than one test method for some
2.1 ASTM Standards:
elements. In some cases, the use of multiple test methods is
E 29 Practice for Using Significant Digits in Test Data to
needed to cover the concentration range of the scope of the
Determine Conformance With Specifications
standard; in others, multiple test methods are supplied to allow
E 50 Practices for Apparatus, Reagents, and Safety Precau-
for variations in availability of instruments and other facilities
tions for Chemical Analysis of Metals
among laboratories.)
E 55 Practice for Sampling Wrought Nonferrous Metals and
Sections
Alloys for Determination of Chemical Composition
Copper:
E 60 Practice for Photometric and Spectrophotometric
Perchloric Acid-Electrolytic Test Method 9 to 13
Sulfuric Acid-Electrolytic Test Method 14 to 18
Methods for Chemical Analysis of Metals
Nickel:
E 88 Practice for Sampling Nonferrous Metals and Alloys
Dimethylglyoxime-Gravimetric Test Method 19 to 22
in Cast Form for Determination of Chemical Composition
Dimethylglyoxime-Electrolytic Test Method 23 to 26
Cobalt:
Alpha-Nitroso-beta-Naphthol Test Method 27 to 29
3. Significance and Use
Nitroso-R-Salt-Photometric Test Method 30 to 37
3.1 These test methods for the chemical analysis of metals
Iron:
Stannous Chloride-Potassium Dichromate Test Method 38 to 40
and alloys are primarily intended to test such materials for
Thiocyanate-Photometric Test Method 41 to 48
compliance with compositional specifications. It is assumed
Manganese:
that all who use these test methods will be trained analysts
Persulfate-Arsenite Test Method 49 to 52
Periodate-Photometric Test Method 53 to 60
capable of performing common laboratory procedures skill-
Carbon, Total, by the Direct Combustion Test Method 61 to 63
fully and safely. It is expected that work will be performed in
Silicon:
a properly equipped laboratory.
Perchloric Acid Test Method 64 to 66
4. Apparatus and Reagents
4.1 Apparatus and reagents required for each determination
These test methods are under the jurisdiction of ASTM Committee E-1 on
are listed in separate sections preceding the procedure. The
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
apparatus, standard solutions, and certain other reagents used
responsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.
in more than one procedure are referred to by number and shall
Current edition approved Dec. 30, 1988. Published February 1989. Originally
published as E 76 – 50 T. Last previous edition E 76 – 83.
conform to the requirements prescribed in Practices E 50,
For procedures for the chemical analysis of copper-nickel alloys containing
50 % and over of copper, see ASTM Test Methods E 75, for Chemical Analysis of
Copper-Nickel and Copper-Nickel-Zinc Alloys, Annual Book of ASTM Standards, Annual Book of ASTM Standards, Vol 14.02.
Vol 03.05. 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.
E76
except that photometers shall conform to the requirements 11.5 Calculation—Calculate the percentage of copper as
prescribed in Practice E 60. follows:
Copper, % 5 ~A/B! 3 100 (1)
5. Hazards
where:
5.1 For precautions to be observed in these test methods,
A 5 copper deposited, g, and
reference shall be made to Practices E 50.
B 5 sample used, g.
11.6 Reserved Electrolyte—If there is any brown deposit on
6. Photometric Practice
the anode, place it in the reserved electrolyte and stir until the
6.1 Photometric practice prescribed in these test methods
deposit dissolves. If necessary, add 1 or 2 drops of H SO to
2 3
shall conform to Practice E 60.
aid in dissolution of the deposit. Transfer the solution to a
250-mL volumetric flask, dilute to the mark, and mix thor-
7. Sampling
oughly. Reserve for determinations of nickel, cobalt, iron, and
7.1 Wrought products shall be sampled in accordance with
manganese as described in Sections 21 and 25, 36, 47, and 59,
Practice E 55. Cast products shall be sampled in accordance
respectively.
with Practice E 88.
12. Procedure for Alloys Containing 2 % and Over of
8. Rounding Calculated Values
Silicon
8.1 Calculated values shall be rounded to the desired num-
12.1 Transfer 1.0000 g of the sample to a 400-mL beaker.
ber of places in accordance with the rounding method given in
Add 20 mL of HClO - HNO mixture. Cover and heat gently
4 3
the Rounding-Off Procedure paragraphs of Practice E 29.
until action ceases. Rinse and remove the cover. Add HF
dropwise, while swirling the solution, until the dark residue
COPPER BY THE PERCHLORIC ACID-
dissolves and the solution is clear green. Evaporate slowly to
ELECTROLYTIC TEST METHOD
copious white fumes, heating carefully in order to avoid losses
by spraying. Heat to incipient boiling; then cover the beaker.
9. Apparatus
Proceed as described in 11.2-11.6.
9.1 Electrodes for Electroanalysis—Apparatus No. 9.
13. Precision and Bias
10. Reagents
13.1 This test method was originally approved for publica-
10.1 Nitric Acid (nitrous acid-free)—Boil a suitable amount
tion before the inclusion of precision and bias statements
of HNO until it is colorless. Cool in running water. Prepare as
within standards was mandated. The original interlaboratory
required, just before use, taking care not to expose the product
test data for this test method are no longer available. The user
to direct sunlight.
is cautioned to verify, by the use of reference materials, if
10.2 Perchloric-Nitric Acid Mixture—To 200 mL of water,
available, that the precision and bias of this test method are
add 200 mL of HNO and 600 mL of HClO .
3 4
adequate for the contemplated use.
11. Procedure for Alloys Containing Under 2 % Silicon
COPPER BY THE SULFURIC ACID-
11.1 Transfer 1.0000 g of the sample to a 250-mL beaker.
ELECTROLYTIC TEST METHOD
Add 20 mL of HClO - HNO mixture. Cover and heat gently
4 3
until action ceases. Insert a glass hook between the cover and 14. Apparatus
beaker, and evaporate to copious white fumes. Heat to incipient
14.1 Electrodes for Electroanalysis—Apparatus No. 9.
boiling and remove the glass hook.
11.2 Boil gently for 10 min at such a rate that most of the 15. Procedure for Alloys Containing Under 0.50 %
HClO is retained. Allow to cool somewhat, add 100 mL of Silicon
warm water, and stir until the perchlorates dissolve.
15.1 Transfer 1.0000 g of the sample to a 300-mL, tall-form
11.3 Filter through a medium paper into a 300-mL tall-form
beaker. Add 15 mL of HNO (1+1). Cover and heat gently until
beaker. Wash the residue with hot water (Note 1). Add 3 mL of
brown fumes have been expelled. Boil gently for 5 min. Add
HNO (HNO -free) to the filtrate.
3 2
100 mL of water and 10 mL of H SO (1+1). Proceed as
2 4
described in 11.4-11.6.
NOTE 1—If the silicon content of the alloy is over 0.5 %, it may be
determined in this residue as described in 65.4-65.8, except that if HF has
16. Procedure for Alloys Containing Under 2 % Silicon
been used in the preliminary treatment any residue present at this stage
should be discarded.
16.1 Transfer 1.0000 g of the sample to a 400-mL beaker.
11.4 Electrolysis—Dilute the solution to 150 mL. Electro- Add 20 mL of HNO (1+1), cover, and heat gently until action
lyze overnight, using platinum gauze electrodes and a current ceases. Add 15 mL of H SO (1+1), insert a glass hook between
2 4
density of 0.5 A/dm . Remove the electrodes and wash them the cover and beaker, and evaporate slowly to dense white
with water, taking the usual precautions against loss. Reserve fumes. Continue heating for 10 min; then let stand until cool.
the electrolyte and washings. Dip the cathode in two successive 16.2 Add 100 mL of water and heat until the sulfates
baths of methanol or ethanol, and dry in an oven at 110°C for dissolve, stirring occasionally to prevent bumping. Proceed as
3 to 5 min. Cool, and weigh the deposit as metallic copper. described in 11.3-11.6.
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.
E76
17. Procedure for Alloys Containing 2 % and Over of nickel was completely precipitated.
Silicon 21.4 Dry the precipitate at 150°C to constant weight. Cool
in a desiccator and weigh as nickel dimethylglyoxime.
17.1 Transfer 1.0000 g of the sample to a 400-mL beaker.
21.5 Calculation—Calculate the percentage of nickel as
Add 20 mL of HNO (1+1). Cover and heat gently until action
follows:
ceases. Rinse and remove the cover. Add HF drop by drop,
while swirling the solution, until the dark residue dissolves and Nickel, % 5 @~A 3 0.2032!/B# 3 100 (2)
the solution is clear green. Add 15 mL of H SO (1+1).
2 4
where:
Evaporate slowly to dense white fumes, heating carefully in
A 5 nickel dimethylglyoxime, g, and
order to avoid losses by spraying. Continue heating for 10 min;
B 5 sample used, g.
then let stand until cool.
17.2 Add 100 mL of water and heat until the sulfates
22. Precision and Bias
dissolve, stirring occasionally to prevent bumping. Proceed as
22.1 This test method was originally approved for publica-
described in 11.3-11.6.
tion before the inclusion of precision and bias statements
within standards was mandated. The original interlaboratory
18. Precision and Bias
test data for this test method are no longer available. The user
18.1 This test method was originally approved for publica-
is cautioned to verify, by the use of reference materials, if
tion before the inclusion of precision and bias statements
available, that the precision and bias of this test method are
within standards was mandated. The original interlaboratory
adequate for the contemplated use.
test data for this test method are no longer available. The user
is cautioned to verify, by the use of reference materials, if
NICKEL BY THE DIMETHYLGLYOXIME-
available, that the precision and bias of this test method are
ELECTROLYTIC TEST METHOD
adequate for the contemplated use.
23. Apparatus
NICKEL BY THE DIMETHYLGLYOXIME-
23.1 Electrodes for Electroanalysis—Apparatus No. 9.
GRAVIMETRIC TEST METHOD
24. Reagents
19. Apparatus
24.1 Ethanol Solution of Dimethylglyoxime (40 g/L)—
19.1 Filter Crucible—Apparatus No. 2. A 30 or 50-mL,
Reagent No. 105.
medium-porosity glass filtering crucible shall be prepared each
24.2 Tartaric Acid Solution (250 g/L)—Reagent No. 116.
time before use as follows: Remove the bulk of the precipitate
25. Procedure
from the previous analysis mechanically. Immerse the crucible
in HCl and heat for 1 h. With the aid of suction, wash with
25.1 Transfer 150.0 mL of the electrolyte from the copper
water, then NH OH, and finally with water. Dry at 150°C, cool
determination to a 600-mL beaker, or, alternatively, treat
in a desiccator, and weigh.
0.6000 g of the sample as described in Sections 11, 12, 15, 16,
or 17, and transfer the electrolyte to a 600-mL beaker.
20. Reagents
25.2 Dilute to 350 mL. Add 1 mL of HNO and heat to
20.1 Ethanol Solution of Dimethylglyoxime (10 g/L)—
boiling. Allow to cool somewhat, and add 10 mL of tartaric
Reagent No. 104.
acid solution. Neutralize with NH OH and add 1 mL in excess.
20.2 Tartaric Acid Solution (250 g/L)—Reagent No. 116.
Heat to 60 to 70°C.
25.3 Add 0.1 mL of hot dimethylglyoxime solution (40 g/L)
21. Procedure
for each milligram of nickel present, and add 5 to 10 mL in
21.1 Transfer 50.0 mL of the reserved electrolyte from the
excess. Stir the mixture vigorously and allow to cool to room
copper determination (11.6) to a 600-mL beaker, or, alterna-
temperature, stirring occasionally. Filter, using a 15-cm me-
tively, treat 0.2000 g of the sample as described in Sections 11,
dium paper, and wash with cool water.
12, 15, 16, or 17, and transfer the electrolyte to a 600-mL
25.4 Add 1 or 2 mL of dimethylglyoxime solution (40 g/L)
beaker. Add 1 mL of HNO and heat to boiling. Add 300 mL
to the filtrate and let stand overnight in order to make certain
of water and 10 mL of tartaric acid solution. Neutralize with
that the nickel was completely precipitated.
NH OH and add 1 mL in excess. Heat to 60 to 70°C.
25.5 Transfer the paper and precipitate to the precipitation
21.2 Add 0.4 mL of dimethylglyoxime solution (10 g/L) for
beaker. Add 40 mL of HNO and 15 mL of HClO . Cover the
3 4
each milligram of nickel present, and add 5 to 10 mL in excess.
beaker and heat until the paper disintegrates. Insert three glass
Stir the mixture vigorously and allow to cool to room tempera-
hooks between the cover and beaker, and evaporate to dryness,
ture, stirring occasionally. Filter, using a fritted-glass crucible
guarding against loss from spraying. Heat the residue at 250°C
of medium porosity prepared as described in Section 19. Wash
until HClO has been driven off completely. Let stand until
with cool water.
cool.
21.3 Add 5 mL of dimethylglyoxime solution (10 g/L) to the
25.6 Add 40 mL of H SO (1+3) and heat until the nickel
2 4
filtrate and let stand ove
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