ASTM E75-76(2004)
(Test Method)Standard Test Methods for Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc Alloys (Withdrawn 2010)
Standard Test Methods for Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc Alloys (Withdrawn 2010)
SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of copper-nickel and copper-nickel-zinc alloys having chemical compositions within the following limits:ElementConcentration Range,%Copper40 and overNickel10 to 50Zinc0 to 40Lead0 to 15Tin0 to 10Iron0.00 to 2Manganese0.00 to 2Cobalt0.00 to 0.5 Includes cobalt.
In the case of copper-base alloys containing 5 % and over of zinc, the zinc is usually calculated by difference.
Whenever possible the technique and procedures for analysis should be checked against a National Institute of Standards and Technology standard sample having a composition comparable to the material being analyzed.
1.2 The test methods appear in the following order:SectionsCobalt:Alpha-Nitroso-Beta-Naphthol Method26 to 28Nitroso-R-Salt (Photometric) Method29 to 37Copper, or Copper and Lead Simultaneously, by the Electrolytic Method2aIron:Dichromate Method38 to 40Thiocyanate (Photometric)Method2aSalicylate (Photometric)Method2aLead:Electrolytic Method12 to 15Sulfate Method2 bManganese:Persulfate Method2 bPeriodate (Photometric)Method 59 to 66Nickel by the Dimethylglyoxime Method2aTin by the Iodimetric Titration Method2bZinc by the Oxide or Ferrocyanide Method 2a
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 precautions to be observed in these test methods, refer to Practices E 50.
WITHDRAWN RATIONALE
These test methods cover procedures for the chemical analysis of copper-nickel and copper-nickel-zinc alloys having chemical compositions within select limits.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these test methods were withdrawn in March 2010. This standard was withdrawn without replacement due to its limited use by the industry.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:E75–76 (Reapproved 2004)
Standard Test Methods for
Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc
Alloys
This standard is issued under the fixed designation E75; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Sections
Lead:
1.1 These test methods cover procedures for the chemical
Electrolytic Method 12 to 15
2b
analysis of copper-nickel and copper-nickel-zinc alloys having
Sulfate Method
Manganese:
chemical compositions within the following limits:
2b
Persulfate Method
Element Concentration Range,%
Periodate (Photometric) 59 to 66
Copper 40 and over
Method
A
Nickel 10 to 50 2a
Nickel by the Dimethylglyoxime Method
B
2b
Zinc 0to40
Tin by the Iodimetric Titration Method
Lead 0 to 15 2a
Zinc by the Oxide or Ferrocyanide Method
Tin 0 to 10
Iron 0.00 to 2
1.3 This standard does not purport to address all of the
Manganese 0.00 to 2
safety concerns, if any, associated with its use. It is the
Cobalt 0.00 to 0.5
responsibility of the user of this standard to establish appro-
A
Includes cobalt.
priate safety and health practices and determine the applica-
B
In the case of copper-base alloys containing 5 % and over of zinc, the zinc is
bility of regulatory limitations prior to use. For precautions to
usually calculated by difference.
be observed in these test methods, refer to Practices E50.
Whenever possible the technique and procedures for analy-
sis should be checked against a National Institute of Standards
2. Referenced Documents
and Technology standard sample having a composition com-
2.1 ASTM Standards:
parable to the material being analyzed.
E29 Practice for Using Significant Digits in Test Data to
1.2 The test methods appear in the following order:
Determine Conformance with Specifications
Sections
E50 Practices for Apparatus, Reagents, and Safety Consid-
Cobalt:
Alpha-Nitroso-Beta-Naphthol Method 26 to 28
erations for Chemical Analysis of Metals, Ores, and
Nitroso-R-Salt (Photometric) Method 29 to 37
Related Materials
2a
Copper, or Copper and Lead Simultaneously, by the
E55 Practice for Sampling Wrought Nonferrous Metals and
Electrolytic Method
Iron:
Alloys for Determination of Chemical Composition
Dichromate Method 38 to 40
E60 Practice for Analysis of Metals, Ores, and Related
2a
Thiocyanate (Photometric)
Method Materials by Molecular Absorption Spectrometry
2a
Salicylate (Photometric)
E88 Practice for Sampling Nonferrous Metals andAlloys in
Method
Cast Form for Determination of Chemical Composition
3. Significance and Use
These test methods are under the jurisdiction of ASTM Committee E01 on
3.1 These test methods for the chemical analysis of metals
Analytical Chemistry for Metals, Ores and Related Materials and are the direct
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, theirAlloys and
and alloys are primarily intended to test such materials for
Related Metals.
compliance with compositional specifications. It is assumed
Current edition approved June 1, 2004. Published August 2004. Originally
that all who use these test methods will be trained analysts
approved in 1950. Last previous edition approved in 1996 as E75 – 76 (1996). DOI:
10.1520/E0075-76R04.
For procedures for the chemical analysis of nickel-copper alloys containing
50 % and over of nickel, see ASTM Methods E76, for Chemical Analysis of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Nickel-Copper Alloys, Annual Book of ASTM Standards, Vol 03.05. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2a
Discontinued as of June 30, 1975. Standards volume information, refer to the standard’s Document Summary page on
2b
Discontinued Aug. 27, 1976. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E75–76 (2004)
capable of performing common laboratory procedures skill- 10.2 Allow to stand on a steam bath for1hor until the
fully and safely. It is expected that work will be performed in precipitate has coagulated. Add paper pulp and filter off the
a properly equipped laboratory. metastannic acid through a fine paper into a 250-mL beaker.
Wash several times with hot HNO (1 + 99) and reserve the
4. Apparatus and Reagents
filtrate and washings.
4.1 Apparatus and reagents required for each determination 10.3 Transfer the filter paper and contents to the original
are listed in separate sections preceding the procedure. The beaker and add 15 mL of H SO and 15 mL of HNO . Heat
2 4 3
apparatus, standard solutions, and certain other reagents used until all organic matter is decomposed, adding additional HNO
in more than one procedure are referred to by number and shall 3 as necessary, and finally evaporate to fumes. Transfer the
conform to the requirements prescribed in Practices E50, digested solution to a 400-mL beaker and dilute to 250 mL.
except that photometers shall conform to the requirements Add NaOH solution until the solution is alkaline and the tin
prescribed in Practice E60. hydroxide has dissolved. Add 20 mL of Na S solution (250 g
Na S/L), stir thoroughly, and digest on the steam bath for
5. Photometric Practice
several hours, or until the supernatant liquid is clear. Cool to
5.1 Photometric practice prescribed in these methods shall room temperature, filter through a fine paper, and wash the
conform to Practice E60. precipitate with Na S solution (20 g Na S/L). Dissolve the
2 2
residue in a few millilitres of HNO (1 + 1), neutralize with
6. Sampling
NH OH, and redissolve any precipitate with a minimum of
6.1 Wrought products shall be sampled in accordance with HNO (1 + 1). Combine with the reserved filtrate (10.2) and
Practice E55. Cast products shall be sampled in accordance continue in accordance with 10.5.
with Practice E88. 10.4 An alternative method for recovering copper and lead
is to return the metastannic acid and paper obtained as
7. Rounding Calculated Values
described in 10.2 to the original beaker, add 15 to 20 mL of
7.1 Calculated values shall be rounded to the desired num- HNO and10to15mLofHClO ,heattocopiouswhitefumes,
3 4
ber of places in accordance with the rounding method given in and boil to destroy organic matter. Cool, wash the cover glass
3.4 and 3.5 of Practice E29. and sides of the beaker, and add 15 to 25 mL of HBr. Heat to
copious white fumes to volatilize the tin. If the solution is not
COPPER, OR COPPER AND LEAD
clear, repeat the treatment with HBr. Evaporate the solution to
SIMULTANEOUSLY,
near dryness, cool, and dissolve the residue in a few millilitres
BY THE ELECTROLYTIC TEST METHOD
ofwater.Combinewiththereservedfiltrate(10.2)andcontinue
(This test method, which consisted of Sections 8-11 of this in accordance with 10.5.
standard, was discontinued in 1975.) 10.5 Add 1 drop of HCl (1 + 99) and 5 mLof sulfamic acid
solution and dilute to 150 mL. Insert the electrodes into the
NOTE 1—Sections 8-11 of this standard were removed as a part of the
solution, cover with a pair of split watch glasses, and electro-
revision of E75 approved June 30, 1975. Since they are no longer an
lyze overnight at a current density of 0.5 A/dm or for a short
approved part of this standard, the sections are included here for reference
purposes only. Subcommittee E03.05 is in the process of updating these period at a current density of 4A/dm (Note 3). The more rapid
methods.
procedure requires the use of gauze cathodes. After the blue
color of the copper has disappeared, wash down the cover
8. Apparatus
glasses, electrodes, and sides of the beaker, and continue the
8.1 Electrodes for Electroanalysis— Apparatus No. 9.
electrolysis until deposition of the copper is complete, as
indicated by failure to plate on a new surface when the level of
9. Reagents
the solution is raised. When no copper appears, it can be
9.1 Sodium Hydroxide Solution (250 g NaOH/L).
assumed that all the lead also has been deposited (Note 4).
9.2 Sodium Sulfide Solution (250 g Na S/L).
2 Reserve the electrolyte.
9.3 Sodium Sulfide Solution (20gNa S/L).
NOTE 3—When agitation of the electrolyte is permissible in order to
9.4 Sulfamic Acid Solution (100 g/L).
decrease the time of deposition, one of the types of rotating forms of
electrodes generally available may be employed.
10. Procedure for Alloys Containing Under 6 % of Lead
NOTE 4—If the electrolyte is not to be used for subsequent determina-
tions, remove a few drops of the solution, place on a porcelain spot plate,
NOTE 2—If more than 6 % of lead is present, the copper only shall be
and treat with saturated H S solution. Continue electrolysis until no CuS
determined by this procedure as the anode deposit is not sufficiently
precipitate is observed.
adherentforsafehandling.Theleadshallthenbedeterminedonaseparate
sample as described in the sulfate method, Sections 16 and 17.
10.6 When deposition of the copper is complete, with the
10.1 Transfer 2.0000 g of the sample to a 250-mL beaker, current still on, lower the beaker slowly, while washing the
cover, and dissolve in 25 mL of HNO (1 + 1). When dissolu- cathode with water. Remove the cathode, rinse it in water, and
tion is complete, boil gently to expel brown fumes.Add 50 mL dip it in two successive baths of ethanol or methanol. Dry in an
of hot water and observe the clarity of the solution. If the oven at 110°C for 3 to 5 min, cool, and weigh the deposit as
solution is clear, proceed as described in 10.5. If enough tin is metallic copper.
present at this point to form a cloud, proceed as described in 10.7 If lead is being determined, remove the anode, rinse
10.2 and 10.3 or 10.2 and 10.4. thoroughlywithwater,anddryat110to120°Cfor30min.The
E75–76 (2004)
depositisfragileandmustbehandledcarefully.Cooltheanode 13.4 When deposition of the lead is complete, without
and weigh the deposit. interrupting the current, siphon off the electrolyte, at the same
10.8 Correction must be made for manganese, which is time filling the beaker with water. Remove the anode quickly,
frequently present in these alloys and some of which may rinse thoroughly with water, and dry at 110 to 120°C for 30
codeposit with the lead. Place the anode in a 150-mL beaker min.The deposit is fragile and must be handled carefully. Cool
and dissolve the deposit in 20 mL of HNO (1+1)and1mL the anode and weigh the deposit.
of H O (3 %). Remove the anode and wash with water. Add 13.5 Correct for manganese and calculate the percentage of
2 2
5mLofH PO andboilfor5to10min.Determinemanganese lead in accordance with 10.8 and 10.9.
3 4
either photometrically by the periodate method (Sections
31–38)orvolumetricallybythepersulfatemethod(Sections56 14. Procedure for Alloys Containing 0.05 % and Over of
to 58). Tin
10.9 Calculation—Calculate the percentages of copper and
14.1 Proceedinaccordancewith13.1or13.2.Removetinin
lead as follows:
accordance with 10.2 and 10.3 or 10.2 and 10.4. Electrolyze
and determine lead as directed in 13.3-13.5.
Copper, % 5 ~A/B! 3 100
Lead,% 5 ~@~C 2 1.58 D! 3 0.866]/B! 3 100
15. Precision and Bias
where:
15.1 This test method was originally approved for publica-
A = grams of copper,
tion before the inclusion of precision and accuracy statements
B = grams of sample used,
within standards was mandated. The original interlaboratory
C = grams of combined deposit of PbO plus MnO , and
2 2
test data is no longer available. The user is cautioned to verify
D = grams of manganese.
bytheuseofreferencematerials,ifavailable,thattheprecision
and accuracy of this method is adequate for the contemplated
11. Precision and Bias
use.
11.1 This method was originally approved for publication
before the inclusion of precision and accuracy statements
LEAD BY THE SULFATE TEST METHOD
within standards was mandated. The original interlaboratory
(This test method, which consisted of Sections 16 and 17,
test data is no longer available. The user is cautioned to verify
was discontinued in 1976.)
bytheuseofreferencematerials,ifavailable,thattheprecision
and accuracy of this method is adequate for the contemplated
TIN BY THE IODOMETRIC TITRATION TEST
use.
METHOD
LEAD BY THE ELECTROLYTIC TEST METHOD
(This test method, which consisted of Sections 18 through
20, was discontinued in 1976.)
12. Apparatus
12.1 Electrodes for Electroanalysis—Apparatus No. 9. Use
ZINC BY THE OXIDE OR FERROCYANIDE TEST
the larger electrode as the anode.
METHOD
(This test method, which consisted of Sections 21 and 22 of
13. Procedure for Alloys Containing Under 0.05 % of Tin
this standard, was discontinued in 1975.)
13.1 Solution of Samples Containing Under 0.1 % of
Lead—Transfer 10 g of the sample to a 400-mL beaker, cover,
NICKEL BY THE DIMETHYLGLYOXIME TEST
and dissolve in 60 mL of HNO (1 + 1). When dissolution is
METHOD
complete, boil gently to expel brown fumes. Wash down the
(Thistestmethod,whichconsistedofSections23through25
cover glass and the sides of the beaker and dilute to 250 mL.
of this standard, was discontinued in 1975.)
13.2 SolutionofSamplesContaining0.1to6 %ofLead(see
Note 2)— Transfer 1.000 g of the sample to a 250-mL beaker,
COBALT BY THE
cover, and dissolve in 20 mL of HNO (1 + 1). When dissolu-
ALPHA-NITROSO-BETA-NAPHTHOL TEST METHOD
tion is complete, boil gently to expel brown fumes.Wash down
the cover glass and the sides of the beaker and dilute to 150
mL.
13.3 Insert the electrodes into the solution, cover with a pair 26. Reagents
of split watch glasses, and electrolyze for2hata current 26.1 Alpha-Nitroso-Beta-Naphthol Solution (70 g/L)—
density of 1.25 to 1.50 A/dm . It is preferable to agitate the Dissolve7gof alpha-nitroso-beta-naphthol in 100 mL of
electrolyte. Electrolysis may take place overnight without glacialaceticacidandfilterthesolution.Preparethisreagentas
agitation and using a lower current density. Wash down the required just before using.
cover glasses, electrodes, and sides of the beaker, and continue 26.2 Zinc Oxide Suspension—Transfer 300 mL of water and
the electrolysis until no darkening of the newly exposed 50 g of finely powdered ZnO to a 500-mL flask. Stopper the
surface of the platinum anode can be detected when the current flask and shake the mixture vigorously each time before using.
has been continued for 15 min after the level of the liquid was
raised. 27. Procedure
E75–76 (2004)
27.1 Transfer5gofthe sample to a 250-mL beaker and COBALT
...
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