ASTM E75-76(1996)
(Test Method)Standard Test Methods for Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc Alloys
Standard Test Methods for Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc Alloys
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: Element Concentration Range, % Copper 40 and over Nickel A 10 to 50 Zinc B 0 to 40 Lead 0 to 15 Tin 0 to 10 Iron 0.00 to 2 Manganese 0.00 to 2 Cobalt 0.00 to 0.5 A Includes cobalt. B 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: Sections Cobalt: Alpha-Nitroso-Beta-Naphthol Method 26 to 28 Nitroso-R-Salt (Photometric) Method 29 to 37 Copper, or Copper and Lead Simultaneously, by the 2a Electrolytic Method Iron: Dichromate Method 38 to 40 Thiocyanate (Photometric) 2a Method Salicylate (Photometric) 2a Method Lead: Electrolytic Method 12 to 15 Sulfate Method 2b Manganese: Persulfate Method 2b Periodate (Photometric) 59 to 66 Method Nickel by the Dimethylglyoxime Method 2a Tin by the Iodimetric Titration Method 2b Zinc by the Oxide or Ferrocyanide Method 2a
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 determine the applicability of regulatory limitations prior to use. For precautions to be observed in these test methods, refer to Practices E50.
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Standards Content (Sample)
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Please contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation:E75–76 (Reapproved 1996)
Standard Test Methods for
Chemical Analysis of Copper-Nickel and Copper-Nickel-Zinc
Alloys
ThisstandardisissuedunderthefixeddesignationE 75;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
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.
1. Scope
Sections
2a
Nickel by the Dimethylglyoxime Method
1.1 These test methods cover procedures for the chemical 2b
Tin by the Iodimetric Titration Method
2a
analysis of copper-nickel and copper-nickel-zinc alloys having
Zinc by the Oxide or Ferrocyanide Method
chemical compositions within the following limits:
1.3 This standard does not purport to address all of the
Element Concentration Range,%
safety concerns, if any, associated with its use. It is the
Copper 40 and over
A
responsibility of the user of this standard to establish appro-
Nickel 10 to 50
B
Zinc 0to40
priate safety and health practices and determine the applica-
Lead 0 to 15
bility of regulatory limitations prior to use. For precautions to
Tin 0 to 10
be observed in these test methods, refer to Practices E 50E50.
Iron 0.00 to 2
Manganese 0.00 to 2
Cobalt 0.00 to 0.5
2. Referenced Documents
A
2.1 ASTM Standards:
Includes cobalt.
B
In the case of copper-base alloys containing 5 % and over of zinc, the zinc is
E29 Practice for Using Significant Digits in Test Data to
usually calculated by difference.
Determine Conformance With Specifications
Whenever possible the technique and procedures for analy-
E50 Practices for Apparatus, Reagents, and Safety Precau-
sis should be checked against a National Institute of Standards
tions for Chemical Analysis of Metals
and Technology standard sample having a composition com-
E55 PracticeforSamplingWroughtNonferrousMetalsand
parable to the material being analyzed.
Alloys for Determination of Chemical Composition
1.2 The test methods appear in the following order:
E60 Practice for Photometric and Spectrophotometric
Sections
Methods for Chemical Analysis of Metals
Cobalt:
E88 Practice for Sampling Nonferrous Metals and Alloys
Alpha-Nitroso-Beta-Naphthol Method 26 to 28
Nitroso-R-Salt (Photometric) Method 29 to 37
in Cast Form for Determination of Chemical Composition
2a
Copper, or Copper and Lead Simultaneously, by the
Electrolytic Method
3. Significance and Use
Iron:
Dichromate Method 38 to 40
3.1 These test methods for the chemical analysis of metals
2a
Thiocyanate (Photometric)
and alloys are primarily intended to test such materials for
Method
2a
compliance with compositional specifications. It is assumed
Salicylate (Photometric)
Method
that all who use these test methods will be trained analysts
Lead:
capable of performing common laboratory procedures skill-
Electrolytic Method 12 to 15
2b
Sulfate Method fully and safely. It is expected that work will be performed in
Manganese:
a properly equipped laboratory.
2b
Persulfate Method
Periodate (Photometric) 59 to 66
4. Apparatus and Reagents
Method
4.1 Apparatus and reagents required for each determination
are listed in separate sections preceding the procedure. The
These test methods are under the jurisdiction of ASTM Committee E-1 on apparatus, standard solutions, and certain other reagents used
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
in more than one procedure are referred to by number and shall
responsibility of Subcommittee E01.07 on Cu and Cu Alloys.
conform to the requirements prescribed in Practices E 50E50,
Current edition approved Aug. 27, 1976. Published October 1976. Originally
except that photometers shall conform to the requirements
published as E75 – 50 T. Last previous edition E75 – 75.
For procedures for the chemical analysis of nickel-copper alloys containing
prescribed in Practice E 60E60.
50 % and over of nickel, see ASTM Methods E 76, for Chemical Analysis of
Nickel-Copper Alloys, Annual Book of ASTM Standards, Vol 03.05.
2a 3
Discontinued as of June 30, 1975. Annual Book of ASTM Standards, Vol 14.02.
2b 4
Discontinued Aug. 27, 1976. Annual Book of ASTM Standards, Vol 03.05.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E75–76 (1996)
5. Photometric Practice Na S/L), stir thoroughly, and digest on the steam bath for
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 E 60E60.
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 3
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 E 55E55. Cast products shall be sampled in accor-
continue in accordance with 10.5.
dance with Practice E 88E88.
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 E 29E29.
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
NOTE 1—Sections 8-11 of this standard were removed as a part of the
solution and dilute to 150 mL. Insert the electrodes into the
revision of E75 approved June 30, 1975. Since they are no longer an
solution, cover with a pair of split watch glasses, and electro-
approved part of this standard, the sections are included here for reference 2
lyze overnight at a current density of 0.5 A/dm or for a short
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
8. Apparatus color of the copper has disappeared, wash down the cover
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).
Reserve the electrolyte.
9.3 Sodium Sulfide Solution (20gNa S/L).
9.4 Sulfamic Acid Solution (100 g/L).
NOTE 3—When agitation of the electrolyte is permissible in order to
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-
NOTE 2—If more than 6 % of lead is present, the copper only shall be
tions, remove a few drops of the solution, place on a porcelain spot plate,
determined by this procedure as the anode deposit is not sufficiently
and treat with saturated H S solution. Continue electrolysis until no CuS
adherentforsafehandling.Theleadshallthenbedeterminedonaseparate
precipitate is observed.
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
10.2 Allow to stand on a steam bath for1hor until the
depositisfragileandmustbehandledcarefully.Cooltheanode
precipitate has coagulated. Add paper pulp and filter off the
and weigh the deposit.
metastannic acid through a fine paper into a 250-mL beaker.
Wash several times with hot HNO (1 + 99) and reserve the 10.8 Correction must be made for manganese, which is
filtrate and washings. frequently present in these alloys and some of which may
10.3 Transfer the filter paper and contents to the original codeposit with the lead. Place the anode in a 150-mL beaker
beaker and add 15 mL of H SO and 15 mL of HNO . Heat and dissolve the deposit in 20 mL of HNO (1+1)and1mL
2 4 3 3
until all organic matter is decomposed, adding additional HNO of H O (3 %). Remove the anode and wash with water. Add
2 2
3 as necessary, and finally evaporate to fumes. Transfer the 5mLofH PO andboilfor5to10min.Determinemanganese
3 4
digested solution to a 400-mL beaker and dilute to 250 mL. either photometrically by the periodate method (Sections
Add NaOH solution until the solution is alkaline and the tin 31–38)orvolumetricallybythepersulfatemethod(Sections56
hydroxide has dissolved. Add 20 mL of Na S solution (250 g to 58).
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E75–76 (1996)
10.9 Calculation—Calculate the percentages of copper and 14. Procedure for Alloys Containing 0.05 % and Over of
lead as follows: Tin
14.1 Proceedinaccordancewith13.1or13.2.Removetinin
Copper, % 5 ~A/B! 3 100
accordance with 10.2 and 10.3 or 10.2 and 10.4. Electrolyze
Lead,% 5 ~@~C 2 1.58 D! 3 0.866]/B! 3 100
and determine lead as directed in 13.3-13.5.
where:
15. Precision and Bias
A = grams of copper,
B = grams of sample used,
15.1 This test method was originally approved for publica-
C = grams of combined deposit of PbO plus MnO , and
2 2
tion before the inclusion of precision and accuracy statements
D = grams of manganese.
within standards was mandated. The original interlaboratory
test data is no longer available. The user is cautioned to verify
11. Precision and Bias
bytheuseofreferencematerials,ifavailable,thattheprecision
and accuracy of this method is adequate for the contemplated
11.1 This method was originally approved for publication
use.
before the inclusion of precision and accuracy statements
within standards was mandated. The original interlaboratory
LEAD BY THE SULFATE TEST METHOD
test data is no longer available. The user is cautioned to verify
(This test method, which consisted of Sections 16 and 17,
bytheuseofreferencematerials,ifavailable,thattheprecision
was discontinued in 1976.)
and accuracy of this method is adequate for the contemplated
use.
TIN BY THE IODOMETRIC TITRATION TEST
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
NICKEL BY THE DIMETHYLGLYOXIME TEST
Lead—Transfer 10 g of the sample to a 400-mL beaker, cover,
METHOD
and dissolve in 60 mL of HNO (1 + 1). When dissolution is
complete, boil gently to expel brown fumes. Wash down the (Thistestmethod,whichconsistedofSections23through25
of this standard, was discontinued in 1975.)
cover glass and the sides of the beaker and dilute to 250 mL.
13.2 SolutionofSamplesContaining0.1to6 %ofLead(see
COBALT BY THE
Note 2)— Transfer 1.000 g of the sample to a 250-mL beaker,
ALPHA-NITROSO-BETA-NAPHTHOL TEST METHOD
cover, and dissolve in 20 mL of HNO (1 + 1). When dissolu-
tion is complete, boil gently to expel brown fumes.Wash down
the cover glass and the sides of the beaker and dilute to 150
26. Reagents
mL.
26.1 Alpha-Nitroso-Beta-Naphthol Solution (70 g/L)—
13.3 Insert the electrodes into the solution, cover with a pair
Dissolve7gof alpha-nitroso-beta-naphthol in 100 mL of
of split watch glasses, and electrolyze for2hata current
2 glacialaceticacidandfilterthesolution.Preparethisreagentas
density of 1.25 to 1.50 A/dm . It is preferable to agitate the
required just before using.
electrolyte. Electrolysis may take place overnight without
26.2 Zinc Oxide Suspension—Transfer 300 mL of water and
agitation and using a lower current density. Wash down the
50 g of finely powdered ZnO to a 500-mL flask. Stopper the
cover glasses, electrodes, and sides of the beaker, and continue
flask and shake the mixture vigorously each time before using.
the electrolysis until no darkening of the newly exposed
surface of the platinum anode can be detected when the current
27. Procedure
has been continued for 15 min after the level of the liquid was
27.1 Transfer5gofthe sample to a 250-mL beaker and
raised.
dissolve in 40 mL of HNO (1 + 1). When dissolution is
13.4 When deposition of the lead is complete, without
complete, boil gently to expel brown fumes. If a precipitate of
interrupting the current, siphon off the electrolyte, at the same
tin is present, add 50 mL of hot water, heat on the steam bath
time filling the beaker with water. Remove the anode quickly,
for 1 h, and filter off the metastannic acid through a fine paper,
rinse thoroughly with water, and dry at 110 to 120°C for
...
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