ASTM E62-89(2004)
(Test Method)Standard Test Methods for Chemical Analysis of Copper and Copper Alloys (Photometric Methods) (Withdrawn 2010)
Standard Test Methods for Chemical Analysis of Copper and Copper Alloys (Photometric Methods) (Withdrawn 2010)
SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended as referee methods to test such materials for compliance with compositional specifications. It is assumed that all who use these 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 photometric procedures for the chemical analysis of copper and copper alloys having chemical compositions within the following limits:
1.2 The analytical procedures appear in the following order:
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 the use of certain reagents, refer to Practices E 50.
WITHDRAWN RATIONALE
These test methods cover photometric procedures for the chemical analysis of copper and copper alloys having chemical compositions within certain set 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jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these test methods were withdrawn in March 2010. This standard was withdrawn without replacement due to its limited use by the industry.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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E62–89(Reapproved 2004)
Standard Test Methods for
Chemical Analysis of Copper and Copper Alloys
(Photometric Methods)
This standard is issued under the fixed designation E62; 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 responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 These test methods cover photometric procedures for
bility of regulatory limitations prior to use. For precautions to
the chemical analysis of copper and copper alloys having
be observed in the use of certain reagents, refer to Practices
chemical compositions within the following limits:
E50.
Copper, % 50 and over
Tin, % 0.0 to 20
2. Referenced Documents
Lead, % 0.0 to 27
Iron, % 0.0 to 4 2
2.1 ASTM Standards:
Manganese, % 0.0 to 6
E29 Practice for Using Significant Digits in Test Data to
Silicon, % 0.0 to 5
Aluminum, % 0.0 to 12
Determine Conformance with Specifications
Nickel, % 0.0 to 5
E50 Practices for Apparatus, Reagents, and Safety Consid-
Sulfur, % 0.0 to 0.1
erations for Chemical Analysis of Metals, Ores, and
Phosphorus, % 0.0 to 1.0
Arsenic, % 0.0 to 1.0
Related Materials
Antimony, % 0.0 to 1.0
E55 Practice for Sampling Wrought Nonferrous Metals and
Zinc remainder
Alloys for Determination of Chemical Composition
1.2 The analytical procedures appear in the following order:
E60 Practice for Analysis of Metals, Ores, and Related
Antimony by the Iodoantimonite (Photometric) Test Method 70 to 79
Materials by Molecular Absorption Spectrometry
Arsenic in Fire-Refined Copper by the Molybdate Test Method 60 to 69
1a E88 Practice for Sampling Nonferrous Metals andAlloys in
Iron by the Thiocyanate Test Method
Manganese by the Periodate Test Method 41 to 48 Cast Form for Determination of Chemical Composition
1a
Nickel by the Dimethylglyoxime-Extraction Photometric Test
E173 Practice for Conducting Interlaboratory Studies of
Method
Methods for Chemical Analysis of Metals
Phosphorus by the Molybdivanadophosphoric Acid Method:
Deoxidized Copper and Phosphorized Brasses 17 to 24
3. Significance and Use
Copper-Base Alloys Containing 0.01 to 1.2 % Phosphorus 25 to 33
Tin by the Phenylfluorone Photometric Test Method 80 to 90
3.1 These test methods for the chemical analysis of metals
Silicon by the Molybdisilicic Acid Test Method 49 to 59
and alloys are primarily intended as referee methods to test
1.3 This standard does not purport to address all of the
such materials for compliance with compositional specifica-
safety concerns, if any, associated with its use. It is the
tions. It is assumed that all who use these methods will be
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of E01.05 Cu, Pb, Zn, Cd, Sn, Be, theirAlloys, and Related Metals on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Cu, Pb, Zn, Cd, Sn, Be, their Alloys and Related Metals. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2004. Published August 2004. Originally the ASTM website.
Withdrawn. The last approved version of this historical standard is referenced
approved in 1946. Last previous edition approved in 1996 as E62 – 89 (1996). DOI:
10.1520/E0062-89R04. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E62–89 (2004)
trained analysts capable of performing common laboratory
proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
performed in a properly equipped laboratory. 20. Interfering Elements
20.1 The elements ordinarily present in deoxidized copper
4. Photometric Practice, Apparatus, and Reagents
and phosphorized brasses do not interfere, with the possible
exception of tin.
4.1 Photometers and Photometric Practice—Photometers
and photometric practice prescribed in these test methods shall
conform to Practice E60.
21. Reagents
4.2 Apparatus other than photometers, standard solutions,
21.1 Ammonium Molybdate Solution (95 g (NH ) Mo -O
4 6 7 2
and certain other reagents used in more than one procedure are
4/L)—Dissolve 100 g of (NH ) Mo O ·4H O in 600 mL of
4 6 7 24 2
referred to by number and shall conform to the requirements
water at 50°C, and dilute to 1 L. Filter before using.
prescribed in Practices E50.
21.2 Ammonium Vanadate Solution (2.5 g NH VO /L)—
4 3
Dissolve 2.50 g of NH VO in 500 mL of hot water. When
4 3
5. Sampling
solution is complete, add 20 mL of HNO (1+1) cool, and
5.1 Wrought products shall be sampled in accordance with
dilute to 1 L.
Practice E55. Cast products shall be sampled in accordance
21.3 Copper (low-phosphorus)—Copper containing under
with Practice E88.
0.0002 % of phosphorus.
21.4 Hydrogen Peroxide (3 %)—Dilute 10 mL of
6. Rounding Calculated Values
H O (30 %) to 100 mL. Store in a dark bottle in a cool place.
2 2
21.5 Potassium Permanganate Solution (10 g KMnO /L).
6.1 Calculated values shall be rounded to the desired num-
ber of places in accordance with the rounding method given in 21.6 Standard Phosphorus Solution (1 mL = 0.05 mg P)—
3.4 and 3.5 of Practice E29. Dissolve 0.2292 g of Na HPO in about 200 mLof water.Add
2 4
100 mLof HNO (1+5) and dilute to 1 Lin a volumetric flask.
NICKEL BY THE DIMETHYLGLYOXIME-
EXTRACTION PHOTOMETRIC TEST METHOD
22. Preparation of Calibration Curve
(This test method, which consisted of Sections 7 through 16
22.1Transfer a 1.000-g portion of low-phosphorus copper to
of this standard, was discontinued in 1975.)
each of six 150-mL beakers.
22.2 Add exactly 10 mL of HNO (2 + 3) to each beaker.
PHOSPHORUS BY THE 3
Cover and let stand on a steam bath until dissolution is
MOLYBDIVANADOPHOSPHORIC ACID TEST
complete.
METHOD
22.3 Carry one portion through as a blank, and to the others
(Deoxidized Copper and Phosphorized Brasses)
add 1.0, 5.0, 10.0, 15.0, and 20.0-mL aliquots of phosphorus
solution (1 mL = 0.05 mg P).
22.4 Boil the covered solutions, including the blank, for
17. Principle of Test Method
about 1 min to expel brown fumes. Avoid vigorous or pro-
17.1Ayellow-colored complex is formed when an excess of
longed boiling, since excessive loss of HNO will affect
molybdate solution is added to an acidified mixture of a
subsequent color development. Add 2 mL of KMnO (10 g/L)
vanadate and an ortho-phosphate. Photometric measurement is
andheatjusttoboiling.Add1mLofH O (3 %)andswirlthe
2 2
made at approximately 420 nm.
sample until excess KMnO is destroyed and the solution
clears. Add 2 mL of ammonium vanadate (2.5 g/L) and boil
gently until the solution is a clear blue, which indicates that
excess H O has been destroyed. Cool to room temperature,
18. Concentration Range
2 2
transfer to a 50-mL volumetric flask, and add 2 mL of
18.1 The recommended concentration range is from 0.04 to
ammonium molybdate (95 g/L). Dilute to the mark, mix
1.0 mg of phosphorus in 50 mL of solution, using a cell depth
thoroughly, and allow to stand 5 min.
of 1 cm.
22.5 Transfer a suitable portion of the solution to an
NOTE 1—This procedure has been written for a cell having a 1-cm light
absorption cell and measure the transmittance or absorbance at
path. Cells having other dimensions may be used, provided suitable
approximately 420 nm. Compensate or correct for the blank.
adjustments can be made in the amounts of sample and reagents used.
22.6 Plot the values obtained against milligrams of phospho-
rus per 50 mL of solution.
19. Stability of Color
19.1The color of the phosphorus complex develops within 5 4
For the determination of phosphorus in the presence of tin, see Sections 25 to
min and is stable for at least 1 h. 32.
E62–89 (2004)
23. Procedure for Deoxidized Copper 27. Stability of Color
23.1 Transfer 1.000 g of the sample (Note 2) to a 150-mL 27.1The color of the phosphorus complex develops within 5
min and is stable for at least 1 h.
beaker.Transfer 1.000 g of low-phosphorus copper to a second
beaker and carry through as a blank. Continue in accordance
with 22.2, 22.4, and 22.5.
28. Interfering Elements
NOTE 2—If tin is present, the time of boiling and period of digestion
28.1 Iron causes a slight interference (Note 4). Silicon and
should be controlled carefully to avoid appreciable reduction of fluoride
arsenic do not interfere when present in amounts up to about
content and resultant precipitation of tin.
1 %, but higher amounts of silicon cause interference by the
23.2 Using the value obtained, read from the calibration
formation of a turbid solution (Note 5).
curve the number of milligrams of phosphorus present in the
NOTE 4—The interference of iron may be avoided by using a portion of
sample.
the sample for the blank and adding all reagents as prescribed in Section
23.3 Calculation—Calculate the percentage of phosphorus
32, with the exception of the molybdate solution. If electrolytic copper is
as follows:
used for the blank, a correction factor should be determined and applied.
Phosphorus, % 5 A/ B 3 10!
~ NOTE 5—Silver, if present in amounts over approximately 0.03 %
(about 10 oz/ton), may cause interference by the formation of a turbid
where:
solution.
A = phosphorus, mg, and
B = sample used, g.
29. Reagents
29.1 Ammonium Molybdate Solution (95 g (NH ) Mo -
4 6 7
24. Procedure for Phosphorized Brasses
O /L)—Dissolve 100 g of (NH ) Mo O ·4H O in 600 mL
24 4 6 7 24 2
24.1 Transfer a portion of the sample containing 1.000 g of
of water at 50°C, and dilute to 1 L. Filter before using.
copper (Note 3) to a 150-mL beaker. Transfer 1.000 g of
29.2 Ammonium Vanadate Solution (2.5 g NH VO /L)—
4 3
low-phosphorus copper to a second beaker and carry through
Dissolve 2.50 g of NH VO in 500 mL of hot water. When
4 3
as a blank. Continue as directed in Section 23, except that in
solution is complete, add 20 mL of HNO (1+1), cool, and
dissolving, add an additional 0.7 mL of HNO (2+3) for each
dilute to 1 L.
0.1 g of sample over 100 g.
29.3 Copper (low-phosphorus)—Copper containing under
NOTE 3—Since Cu(NO ) shows a slight absorption at 420 nm, it is
3 2 0.0002 % of phosphorus.
desirable that the amount of copper present in the sample be approxi-
29.4 Hydrogen Peroxide (3 %)—Dilute 10 mL of
mately the same as that present in the solutions used for the preparation of
H O (30 %) to 100 mL. Store in a dark bottle in a cool place.
2 2
the calibration curve, as well as that present in the blank.
29.5 Mixed Acids—Add 320 mL of HNO and 120 mL of
HCl to 500 mL of water. Cool, dilute to 1 L, and mix.
29.6 Standard Phosphorus Solution (1 mL = 0.05 mg P)—
Dilute one volume of phosphorus solution (1 mL = 0.4 mg P)
PHOSPHORUS BY THE
with seven volumes of water.
MOLYBDIVANADOPHOSPHORIC ACID TEST
29.7 Standard Phosphorus Solution (1 mL = 0.2 mg P)—
METHOD
Dilute one volume of phosphorus solution (1 mL = 0.4 mg P)
(Copper Alloys containing 0.01 to 1.2 % of Phosphorus, with
with one volume of water.
or without Tin)
29.8 Standard Phosphorus Solution (1 mL = 0.4 mg P)—
Dissolve 1.8312 g of Na HPO in about 200 mLof water.Add
2 4
100mLofHNO (1 + 5)anddiluteto1Linavolumetricflask.
25. Principle of Test Method
25.1Ayellow-colored complex is formed when an excess of
molybdate solution is added to an acidified mixture of a
30. Preparation of Calibration Curve for Alloys
vanadate and an ortho-phosphate. Photometric measurement is
Containing 0.01 to 0.2 % of Phosphorus
made at approximately 470 nm.
30.1Transfer1.00goflow-phosphoruscoppertoeachoften
150-mL beakers. Transfer 2.0, 4.0, 6.0, 8.0, and 10.0-mL
aliquots of phosphorus solution (1 mL = 0.05 mg P) to five of
26. Concentration Range the beakers and transfer 4.0, 6.0, 8.0, and 10.0-mL aliquots of
phosphorus solution (1 mL = 0.2 mg P) to four of the beakers.
26.1 The recommended concentration range for low phos-
Carry the tenth through as a blank.
phorus contents is from 0.1 to 2 mg of phosphorus in 50 mLof
solution, and for high phosphorus contents is from 0.3 to 6 mg 30.2Add 15.0 mLof the mixed acids (Note 6) and add a few
ofphosphorusin100mLofsolution,usingacelldepthof1cm glass beads. Cover and heat moderately until dissolution is
(see Note 1). complete.
E62–89 (2004)
NOTE 6—The mixed acids should be measured accurately, since the
32.4 Calculation—Calculate the percentage of phosphorus
time required for full color development is dependent on the pH of the
as follows:
solution.
Phosphorus, % 5 A/~B 3 10!
30.3Add1mLofH O (3 %)tothesolution,andboilgently
2 2
where:
for 3 to 5 min, avoiding vigorous or prolonged boiling, since
A = phosphorus, mg, and
excessive loss of acid will affect the subsequent color devel-
B = sample used, g.
opment. Remove from heat, add 5 mL of ammonium vanadate
(2.5 g/L), cool to room temperature, and transfer to a 50-mL
volumetric flask.Add 5 mLof ammonium molybdate (95 g/L),
33. Precision and Bias
dilute to 50 mL, and mix thoroughly.Allow to stand for 5 min.
33.1 This test method was originally approved for publica-
30.4 Transfer a suitable portion of the solution to an
tion before the inclusion of precision and bias statements
absorption cell, and measure the transmittancy or absorbancy
within standards was mandated. The original interlaboratory
at approximately 470 nm. Compensate or correct for the blank.
test data is no longer available. The user is cautioned to verify
30.5 Plot the values obtained against milligrams of phospho-
bytheuseofreferencematerials,ifavailable,thattheprecision
rus per 50 mL of solution.
and bias of this test method is adequate for the contemplated
use.
31.PreparationofCalibrationCurveforAlloysContaining
IRON BY THE THIOCYANATE TEST METHOD
0.06 to 1.2 % of Phosphorus
(Thistestmethod,whichconsistedofSections34through40
31.1 Transfer 0.500 g of low-phosphorus copper to each of
of this standard, was discontinued in 1975.)
nine 150-mL beakers. Transfer 1.0, 2.0, 3.0, 5.0, and 10.0-mL
aliquots of phosphorus solution (1 mL = 0.2 mg P) to five of
MANGANESE BY THE PERIODATE TEST METHOD
the beakers and transfer 8.0, 10.0, and 15.0-mL aliquots of
(For Manganese Bronze)
phosphorus solution (1 mL = 0.4 mg P) to three of the beakers.
Carry the ninth through as a blank.
31.2 Add 20.0 mL of the mixed acids (Note 6) and a few
41. Pr
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