ASTM E62-89(1996)
(Test Method)Standard Test Methods for Chemical Analysis of Copper and Copper Alloys (Photometric Methods)
Standard Test Methods for Chemical Analysis of Copper and Copper Alloys (Photometric Methods)
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: Copper, % 50 and over Tin, % 0.0 to 20 Lead, % 0.0 to 27 Iron, % 0.0 to 4 Manganese, % 0.0 to 6 Silicon, % 0.0 to 5 Aluminum, % 0.0 to 12 Nickel, % 0.0 to 5 Sulfur, % 0.0 to 0.1 Phosphorus, % 0.0 to 1.0 Arsenic, % 0.0 to 1.0 Antimony, % 0.0 to 1.0 Zinc remainder
1.2 The analytical procedures appear in the following order: Antimony by the Iodoantimonite (Photometric) Test Method 70 to 79 Arsenic in Fire-Refined Copper by the Molybdate Test Method 60 to 69 Iron by the Thiocyanate Test Method 1a Manganese by the Periodate Test Method 41 to 48 Nickel by the Dimethylglyoxime-Extraction Photometric Test Method 1a Phosphorus by the Molybdivanadophosphoric Acid Method: Deoxidized Copper and Phosphorized Brasses 17 to 24 Copper-Base Alloys Containing 0.01 to 1.2% Phosphorus 25 to 33 Tin by the Phenylfluorone Photometric Test Method 80 to 90 Silicon by the Molybdisilicic Acid Test Method 49 to 59
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 the use of certain reagents, refer to Practices E50.
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Standards Content (Sample)
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Designation:E62–89(Reapproved 1996)
Standard Test Methods for
Chemical Analysis of Copper and Copper Alloys
(Photometric Methods)
ThisstandardisissuedunderthefixeddesignationE 62;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 Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Precau-
1.1 These test methods cover photometric procedures for
tions for Chemical Analysis of Metals
the chemical analysis of copper and copper alloys having
E55 PracticeforSamplingWroughtNonferrousMetalsand
chemical compositions within the following limits:
Alloys for Determination of Chemical Composition
Copper, % 50 and over
E60 Practice for Photometric and Spectrophotometric
Tin, % 0.0 to 20
Lead, % 0.0 to 27
Methods for Chemical Analysis of Metals
Iron, % 0.0 to 4
E88 Practice for Sampling Nonferrous Metals and Alloys
Manganese, % 0.0 to 6
in Cast Form for Determination of Chemical Composition
Silicon, % 0.0 to 5
Aluminum, % 0.0 to 12
E 173 Practice for Conducting Interlaboratory Studies of
Nickel, % 0.0 to 5
Methods for Chemical Analysis of Metals
Sulfur, % 0.0 to 0.1
Phosphorus, % 0.0 to 1.0
3. Significance and Use
Arsenic, % 0.0 to 1.0
Antimony, % 0.0 to 1.0
3.1 These test methods for the chemical analysis of metals
Zinc remainder
and alloys are primarily intended as referee methods to test
1.2 The analytical procedures appear in the following order:
such materials for compliance with compositional specifica-
Antimony by the Iodoantimonite (Photometric) Test Method 70 to 79
tions. It is assumed that all who use these methods will be
Arsenic in Fire-Refined Copper by the Molybdate Test Method 60 to 69
1a trained analysts capable of performing common laboratory
Iron by the Thiocyanate Test Method
Manganese by the Periodate Test Method 41 to 48 proceduresskillfullyandsafely.Itisexpectedthatworkwillbe
1a
Nickel by the Dimethylglyoxime-Extraction Photometric Test
performed in a properly equipped laboratory.
Method
Phosphorus by the Molybdivanadophosphoric Acid Method:
4. Photometric Practice, Apparatus, and Reagents
Deoxidized Copper and Phosphorized Brasses 17 to 24
Copper-Base Alloys Containing 0.01 to 1.2 % Phosphorus 25 to 33
4.1 Photometers and Photometric Practice—Photometers
Tin by the Phenylfluorone Photometric Test Method 80 to 90
and photometric practice prescribed in these test methods shall
Silicon by the Molybdisilicic Acid Test Method 49 to 59
conform to Practice E 60E60.
1.3 This standard does not purport to address all of the
4.2 Apparatus other than photometers, standard solutions,
safety concerns, if any, associated with its use. It is the
and certain other reagents used in more than one procedure are
responsibility of the user of this standard to establish appro-
referred to by number and shall conform to the requirements
priate safety and health practices and determine the applica-
prescribed in Practices E 50E50.
bility of regulatory limitations prior to use. For precautions to
be observed in the use of certain reagents, refer to Practices
5. Sampling
E50E50.
5.1 Wrought products shall be sampled in accordance with
Practice E 55E55. Cast products shall be sampled in accor-
2. Referenced Documents
dance with Practice E 88E88.
2.1 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to
6. Rounding Calculated Values
6.1 Calculated values shall be rounded to the desired num-
ber of places in accordance with the rounding method given in
These test methods are under the jurisdiction of ASTM Committee E-1 on
3.4 and 3.5 of Practice E 29E29.
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommitee E01.07 on Cu and Cu Alloys.
Current edition approved Jan. 27, 1989. Published March 1989. Originally
´2 2
published as E 62 – 46 T. Last previous edition E 62 – 76 (84) . Annual Book of ASTM Standards, Vol 14.02.
1a 3
Discontinued as of June 30, 1975. 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.
E62–89 (1996)
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
and heat just to boiling.Add 1 mLof H O (3 %) and swirl the
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
18. Concentration Range
excess H O has been destroyed. Cool to room temperature,
2 2
18.1 The recommended concentration range is from 0.04 to
transfer to a 50-mL volumetric flask, and add 2 mL of
1.0 mg of phosphorus in 50 mL of solution, using a cell depth
ammonium molybdate (95 g/L). Dilute to the mark, mix
of 1 cm.
thoroughly, and allow to stand 5 min.
NOTE 1—This procedure has been written for a cell having a 1-cm light
22.5 Transfer a suitable portion of the solution to an
path. Cells having other dimensions may be used, provided suitable
absorption cell and measure the transmittance or absorbance at
adjustments can be made in the amounts of sample and reagents used.
approximately 420 nm. Compensate or correct for the blank.
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
min and is stable for at least 1 h.
23. Procedure for Deoxidized Copper
23.1 Transfer 1.000 g of the sample (Note 2) to a 150-mL
beaker.Transfer 1.000 g of low-phosphorus copper to a second
20. Interfering Elements
beaker and carry through as a blank. Continue in accordance
20.1 The elements ordinarily present in deoxidized copper
with 22.2, 22.4, and 22.5.
and phosphorized brasses do not interfere, with the possible
NOTE 2—If tin is present, the time of boiling and period of digestion
exception of tin.
should be controlled carefully to avoid appreciable reduction of fluoride
content and resultant precipitation of tin.
23.2 Using the value obtained, read from the calibration
21. Reagents
curve the number of milligrams of phosphorus present in the
21.1 Ammonium Molybdate Solution (95 g (NH ) Mo -O
4 6 7 2
sample.
4/L)—Dissolve 100 g of (NH ) Mo O ·4H O in 600 mL of
4 6 7 24 2
23.3 Calculation—Calculate the percentage of phosphorus
water at 50°C, and dilute to 1 L. Filter before using.
as follows:
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 Phosphorus, % 5 A/~B 3 10!
4 3
solution is complete, add 20 mL of HNO (1+1) cool, and
where:
dilute to 1 L.
A = phosphorus, mg, and
21.3 Copper (low-phosphorus)—Copper containing under
B = sample used, g.
0.0002 % of phosphorus.
21.4 Hydrogen Peroxide (3 %)—Dilute 10 mL of
H O (30 %) to 100 mL. Store in a dark bottle in a cool place.
2 2
24. Procedure for Phosphorized Brasses
21.5 Potassium Permanganate Solution (10 g KMnO /L).
24.1 Transfer a portion of the sample containing 1.000 g of
21.6 Standard Phosphorus Solution (1 mL = 0.05 mg P)—
copper (Note 3) to a 150-mL beaker. Transfer 1.000 g of
Dissolve 0.2292 g of Na HPO in about 200 mLof water.Add
2 4
low-phosphorus copper to a second beaker and carry through
100 mLof HNO (1+5) and dilute to 1 Lin a volumetric flask.
as a blank. Continue as directed in Section 23, except that in
dissolving, add an additional 0.7 mL of HNO (2+3) for each
0.1 g of sample over 100 g.
For the determination of phosphorus in the presence of tin, see Sections 25 to
32. NOTE 3—Since Cu(NO ) shows a slight absorption at 420 nm, it is
3 2
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.
E62–89 (1996)
desirable that the amount of copper present in the sample be approxi-
29.5 Mixed Acids—Add 320 mL of HNO and 120 mL of
mately the same as that present in the solutions used for the preparation of
HCl to 500 mL of water. Cool, dilute to 1 L, and mix.
the calibration curve, as well as that present in the blank.
29.6 Standard Phosphorus Solution (1 mL = 0.05 mg P)—
Dilute one volume of phosphorus solution (1 mL = 0.4 mg P)
with seven volumes of water.
29.7 Standard Phosphorus Solution (1 mL = 0.2 mg P)—
PHOSPHORUS BY THE
Dilute one volume of phosphorus solution (1 mL = 0.4 mg P)
MOLYBDIVANADOPHOSPHORIC ACID TEST
with one volume of water.
METHOD
29.8 Standard Phosphorus Solution (1 mL = 0.4 mg P)—
(Copper Alloys containing 0.01 to 1.2 % of Phosphorus, with
Dissolve 1.8312 g of Na HPO in about 200 mLof water.Add
2 4
or without Tin)
100mLofHNO (1 + 5)anddiluteto1Linavolumetricflask.
25. Principle of Test Method
30. Preparation of Calibration Curve for Alloys
25.1Ayellow-colored complex is formed when an excess of
Containing 0.01 to 0.2 % of Phosphorus
molybdate solution is added to an acidified mixture of a
30.1Transfer1.00goflow-phosphoruscoppertoeachoften
vanadate and an ortho-phosphate. Photometric measurement is
150-mL beakers. Transfer 2.0, 4.0, 6.0, 8.0, and 10.0-mL
made at approximately 470 nm.
aliquots of phosphorus solution (1 mL = 0.05 mg P) to five of
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. Concentration Range
Carry the tenth through as a blank.
26.1 The recommended concentration range for low phos-
30.2Add 15.0 mLof the mixed acids (Note 6) and add a few
phorus contents is from 0.1 to 2 mg of phosphorus in 50 mLof
glass beads. Cover and heat moderately until dissolution is
solution, and for high phosphorus contents is from 0.3 to 6 mg
complete.
ofphosphorusin100mLofsolution,usingacelldepthof1cm
NOTE 6—The mixed acids should be measured accurately, since the
(see Note 1).
time required for full color development is dependent on the pH of the
solution.
30.3Add1mLofH O (3 %)tothesolution,andboilgently
27. Stability of Color
2 2
for 3 to 5 min, avoiding vigorous or prolonged boiling, since
27.1The color of the phosphorus complex develops within 5
excessive loss of acid will affect the subsequent color devel-
min and is stable for at least 1 h.
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),
28. Interfering Elements
dilute to 50 mL, and mix thoroughly.Allow to stand for 5 min.
28.1 Iron causes a slight interference (Note 4). Silicon and
30.4 Transfer a suitable portion of the solution to an
arsenic do not interfere when present in amounts up to about
absorption cell, and measure the transmittancy or absorbancy
1 %, but higher amounts of silicon cause interference by the
at approximately 470 nm. Compensate or correct for the blank.
formation of a turbid solution (Note 5).
30.5 Plot the values obtained against milligrams of phospho-
NOTE 4—The interference of iron may be avoided by using a portion of
rus per 50 mL of solution.
the sample for the blank and adding all reagents as prescribed in Section
32, with the exception of the molybdate solution. If electrolytic copper is
used for the blank, a correction factor should be determined and applied.
NOTE 5—Silver, if present in amounts over approximately 0.03 % 31.PreparationofCalibrationCurveforAlloysContaining
(about 10 oz/ton), may cause interference by the formation of a turbid
solution.
0.06 to 1.2 % of Phosphorus
31.1 Transfer 0.500 g of low-phosphorus copper to each of
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
29. Reagents
29.1 Ammonium Molybdate Solution (95 g (NH ) Mo - the beakers and transfer 8.0, 10.0, and 15.0-mL aliquots of
4 6 7
phosphorus solution (1 mL = 0.4 mg P) to three of the beakers.
O /L)—Dissolve 100 g of (NH ) Mo O ·4H O in 600 mL
24 4 6 7 24 2
of water at 50°C, and dilute to 1 L. Filter before using. Carry the ninth through as a blank.
29.2 Ammonium Vanadate Solution (2.5 g NH VO /L)— 31.2 Add 20.0 mL of the mixed acids (Note 6) and a few
4 3
Dissolve 2.50 g of NH VO in 500 mL of hot water. When grains of silicon carbide. Cover and heat moderately until
4 3
dissolution is complete.
solution is complete, add 20 mL of HNO (1+1), cool, and
dilute to 1 L. 31.3Add1mLofH O (3 %)tothesolution,andboilgently
2 2
29.3 Copper (low-phosphorus)—Copper containing under for 3 to 5 min, avoiding vigorous or prolonged boiling, since
0.0002 % of phosphorus. excessive loss of acid will affect the subsequent color devel-
29.4 Hydrogen Peroxide (3 %)—Dilute 10 mL of opment.Removefromheat,add10mLofammoniumvanadate
H O (30 %) to 100 mL. Store in a dark bottle in a cool place. (2.5 g/L), cool to room temperature, and transfer to a 100-mL
2 2
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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E62–89 (1996)
volumetric flask. Add 10 mL of ammonium molybdate (95 42.1 The recommended concentration range is from 0.1 to 2
g/L), dilute to 100 mL, and mix thoroughly.Allow to stand for mg of manganese in 100 mL of solution, using a cell depth of
5 min. 1 cm (see Note 1).
31.4 Transfer a suitable portion
...
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