ASTM E396-98

Standard Test Methods for Chemical Analysis of Cadmium

SCOPE
1.1 These test methods cover the chemical analysis of cadmium having chemical compositions with the following limits:  Element Concentration, max, % Zinc 0.035 Copper 0.015 Lead 0.025 Tin 0.010 Silver 0.010 Antimony 0.001 Arsenic 0.003 Thallium 0.003
1.2 The test methods appear in the following order:  Sections Copper by the Neocuproine Photometric Method 9 to 18 Lead by the Dithizone Photometric Method 19 to 28 Thallium by the Rhodamine B Photometric Method 29 to 38 Arsenic by the Molybdenum Blue Photometric Method 39 to 49 Copper, Lead, Silver, and Zinc by the Atomic Absorption Method 50 to 60 Antimony by the Rhodamine B Photometric Method 61 to 71 Tin by the 8-Quinolinol Photometric Method 72 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 determine the applicability of regulatory limitations prior to use. Specific precautionary information is given in Section 5 and Note 4.

General Information

• Status: Historical
• Publication Date: 09-May-1998
• ICS: 71.040.40 - Chemical analysis
• ICS: 77.040.30 - Chemical analysis of metals
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.05 - Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals

Relations

• Referred By: ASTM B440-12(2021) - Standard Specification for Cadmium
• Effective Date: 10-May-1998
• Referred By: ASTM B816-00(2021) - Standard Specification for Coatings of Cadmium-Zinc Mechanically Deposited
• Effective Date: 10-May-1998
• Referred By: ASTM B635-00(2023) - Standard Specification for Coatings of Cadmium-Tin Mechanically Deposited
• Effective Date: 10-May-1998
• Referred By: ASTM B699-86(2021)e1 - Standard Specification for Coatings of Cadmium Vacuum-Deposited on Iron and Steel
• Effective Date: 10-May-1998

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E 396 – 98
Standard Test Methods for
Chemical Analysis of Cadmium
This standard is issued under the fixed designation E 396; 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 tions for Chemical Analysis of Metals
E 55 Practice for Sampling Wrought Nonferrous Metals and
1.1 These test methods cover the chemical analysis of
Alloys for Determination of Chemical Composition
cadmium having chemical compositions with the following
E 60 Practice for Photometric and Spectrophotometric
limits:
Methods for Chemical Analysis of Metals
Element Concentration, max, %
E 88 Practice for Sampling Nonferrous Metals and Alloys
Antimony 0.001
in Cast Form for Determination of Chemical Composition
Arsenic 0.003
E 173 Practices for Conducting Interlaboratory Studies of
Copper 0.015
Methods for Chemical Analysis of Metals
Lead 0.025
Silver 0.010
Thallium 0.003
3. Significance and Use
Tin 0.010
3.1 These test methods for the chemical analysis of metals
Zinc 0.035
and alloys are primarily intended to test such materials for
1.2 The test methods appear in the following order:
compliance with compositional specifications. It is assumed
Sections
that all who use these test methods will be trained analysts
Antimony by the Rhodamine B Photometric Method 61-71
Arsenic by the Molybdenum Blue Photometric Method 39-49 capable of performing common laboratory procedures skill-
Copper by the Neocuproine Photometric Method 9-18
fully and safely. It is expected that work will be performed in
Copper, Lead, Silver, and Zinc by the Atomic Absorption Method 50-60
a properly equipped laboratory.
Lead by the Dithizone Photometric Method 19-28
Thallium by the Rhodamine B Photometric Method 29-38
4. Apparatus, Reagents, and Photometric Practice
Tin by the 8-Quinolinol Photometric Method 72-81
4.1 Apparatus and reagents required for each determination
1.3 This standard does not purport to address all of the
are listed in separate sections preceding the procedure. The
safety problems, if any, associated with its use. It is the
apparatus, standard solutions, and certain other reagents used
responsibility of the user of this standard to establish appro-
in more than one procedure are referred to by number and shall
priate safety and health practices and determine the applica-
conform to the requirements prescribed in Practices E 50,
bility of regulatory limitations prior to use. Specific precau-
except that photometers shall conform to the requirements
tionary information is given in Section 5 and Note 4.
prescribed in Practice E 60.
2. Referenced Documents
4.2 Photometric practice prescribed in these methods shall
conform to Practice E 60.
2.1 ASTM Standards:
B 440 Specification for Cadmium
5. Safety Precautions
E 29 Practice for Using Significant Digits in Test Data to
5.1 For precautions to be observed in the use of certain
Determine Conformance with Specifications
reagents in these test methods, refer to Practices E 50.
E 50 Practices for Apparatus, Reagents, and Safety Precau-
6. Sampling
6.1 Wrought products shall be sampled in accordance with
These test methods are under the jurisdiction of ASTM Committee E-1 on
Practice E 55. Cast products shall be sampled in accordance
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
with Practice E 88. However, these test methods do not
responsibility of Subcommittee E01.05 on Zinc, Tin, Lead, Cadmium, Beryllium,
supersede any sampling requirements specified in a specific
and Other Metals.
Current edition approved May 10, 1998. Published July 1998. Originally ASTM material specification.
e1
published as E 396 – 70 T. Last previous edition E 396 – 72a(93) .
Annual Book of ASTM Standards, Vol 02.04.
3 4
Annual Book of ASTM Standards, Vol 14.02. Annual Book of ASTM Standards, Vol 03.05.
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E 396
7. Rounding Calculated Values 14.6 Sodium Citrate Solution (300 g/L)—Dissolve 300 g of
sodium citrate dihydrate in water, dilute to 1 L, and mix.
7.1 Calculated values shall be rounded to the desired num-
ber of places as directed in 3.4 to 3.6 of Practice E 29.
15. Preparation of Calibration Curve
8. Interlaboratory Studies 15.1 Calibration Solution:
15.1.1 Using pipets, transfer 2, 5, 10, 15, and 20 mL of
8.1 These test methods have been evaluated in accordance
copper solution (1 mL 5 0.01 mg Cu) to five 150-mL beakers,
with Practices E 173, unless otherwise noted in the precision
and dilute to about 40 mL.
section.
15.1.2 Add 2 drops of metacresol purple indicator solution,
and then add HNO (1 + 1) dropwise to the red color change of
COPPER BY THE NEOCUPROINE PHOTOMETRIC
the indicator. Proceed as directed in 15.3.
METHOD
15.2 Reference Solution—Add 40 mL of water to a 150- mL
9. Scope beaker. Proceed as directed in 15.1.2.
15.3 Color Development:
9.1 This test method covers the determination of copper in
15.3.1 Add 10 mL of NH OH · HCl solution, and stir. Add
concentrations from 0.002 to 0.030 %.
10 mL of sodium citrate solution, and stir. Add NH OH to the
purple color of the indicator (pH about 8.5). Add 5.0 mL of
10. Summary of Test Method
neocuproine solution, stir, and allow to stand for 5 min.
10.1 Copper is separated as cuprous copper from other
metals by extraction of the copper-neocuproine complex with
NOTE 2—The precipitate that may form upon addition of sodium citrate
chloroform. Photometric measurement is made at approxi- solution will redissolve when the pH is raised to 8.5 with NH OH.
mately 455 nm.
15.3.2 Transfer to a 125-mL separatory funnel marked at 80
mL, and dilute to the mark with water. Add 25.0 mL of CHCl .
11. Concentration Range
Shake vigorously for 45 s, and allow the layers to separate.
11.1 The recommended concentration range is from 0.01 to
Draw off and discard about 1 mL of the CHCl layer to rinse
0.15 mg of copper for each 25 mL of solution, using a 1-cm
the stem of the separatory funnel.
cell.
15.4 Photometry:
15.4.1 Multiple-Cell Photometer—Measure the cell correc-
NOTE 1—This test method has been written for cells having a 1-cm
tion using absorption cells with a 1-cm light path and a light
light path. Cells having other dimensions may be used, provided suitable
band centered at approximately 455 nm (Note 3). Using the test
adjustments can be made in the amounts of sample and reagents used.
cell, take the photometric readings of the calibration solutions.
12. Stability of Color
NOTE 3—Avoid transfer of water to the absorption cell in the following
12.1 The color develops within 5 min and the extracted
manner. Insert a loose plug of sterilized absorbent cotton into the stem of
complex is stable. However, because of the volatile nature of
each separatory funnel. Just prior to filling the absorption cell with the
the solvent, it is advisable to take photometric readings
solution in the separatory funnel, discard about 1 mL of the CHCl layer
through the cotton plug and immediately transfer a suitable portion of the
promptly.
CHCl layer into the dry absorption cell.
13. Interferences
15.4.2 Single-Cell Photometer—Transfer a suitable portion
13.1 The elements ordinarily present do not interfere if their
of the reference solution to an absorption cell with a 1-cm light
concentrations are under the maximum limits shown in 1.1. path and adjust the photometer to the initial setting, using a
light band centered at approximately 455 nm (Note 1). While
14. Reagents
maintaining this adjustment, take the photometric readings of
the calibration solutions.
14.1 Chloroform (CHCl ).
15.5 Calibration Curve—Plot the net photometric readings
14.2 Copper, Standard Solution (1 mL 5 0.01 mg Cu)—
Dissolve 0.1000 g of copper (purity: 99.9 % min) in 10 mL of of the calibration solutions against milligrams of copper per 25
mL of solution.
HNO (1 + 1). Add 25 mL of water, heat to boiling, and boil
gently for 2 min to eliminate oxides of nitrogen. Cool, transfer
16. Procedure
to a 100-mL volumetric flask, dilute to volume, and mix.
Transfer 5.00 mL to a 500-mL volumetric flask. Add 1 mL of 16.1 Test Solution—Transfer a 0.5-g sample, weighed to the
HNO (1 + 1), dilute to volume, and mix. nearest 1 mg, to a 150-mL beaker. Add 5 mL of HNO (1 + 1).
3 3
14.3 Hydroxylamine Hydrochloride Solution (100 g/L)— When dissolution is complete, add 20 mL of water and boil
Reagent 131. gently to eliminate oxides of nitrogen. Cool, dilute to about 40
14.4 Metacresol Purple Indicator Solution (1 g/L)— mL, and add 2 drops of metacresol purple indicator solution.
Dissolve 0.100 g of metacresol purple together with 1 pellet of Proceed as directed in 16.3.
sodium hydroxide (NaOH) in about 10 mL of water by 16.2 Reference Solution—Carry a reagent blank through the
warming. Dilute to 100 mL, and mix. entire procedure using the same amount of all reagents with the
14.5 Neocuproine Solution (1 g/L)—Dissolve 0.10 g of sample omitted, for use as the reference solution.
neocuproine (2,9-dimethyl-1,10-phenanthroline hemihydrate) 16.3 Color Development—Proceed as directed in 15.3.
in 100 mL of either methanol or 95 % ethanol. 16.4 Photometry—Proceed as directed in 15.4.
E 396
17. Calculation 24. Reagents
17.1 Convert the net photometric reading of the test solution 24.1 Ascorbic Acid.
to milligrams of copper by means of the calibration curve. 24.2 Bromine Water (Saturated).
Calculate the percentage of copper as follows: 24.3 Chloroform (CHCl ).
24.4 Dithizone Solution (0.01 g/L of CHCl )—Dissolve
Copper, % 5 A/~B 3 10! (1)
0.05 g of dithizone (diphenylthiocarbazone) in a freshly
where: opened 700-g bottle of CHCl . Mix several times over a period
A 5 copper found in the 25 mL of final test solution, mg,
of several hours. Store in a cool, dark place. Just before use,
and
dilute 50 mL of this solution to 500 mL with CHCl in a dry
B 5 sample represented in 25 mL of final test solution, g.
borosilicate bottle or flask, and mix.
24.5 Lead, Standard Solution (1 mL 5 0.005 mg Pb)—
Dissolve 0.1000 g of lead (purity: 99.9 % min) in 20 mL of
18. Precision and Bias
HNO (1 + 1), and boil gently to eliminate oxides of nitrogen.
18.1 Precision—Eight laboratories cooperated in testing Cool, transfer to a 200-mL volumetric flask, dilute to volume,
and mix. Transfer 5.00 mL to a 500-mL volumetric flask, dilute
this test method and obtained the data summarized in Table 1.
to volume, and mix. Prepare the final solution fresh as needed.
18.2 Accuracy—No certified reference materials suitable
24.6 Metacresol Purple Indicator Solution (1 g/L)—
for testing this test method were available when the interlabo-
Proceed as directed in 14.4.
ratory testing program was conducted. The user of this test
24.7 Potassium Cyanide Solution (200 g/L)—Dissolve 200
method is encouraged to employ accepted reference materials,
g of potassium cyanide (KCN) (low in lead and sulfide)
if available, to determine the accuracy of this test method as
(Caution: See Note 4) in water, and dilute to 1 L. Bring to a
applied in a specific laboratory.
boil and boil for 2 min. Cool, and store in a polyethylene bottle.
LEAD BY THE DITHIZONE PHOTOMETRIC 24.8 Sodium Sulfite Wash Solution—Dissolve1gof sodium
sulfite (Na SO ) in about 300 mL of water in a 1-L volumetric
METHOD
2 3
flask. Add 20 mL of the KCN solution (Caution: see Note 4)
19. Scope and 475 mL of NH OH (1 + 1) which has been prepared from
a freshly opened bottle. Dilute to volume, and mix. Store in a
19.1 This test method covers the determination of lead in
polyethylene bottle.
concentrations from 0.001 to 0.05 %.
NOTE 4—Caution: The preparation, storage, and use of KCN solutions
20. Summary of Test Method
require care and attention. Avoid inhalation of fumes and exposure of the
skin to the chemical and its solutions. Do not allow solutions containing
20.1 Lead dithizonate is extracted with chloroform from a
cyanide to come in contact with strongly acidic solutions. Work in a
buffered cyanide solution at a pH of 8.5. The excess dithizone
well-ventilated hood. Refer to Section 6 of Practices E 50.
in the chloroform is then removed by extraction with an
24.9 Sodium Tartrate Solution (250 g/L)—Dissolve 50 g of
ammoniacal sulfite solution. Photometric measurement is made
sodium tartrate dihydrate in water, and dilute to 200 mL.
at approximately 515 nm.
24.10 Thioglycolic Acid Solution (1 + 99)—Dilute 1.0 mL
of thioglycolic acid (mercaptoacetic acid) to 100 mL with
21. Concentration Range
water. Refrigerate both the concentrated and diluted acid
21.1 The recommended concentration range is from 0.005
solutions. Do not use concentrated acid that is more than 1 year
to 0.050 mg of lead for each 25 mL of solution, using a 1-cm
old, nor diluted acid that has stood for more than 1 week.
cell (Note 1).
25. Preparation of Calibration Curve
22. Stability of Color
25.1 Calibration Solutions—Using pipets, transfer 1, 2, 3,
22.1 The color is stable for at least2hif protected from
5, and 10-mL volumes of lead solution (1 mL 5 0.005 mg Pb)
direct sunlight; however, because of the volatile nature of the
to 125-mL separatory funnels (set No. 1). Dilute to 15 mL with
solvent, it is advisable to take photometric readings promptly.
water and add 1 drop of metacresol purple indicator solution.
25.2 Reference Solution—Transfer 15 mL of water to a
23. Interferences
125-mL separatory funnel (one of set No. 1), and add 1 drop of
23.1 The elements ordinarily present in cadmium do not
metacresol purple indicator solution.
interfere if their concentrations are under the maximum limits
25.3 Color Development:
shown in 1.1.
25.3.1 Add NH OH (1 + 1) dropwise, with swirling, until
the indicator color begins to change from red to yellow. Add 2
drops of HNO . Extract with successive 10-mL portions of
TABLE 1 Statistical Information
dithizone solution until the color of the dithizone remains
Copper Found, Repeatability Reproducibility
Specimen unchanged. Discard all extracts.
% (R , E 173) (R , E 173)
1 2
25.3.2 Add 2 mL of sodium tartrate solution, about 20 mg of
1 0.0074 0.003 0.0013
ascorbic acid, and 2 drops of thioglycolic acid solution
2 0.0173 0.0018 0.0031
(1 + 99). Add NH OH (1 + 1), while mixing, until the solution
E 396
turns yellow. Add 20 mL of KCN solution (Caution: see Note
A 5 lead in the 25 mL of final test solution, mg, and
4) and mix. Add 10 mL of acetic acid (1 + 4), and mix.
B 5 sample repre
...