ASTM E396-05(2011)
(Test Method)Standard Test Methods for Chemical Analysis of Cadmium
Standard Test Methods for Chemical Analysis of Cadmium
SIGNIFICANCE AND USE
These test methods for the chemical analysis of cadmium are primarily intended to test such material for compliance with compositional specifications in Specification B440. 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 the chemical analysis of cadmium having chemical compositions with the following limits:
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
Designation:E396–05 (Reapproved 2011)
Standard Test Methods for
Chemical Analysis of Cadmium
This standard is issued under the fixed designation E396; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 These test methods cover the chemical analysis of 2.1 ASTM Standards:
cadmium having chemical compositions with the following B440 Specification for Cadmium
limits: D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to
Element Concentration, max, %
Determine Conformance with Specifications
Antimony 0.001
E50 Practices for Apparatus, Reagents, and Safety Consid-
Arsenic 0.003
erations for Chemical Analysis of Metals, Ores, and
Copper 0.015
Lead 0.025
Related Materials
Silver 0.010
E55 Practice for Sampling Wrought Nonferrous Metals and
Thallium 0.003
Tin 0.010 Alloys for Determination of Chemical Composition
Zinc 0.035
E60 Practice for Analysis of Metals, Ores, and Related
Materials by Spectrophotometry
1.2 The test methods appear in the following order:
E88 Practice for Sampling Nonferrous Metals andAlloys in
Sections
Antimony by the Rhodamine B Photometric Method 62-72 Cast Form for Determination of Chemical Composition
[0.0002 to 0.0010%]
E135 Terminology Relating to Analytical Chemistry for
Arsenic by the Molybdenum Blue Photometric Method 40-50
Metals, Ores, and Related Materials
[0.001 to 0.005%]
Copper by the Neocuproine Photometric Method [0.002 to 0.030%] 10-19 E173 Practice for Conducting Interlaboratory Studies of
Copper, Lead, Silver, and Zinc by the Atomic Absorption Method 51-61 3
Methods for Chemical Analysis of Metals
[0.004 to 0.02% Cu, 0.01 to 0.05% Pb, 0.004 to 0.02 % Ag
E1601 Practice for Conducting an Interlaboratory Study to
and 0.01 to 0.05% Zn]
Lead by the Dithizone Photometric Method [0.001 to 0.05%] 20-29
Evaluate the Performance of an Analytical Method
Thallium by the Rhodamine B Photometric Method 30-39
[0.0003 to 0.005%]
3. Terminology
Tin by the 8-Quinolinol Photometric Method [0.0025 to 0.0150%] 73-82
3.1 For definitions of terms used in this test method, refer to
1.3 The values stated in SI units are to be regarded as
Terminology E135.
standard. No other units of measurement are included in this
standard.
4. Significance and Use
1.4 This standard does not purport to address all of the
4.1 These test methods for the chemical analysis of cad-
safety concerns, if any, associated with its use. It is the
mium are primarily intended to test such material for compli-
responsibility of the user of this standard to establish appro-
ance with compositional specifications in Specification B440.
priate safety and health practices and determine the applica-
Itisassumedthatallwhousethesetestmethodswillbetrained
bility of regulatory limitations prior to use. Specific precau-
analysts capable of performing common laboratory procedures
tionary information is given in Section 6 and 25.8.
skillfully and safely. It is expected that work will be performed
in a properly equipped laboratory.
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 Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, theirAlloys, and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Related Metals. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 15, 2011. Published May 2011. Originally the ASTM website.
approved in 1970. Last previous edition approved in 2005 as E396 – 05. DOI: Withdrawn. The last approved version of this historical standard is referenced
10.1520/E0396-05R11. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
E396–05 (2011)
5. Apparatus, Reagents, and Photometric Practice 15. Reagents
5.1 Apparatus and reagents required for each determination 15.1 Chloroform (CHCl ).
are listed in separate sections preceding the procedure. The 15.2 Copper, Standard Solution (1 mL = 0.01 mg Cu)—
apparatus,standardsolutions,andreagentsshallconformtothe Dissolve 0.1000 g of copper (purity: 99.9 % min) in 10 mL of
requirements prescribed in Practices E50. Photometers shall HNO (1 + 1). Add 25 mL of water, heat to boiling, and boil
conform to the requirements prescribed in Practice E60. gently for 2 min to eliminate oxides of nitrogen. Cool, transfer
5.2 Photometric practice prescribed in these methods shall to a 100-mL volumetric flask, dilute to volume, and mix.
conform to Practice E60. Transfer 5.00 mL to a 500-mL volumetric flask. Add 1 mL of
HNO (1 + 1), dilute to volume, and mix.
6. Safety Hazards
15.3 Hydroxylamine Hydrochloride Solution (100 g/L)—
6.1 For precautions to be observed in the use of certain Dissolve 5.0 g of hydroxylamine hydrochloride
reagents in these test methods, refer to Practices E50.
(NH OH · HCl) in 50 mL of water. Prepare fresh as needed.
15.4 Metacresol Purple Indicator Solution (1 g/L)—
7. Sampling
Dissolve 0.100 g of metacresol purple together with 1 pellet of
7.1 Wrought products shall be sampled in accordance with
sodium hydroxide (NaOH) in about 10 mL of water by
Practice E55. Cast products shall be sampled in accordance warming. Dilute to 100 mL, and mix.
with Practice E88. However, these test methods do not super-
15.5 Neocuproine Solution (1 g/L)—Dissolve 0.10 g of
sede any sampling requirements specified in a specific ASTM neocuproine (2,9-dimethyl-1,10-phenanthroline hemihydrate)
material specification.
in 100 mL of either methanol or 95 % ethanol.
15.6 Sodium Citrate Solution (300 g/L)—Dissolve 300 g of
8. Rounding Calculated Values
sodium citrate dihydrate in water, dilute to 1 L, and mix.
8.1 Calculated values shall be rounded to the desired num-
15.7 PurityofWater—Unlessotherwiseindicated,reference
ber of places as directed in Practice E29.
to water shall be understood to mean reagent water as defined
by Type II of Specification D1193.
9. Interlaboratory Studies
9.1 These test methods have been evaluated in accordance 16. Preparation of Calibration Curve
with Practices E173, unless otherwise noted in the precision
16.1 Calibration Solution:
section.
16.1.1 Using pipets, transfer 2, 5, 10, 15, and 20 mL of
copper solution (1 mL = 0.01 mg Cu) to five 150-mL beakers,
COPPER BY THE NEOCUPROINE PHOTOMETRIC
and dilute to about 40 mL.
METHOD
16.1.2 Add 2 drops of metacresol purple indicator solution,
and then add HNO (1 + 1) dropwise to the red color change of
10. Scope 3
the indicator. Proceed as directed in 16.3.
10.1 This test method covers the determination of copper in
16.2 ReferenceSolution—Add40mLofwatertoa150-mL
concentrations from 0.002 to 0.030 %.
beaker. Proceed as directed in 16.1.2.
16.3 Color Development:
11. Summary of Test Method
16.3.1 Add 10 mL of NH OH · HCl solution, and stir. Add
11.1 Copper is separated as cuprous copper from other
10 mL of sodium citrate solution, and stir. Add NH OH to the
metals by extraction of the copper-neocuproine complex with
purple color of the indicator (pH about 8.5). Add 5.0 mL of
chloroform. Photometric measurement is made at approxi-
neocuproine solution, stir, and allow to stand for 5 min.
mately 455 nm.
NOTE 2—The precipitate that may form upon addition of sodium citrate
12. Concentration Range
solution will redissolve when the pH is raised to 8.5 with NH OH.
12.1 The recommended concentration range is from 0.01 to
16.3.2 Transfer to a 125-mLseparatory funnel marked at 80
0.15 mg of copper for each 25 mL of solution, using a 1-cm
mL, and dilute to the mark with water.Add 25.0 mLof CHCl .
cell.
Shake vigorously for 45 s, and allow the layers to separate.
Draw off and discard about 1 mL of the CHCl layer to rinse
NOTE 1—This test method has been written for cells having a 1-cm 3
the stem of the separatory funnel.
light path. Cells having other dimensions may be used, provided suitable
adjustments can be made in the amounts of sample and reagents used.
16.4 Photometry:
16.4.1 Multiple-Cell Photometer—Measure the cell correc-
13. Stability of Color
tion using absorption cells with a 1-cm light path and a light
13.1 The color develops within 5 min and the extracted
bandcenteredatapproximately455nm(Note3).Usingthetest
complex is stable. However, because of the volatile nature of
cell, take the photometric readings of the calibration solutions.
the solvent, it is advisable to take photometric readings
NOTE 3—Avoid transfer of water to the absorption cell in the following
promptly.
manner. Insert a loose plug of sterilized absorbent cotton into the stem of
each separatory funnel. Just prior to filling the absorption cell with the
14. Interferences
solution in the separatory funnel, discard about 1 mL of the CHCl layer
14.1 The elements ordinarily present do not interfere if their
through the cotton plug and immediately transfer a suitable portion of the
concentrations are under the maximum limits shown in 1.1. CHCl layer into the dry absorption cell.
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.
E396–05 (2011)
16.4.2 Single-Cell Photometer—Transfer a suitable portion in the chloroform is then removed by extraction with an
of the reference solution to an absorption cell with a 1-cm light ammoniacalsulfitesolution.Photometricmeasurementismade
path and adjust the photometer to the initial setting, using a at approximately 515 nm.
light band centered at approximately 455 nm (Note 1). While
22. Concentration Range
maintaining this adjustment, take the photometric readings of
22.1 The recommended concentration range is from 0.005
the calibration solutions.
16.5 Calibration Curve—Plot the net photometric readings to 0.050 mg of lead for each 25 mL of solution, using a 1-cm
cell (Note 1).
of the calibration solutions against milligrams of copper per 25
mL of solution.
23. Stability of Color
17. Procedure
23.1 The color is stable for at least2hif protected from
direct sunlight; however, because of the volatile nature of the
17.1 TestSolution—Transfer a 0.5-g sample, weighed to the
solvent, it is advisable to take photometric readings promptly.
nearest 1 mg, to a 150-mL beaker.Add 5 mL of HNO (1 + 1).
When dissolution is complete, add 20 mL of water and boil
24. Interferences
gently to eliminate oxides of nitrogen. Cool, dilute to about 40
24.1 The elements ordinarily present in cadmium do not
mL, and add 2 drops of metacresol purple indicator solution.
interfere if their concentrations are under the maximum limits
Proceed as directed in 17.3.
shown in 1.1.
17.2 ReferenceSolution—Carry a reagent blank through the
entireprocedureusingthesameamountofallreagentswiththe
25. Reagents
sample omitted, for use as the reference solution.
25.1 Ascorbic Acid.
17.3 Color Development—Proceed as directed in 16.3.
25.2 Bromine Water (Saturated).
17.4 Photometry—Proceed as directed in 16.4.
25.3 Chloroform (CHCl ).
18. Calculation 25.4 Dithizone Solution (0.01 g/L of CHCl )—Dissolve
0.05 g of dithizone (diphenylthiocarbazone) in a freshly
18.1 Convertthenetphotometricreadingofthetestsolution
opened 700-g bottle of CHCl . Mix several times over a period
to milligrams of copper by means of the calibration curve. 3
of several hours. Store in a cool, dark place. Just before use,
Calculate the percentage of copper as follows:
dilute 50 mL of this solution to 500 mL with CHCl in a dry
Copper, % 5A/ B 3 10! (1)
~
borosilicate bottle or flask, and mix.
25.5 Lead, Standard Solution (1 mL=0.005 mg Pb)—
where:
Dissolve 0.1000 g of lead (purity: 99.9 % min) in 20 mL of
A = copper found in the 25 mL of final test solution, mg,
HNO (1 + 1), and boil gently to eliminate oxides of nitrogen.
and
B = sample represented in 25 mL of final test solution, g. Cool, transfer to a 200-mL volumetric flask, dilute to volume,
andmix.Transfer5.00mLtoa500-mLvolumetricflask,dilute
to volume, and mix. Prepare the final solution fresh as needed.
19. Precision and Bias
25.6 Metacresol Purple Indicator Solution (1 g/L)—
Proceed as directed in 15.4.
19.1 Precision—Eight laboratories cooperated in testing
25.7 Potassium Cyanide Solution (200 g/L)—Dissolve 200
this test method and obtained the data summarized in Table 1.
g of potassium cyanide (KCN) (low in lead and sulfide)
19.2 Accuracy—No certified reference materials suitable
(Warning —See 25.8) in water, and dilute to 1 L. Bring to a
for testing this test method were available when the interlabo-
boilandboilfor2min.Cool,andstoreinapolyethylenebottle.
ratory testing program was conducted. The user of this test
25.8 SodiumSulfiteWashSolution—Dissolve1gof sodium
method is encouraged to employ accepted reference materials,
sulfite (Na SO ) in about 300 mLof water in a 1-Lvolumetric
if available, to determine the accuracy of this test method as
2 3
flask.Add 20 mLof the KCN solution and 475 mLof NH OH
applied in a specific laboratory.
(1 + 1) which has been prepared from a freshly opened bottle.
19.3 E173 has been replaced by Practice E1601. The repro-
Dilute to volume, and mix. Store in a polyethylene bottle.
ducibility Index R corresponds to the Reproducibility Index R
(Warning—The preparation, storage, and use of KCN solu-
of Practice E1601. Likewise the Repeatability Index R corre-
tions require care and attention.Avoid inhalation of fumes and
sponds to the Repeatability Index r of Practice E1601.
exposure of the skin to the chemical and its solutions. Do not
LEAD BY THE DITHIZONE PHOTOMETRIC
allow solutions containing cyanide to come in contact with
METHOD
stronglyacidicsolutions.Workinawell-ventilatedhood.Refer
to Section 6 of Practices E50.)
20. Scope
25.9 Sodium Tartrate Solution (250 g/L)—Dissolve 50 g of
20.1 This test method covers the determination of lead in
sodium tartrate dihydrate in water, and dilute to 200 mL.
concentrations from 0.001 to 0.05 %. 25.10 Thioglycolic Acid Solution (1+99)—Dilute 1.0 mL
of thioglycolic acid (mercaptoacetic acid) to 100 mL with
21. Summary of Test Method
water. Refrigerate both the concentrated and diluted acid
21.1 Lead dithizonate is extracted with chlorofor
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.