ASTM E37-05(2011)
(Test Method)Standard Test Methods for Chemical Analysis of Pig Lead (Withdrawn 2020)
Standard Test Methods for Chemical Analysis of Pig Lead (Withdrawn 2020)
SIGNIFICANCE AND USE
These test methods for the chemical analysis of metals and alloys are primarily intended 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 the chemical analysis of pig lead having chemical compositions within the following limits:
WITHDRAWN RATIONALE
These test methods covered the chemical analysis of pig lead.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, these test methods were withdrawn in July 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E37 − 05 (Reapproved 2011)
Standard Test Methods for
Chemical Analysis of Pig Lead
This standard is issued under the fixed designation E37; 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.
1. Scope erations for Chemical Analysis of Metals, Ores, and
Related Materials
1.1 These test methods cover the chemical analysis of pig
E60 Practice for Analysis of Metals, Ores, and Related
lead having chemical compositions within the following limits:
Materials by Spectrophotometry
Element Concentration Range, %
E135 Terminology Relating to Analytical Chemistry for
Antimony 0.001 to 0.02
Metals, Ores, and Related Materials
Arsenic 0.0005 to 0.02
Bismuth 0.002 to 0.2 E173 Practice for Conducting Interlaboratory Studies of
Copper 0.001 to 0.1
Methods for Chemical Analysis of Metals (Withdrawn
Iron 0.0005 to 0.005
1998)
Lead 99.5 to 99.99
E1601 Practice for Conducting an Interlaboratory Study to
Silver 0.001 to 0.03
Tin 0.001 to 0.02
Evaluate the Performance of an Analytical Method
Zinc 0.001 to 0.005
1.2 The test methods appear in the following order:
3. Terminology
Sections
3.1 For definitions of terms used in this test method, refer to
Antimony by the Rhodamine-B Photometric Method 21-30
Terminology E135.
Copper, Bismuth, Silver, and Zinc by the Atomic Absorption 10-20
Method
4. Significance and Use
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4.1 These test methods for the chemical analysis of metals
standard.
and alloys are primarily intended to test such materials for
1.4 This standard does not purport to address all of the compliance with compositional specifications. It is assumed
safety concerns, if any, associated with its use. It is the that all who use these methods will be trained analysts capable
responsibility of the user of this standard to consult and of performing common laboratory procedures skillfully and
establish appropriate safety and health practices and deter- safely. It is expected that work will be performed in a properly
mine the applicability of regulatory limitations prior to use.
equipped laboratory.
Specific precautionary statements are given in the individual
test methods. 5. Apparatus, Reagents, and Photometric Practice
5.1 Apparatus and reagents required for each determination
2. Referenced Documents
are listed in separate sections of each test method. The
2.1 ASTM Standards:
apparatus, standard solutions, and reagents conform to the
B29 Specification for Refined Lead
requirements prescribed in Practices E50. Photometers shall
E29 Practice for Using Significant Digits in Test Data to
conform to the requirements prescribed in Practice E60.
Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Consid- 6. Safety Hazards
6.1 For precautions to be observed in the use of certain
reagents in these test methods, refer to Practices E50.
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, theirAlloys, and
7. Sampling
Related Metals.
7.1 For procedures for sampling the material, refer to
Current edition approved Feb. 1, 2011. Published March 2011. Originally
approved in 1942. Last previous edition approved in 2005 as E37 – 05. DOI:
Specification B29.
10.1520/E0037-05R11.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E37 − 05 (2011)
8. Rounding Calculated Values 12.1.4 If the minimum response is not achieved, prepare
another dilute standard solution to provide a higher concentra-
8.1 Calculated values shall be rounded to the desired num-
tionrange,andrepeat12.1.2and12.1.3.Ifthecalibrationcurve
ber of places as directed in Practice E29.
does not meet the linearity criterion, prepare another dilute
9. Interlaboratory Studies
standard solution to provide a lower concentration range, and
repeat 12.1.2 and 12.1.3. If a concentration range cannot be
9.1 These test methods have been evaluated in accordance
found for which both criteria can be met, do not use this
with Practice E173, unless otherwise noted in the precision
method until the performance of the apparatus has been
section.
improved.
COPPER, BISMUTH, SILVER, AND ZINC BY THE
12.1.5 Perform the stability test as directed in 14.1.3.If
ATOMIC ABSORPTION METHOD
either of the minimum stability requirements is not met, do not
use this method until the repeatability of the readings has been
10. Scope
suitably improved.
10.1 This test method covers the determination of bismuth
in concentrations from 0.002 to 0.2 %, copper from 0.001 to
13. Interferences
0.1 %, silver from 0.001 to 0.03 %, and zinc from 0.001 to
0.005 %.
13.1 Elements ordinarily present do not interfere if their
concentrations are under the maximum limits shown in 1.1.
11. Summary of Test Method
11.1 The sample is dissolved in a nitric-perchloric acid
14. Apparatus
mixture, the solution is fumed, and hydrochloric acid is added
14.1 Atomic Absorption Spectrophotometer—Use hollow-
to precipitate lead chloride. The hydrochloric-perchloric acid
cathode lamps, operated in accordance with manufacturers’
solution is aspirated into the air-acetylene flame of an atomic
recommendations as sources for the following lines: Cu 324.7,
absorption spectrophotometer. The absorption of the resonance
Bi 223.0, Ag 328.0, and Zn 213.8 nm. Aspirate the solutions
line energy from the spectrum of each element is measured and
compared with that of calibration solutions of the same into an air-acetylene flame of a premix burner. Determine that
element. The lines used were Cu 324.7, Bi 223.0, Ag 328.0, the atomic absorption spectrophotometer is satisfactory for use
and Zn 213.8 nm in this method by proceeding as directed in 14.1.1-14.1.3.
12. Concentration Range NOTE 1—Optimum settings for the operating parameters of the atomic
absorption spectrophotometer vary from instrument to instrument.
12.1 The concentration range for each element must be
determined experimentally because the optimum range will 14.1.1 Minimum Response— Calculate the difference be-
tween the readings of the two highest of five equally spaced
depend upon the individual instrument. Determine the appro-
priate concentration range of each element as follows: (16.2) calibration solutions. This difference must be at least 40
12.1.1 Prepare a dilute standard solution as directed in scale units.
Section 16. Refer to 16.1 for suggested initial concentrations.
NOTE 2—The scale unit is defined as the smallest numerical interval
12.1.2 Prepare the instrument for use as directed in 18.1.
that is estimated in taking each reading on the instrument. If the scale is
Measure the instrument response while aspirating water, the
non-linear, the largest unit defined in this manner is used.
calibration solution with the lowest concentration, and the two
14.1.2 Curve Linearity— Calculate the difference between
with the highest concentrations. Determine the minimum
the scale readings obtained with water and the lowest of the
response and the curve linearity as directed in 14.1.1 and
five equally spaced calibration solutions. If necessary, convert
14.1.2, respectively.
this difference and the difference calculated in 14.1.1 to
12.1.3 If the instrument meets or surpasses the minimum
absorbance. Divide the difference for the highest interval by
response and curve linearity criteria, the initial concentration
range may be considered suitable for use. In this case proceed that for the lowest interval. If this ratio is not 0.70 or greater,
as directed in 12.1.5. proceed as directed in 12.1.4.
E37 − 05 (2011)
14.1.3 Minimum Stability—If the variability of the readings concentrations equal to that of the corresponding test solution,
of the highest calibration solution and of water is not less than dilute to volume, and mix. Do not use solutions that have stood
1.8 % and 1.4 %, respectively, as calculated below, proceed as more than 24 h.
directed in 12.1.5.
17. Procedure
¯
100 ~C 2 C!
(
Œ
V 5 (1) 17.1 Test Solution:
C
¯ n 2 1
C
17.1.1 Transfer a 10 g sample, weighed to the nearest 10
mg, to a 300-mL Erlenmeyer flask (Note 3). Add 3 mL of
¯
100 ~O 2 O!
(
ΠHNO and 15 mL of HClO , and heat until dissolution is
V 5 (2)
o 3 4
¯ n 2 1
C
complete. Evaporate to strong fumes of perchloric acid and
cool.
where:
V = percent variability of the highest calibration
NOTE 3—Due to the limited solubility of silver chloride, the silver
C
concentration in the sample solution should be less than 1 mg/100 mL. If
readings,
¯ the expected silver concentration is higher than 0.01 %, choose a sample
C = average absorbance value for the highest cali-
weight that limits the silver concentration to less than 1 mg/100 mL.
bration solution,
¯
∑ (C−X) = sum of the squares of the n differences be- 17.1.2 Add 50 mL of water and, while swirling, heat to
tween the absorbance readings of the highest boiling.Add 25 mL of HCl. If less than a 10-g sample is used,
calibration solution and their average,
add 20 mL HCl plus 0.5 mL for each gram of sample used.
V = percent variability of the readings on water
Heat again to boiling and cool to room temperature.
O
¯
relative to C,
17.1.3 Transfer the solution and precipitate to a 100-mL
¯
O = average absorbance value of water,
volumetric flask, dilute to volume with water, and mix thor-
¯
∑(O−O) = sumofthesquaresofthendifferencebetween
oughly. Allow the precipitated lead chloride to settle. Use the
the absorbance readings of water and their
supernatant solution, or dilute an appropriate aliquot of the
average, and
supernatant solution to provide a concentration of the element
n = number of determinations, three or more.
being measured which lies within the concentration range
determined in Section 12.
15. Reagents
17.2 Reagent Blank Solution—Prepare a reagent blank by
15.1 Bismuth, Standard Solution (1 mL = 1 mg Bi)—
adding 3 mL of HNO and 15 mL of HClO to a 300-mL
3 4
Transfer1gof bismuth (purity: 99.9 % min) to a 400-mL
Erlenmeyer flask and proceed as directed in 17.1.
beaker and dissolve in 50 mL of HNO (1 + 1), heating gently
if necessary. When dissolution is complete, cool, transfer to a
18. Measurement
1-L volumetric flask, add 100 mL of HNO (1 + 1), dilute to
18.1 Instrument Adjustment—Optimize the response of the
volume, and mix. Store in a polyethylene bottle.
instrument as directed in 18.1.1-18.1.4.
15.2 Copper, Standard Solution (1 mL = 1 mg Cu)—
18.1.1 Set the instrument parameters approximately at the
Proceedasdirectedin15.1,butsubstitute1gofcopper(purity:
values obtained in 14.1, and light the burner.
99.9 % min) for the bismuth.
18.1.2 Adjust the instrument to the approximate wavelength
15.3 Silver, Standard Solution (1 mL = 1 mg Ag)—Proceed
for the element to be determined, permit the instrument to
as directed in 15.1 but substitute1gof silver (purity: 99.9 % reach thermal equilibrium, and complete the wavelength ad-
min) for the bismuth.
justment to obtain maximum absorption while aspirating the
highest calibration solution.
15.4 Zinc, Standard Solution (1 mL = 0.1 mg Zn)—Proceed
18.1.3 Optimize fuel, air, and burner adjustments while
as directed in 15.1 but substitute 0.1 g of zinc (purity: 99.9 %
aspirating the highest calibration solution.
min) for the bismuth.
18.1.4 Aspirate water long enough to establish that the
absorbance reading is stable and then set the initial reading
16. Calibration
(approximately zero absorbance or 100 % transmittance).
16.1 Dilute Standard Solution—Using pipets, transfer to
18.2 Photometry:
500-mL volumetric flasks the following volumes of each
18.2.1 Aspirate the test solution and note, but do not record
standard solution: bismuth, 20 mL; copper, 10 mL; silver, 5
the reading.
mL; and zinc, 10 mL. Dilute to volume and mix. Adjust the
concentration of a dilute standard solution if the proper range
NOTE 4—Avoid transferring particles of precipitated lead chloride that
is not obtained when the 5, 10, 15, 20, and 25-mL portions are may clog the aspirator during the measurements of the test solution.
diluted to 100 mL and tested.
18.2.2 Aspirate water until the initial reading is again
16.2 Calibration Solutions—Prepare five calibration solu- obtained.Aspirate the calibration solutions and test solution in
order of increasing instrument response, starting with the
tions for each element to be determined. Using pipets, transfer
5, 10, 15, 20, and 25-mL portions of the appropriate dilute reagent blank. When a stable response is obtained for each
solution, record the reading.
standard solution to 100-mL volumetric flasks. Add sufficient
volumes of HCl and HClO to each flask to yield final acid 18.2.3 Proceed as directed in 18.2.2 at least twice more.
E37 − 05 (2011)
19. Calculations ANTIMONY BY THE RHODAMINE-B
PHOTOMETRIC METHOD
19.1 Calculate the variability of the readings for water and
the highest calibration solution as directed in 14.1.3 to deter-
21. Scope
mine whether they are less than 1.4 % and 1.8 %, respectively.
21.1 This test method covers the determination of antimony
If they are not, disregard the data, readjust the instrument, and
in pig lead in concentrations from 0.0008 to 0.005 %.
proceed again as directed in 18.2.
19.2 If necessary, convert the average of the readings for
22. Summary of Test Method
each calibration solution to absorbance. Calculate the net
22.1 After nitric acid dissolution of the sample, lead is
absorbanceofthetestsolutionbysubtractingtheabsorbanceof
separated as the sulfate.Antimony is oxidized with sulfatoceric
the reagent blank solution.
acid and extracted into isopropyl ether; rhodamine-B is added
19.3 Prepare a calibration curve by plotting the absorbance
and photometric measurement is made at approximately 550
values for the calibration solutions against milligrams of the
nm.
elements per millilitre.
19.4 Convert the net absorbance value of the test solution to 23. Concentration Range
milligrams of the element per millilitre by means
...
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