ASTM E37-00
(Test Method)Standard Test Methods for Chemical Analysis of Pig Lead
Standard Test Methods for Chemical Analysis of Pig Lead
SCOPE
1.1 These test methods cover the chemical analysis of pig lead having chemical compositions within the following limits: ElementConcentration Range, %Antimony0.001 to 0.02Arsenic0.0005 to 0.02Bismuth0.002 to 0.2Copper0.001to 0.1Iron0.0005to 0.005Lead99.5to 99.99Silver0.001to 0.03Tin0.001to 0.02Zinc0.001to 0.005
1.2 The test methods appear in the following order: SectionsAntimony by the Rhodamine-B Photometric Method19-28Copper, Bismuth, Silver, and Zinc by the Atomic Absorption Method 8-18
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 consult and 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. Specific hazard statements are given in the individual test methods.
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Designation:E37–00
Standard Test Methods for
Chemical Analysis of Pig Lead
ThisstandardisissuedunderthefixeddesignationE 37;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals
1.1 These test methods cover the chemical analysis of pig
E 60 Practice for Photometric and Spectrophotometric
lead having chemical compositions within the following limits:
Methods for Chemical Analysis of Metals
Element Concentration Range, %
E 173 Practice for Conducting Interlaboratory Studies of
Antimony 0.001 to 0.02
Methods for Chemical Analysis of Metals
Arsenic 0.0005 to 0.02
Bismuth 0.002 to 0.2
Copper 0.001 to 0.1
3. Significance and Use
Iron 0.0005 to 0.005
3.1 These test methods for the chemical analysis of metals
Lead 99.5 to 99.99
Silver 0.001 to 0.03
and alloys are primarily intended to test such materials for
Tin 0.001 to 0.02
compliance with compositional specifications. It is assumed
Zinc 0.001 to 0.005
that all who use these methods will be trained analysts capable
1.2 The test methods appear in the following order:
of performing common laboratory procedures skillfully and
Sections
safely. It is expected that work will be performed in a properly
Antimony by the Rhodamine-B Photometric Method 19-28
equipped laboratory.
Copper, Bismuth, Silver, and Zinc by the Atomic Absorption
Method 8-18
4. Apparatus, Reagents, and Photometric Practice
1.3 This standard does not purport to address all of the
4.1 Apparatus and reagents required for each determination
safety concerns, if any, associated with its use. It is the
are listed in separate sections of each test method. The
responsibility of the user of this standard to consult and
apparatus, standard solutions, and certain other reagents used
establish appropriate safety and health practices and deter-
in more than one procedure are referred to by number and shall
mine the applicability of regulatory limitations prior to use.
conform to the requirements prescribed in Practices E 50,
For precautions to be observed in the use of certain reagents,
except that photometers shall conform to the requirements
refer to Practices E 50. Specific hazard statements are given in
prescribed in Practice E 60.
the individual test methods.
5. Sampling
2. Referenced Documents
5.1 For procedures for sampling the material, refer to
2.1 ASTM Standards:
Specification B 29.
B 29 Specification for Pig Lead
E 29 Practice for Using Significant Digits in Test Data to
6. Rounding Calculated Values
Determine Conformance With Specifications
6.1 Calculated values shall be rounded to the desired num-
ber of places as directed in 3.4 to 3.6 of Practice E 29.
7. Interlaboratory Studies
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
7.1 These test methods have been evaluated in accordance
responsibility of Subcommittee E01.05 on Zinc, Tin, Lead, Cadmium, Beryllium
with Practice E 173, unless otherwise noted in the precision
and Other Metals.
Current edition approved Nov. 10, 2000. Published February 2001. Originally section.
published as E 37 – 42 T. Last previous edition E 37 – 95.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E37
COPPER, BISMUTH, SILVER, AND ZINC BY THE Bi 223.0, Ag 328.0, and Zn 213.8 nm. Aspirate the solutions
ATOMIC ABSORPTION METHOD into an air-acetylene flame of a premix burner. Determine that
the atomic absorption spectrophotometer is satisfactory for use
8. Scope
in this method by proceeding as directed in 12.1.1-12.1.3.
8.1 This test method covers the determination of bismuth in
NOTE 1—Optimum settings for the operating parameters of the atomic
concentrations from 0.002 to 0.2 %, copper from 0.001 to
absorption spectrophotometer vary from instrument to instrument.
0.1 %, silver from 0.001 to 0.03 %, and zinc from 0.001 to
0.005 %.
12.1.1 Minimum Response— Calculate the difference be-
tween the readings of the two highest of five equally spaced
9. Summary of Test Method
(14.2) calibration solutions. This difference must be at least 40
9.1 The sample is dissolved in a nitric-perchloric acid
scale units.
mixture, the solution is fumed, and hydrochloric acid is added
NOTE 2—The scale unit is defined as the smallest numerical interval
to precipitate lead chloride. The hydrochloric-perchloric acid
that is estimated in taking each reading on the instrument. If the scale is
solution is aspirated into the air-acetylene flame of an atomic
non-linear, the largest unit defined in this manner is used.
absorption spectrophotometer. The absorption of the resonance
line energy from the spectrum of each element is measured and
12.1.2 Curve Linearity— Calculate the difference between
compared with that of calibration solutions of the same
the scale readings obtained with water and the lowest of the
element. The lines used were Cu 3247, Bi 2230,Ag 3280, and
five equally spaced calibration solutions. If necessary, convert
Zn 2138 Å.
this difference and the difference calculated in 12.1.1 to
absorbance. Divide the difference for the highest interval by
10. Concentration Range
that for the lowest interval. If this ratio is not 0.70 or greater,
10.1 The concentration range for each element must be
proceed as directed in 10.1.4.
determined experimentally because the optimum range will
12.1.3 Minimum Stability—If the variability of the readings
depend upon the individual instrument. Determine the appro-
of the highest calibration solution and of water is not less than
priate concentration range of each element as follows:
1.8 % and 1.4 %, respectively, as calculated below, proceed as
10.1.1 Prepare a dilute standard solution as directed in
directed in 10.1.5.
Section 14. Refer to 14.1 for suggested initial concentrations.
¯
10.1.2 Prepare the instrument for use as directed in 16.1.
100 (~C – C!
V 5 Π(1)
C
Measure the instrument response while aspirating water, the
¯ n–1
C
calibration solution with the lowest concentration, and the two
¯
100 (~O – O!
with the highest concentrations. Determine the minimum
V 5
Œ
o
¯ n–1
C
response and the curve linearity as directed in 12.1.1 and
12.1.2, respectively.
where:
10.1.3 If the instrument meets or surpasses the minimum
V = percent variability of the highest calibration
C
response and curve linearity criteria, the initial concentration
readings,
range may be considered suitable for use. In this case proceed
¯
C = average absorbance value for the highest
as directed in 10.1.5.
calibration solution,
10.1.4 If the minimum response is not achieved, prepare 2
¯
( (C−X) = sum of the squares of the n differences
another dilute standard solution to provide a higher concentra-
between the absorbance readings of the high-
tionrange,andrepeat10.1.2and10.1.3.Ifthecalibrationcurve
est calibration solution and their average,
does not meet the linearity criterion, prepare another dilute
V = percent variability of the readings on water
O
standard solution to provide a lower concentration range, and
¯
relative to C,
repeat 10.1.2 and 10.1.3. If a concentration range cannot be
¯
O = average absorbance value of water,
found for which both criteria can be met, do not use this
( (O − = sum of the squares of the n difference be-
method until the performance of the apparatus has been ¯
O) tween the absorbance readings of water and
improved.
their average, and
10.1.5 Perform the stability test as directed in 12.1.3. If
n = number of determinations, three or more.
either of the minimum stability requirements is not met, do not
use this method until the repeatability of the readings has been
13. Reagents
suitably improved.
13.1 Bismuth, Standard Solution (1 mL = 1.00 mg Bi)—
Transfer 1.00 g of bismuth (purity: 99.9 % min) to a 400-mL
11. Interferences
beaker and dissolve in 50 mL of HNO (1 + 1), heating gently
11.1 Elements ordinarily present do not interfere if their
if necessary. When dissolution is complete, cool, transfer to a
concentrations are under the maximum limits shown in 1.1.
1-L volumetric flask, add 100 mL of HNO (1 + 1), dilute to
12. Apparatus volume, and mix. Store in a polyethylene bottle.
12.1 Atomic Absorption Spectrophotometer—Use hollow- 13.2 Copper, Standard Solution (1 mL = 1.00 mg Cu)—
Proceed as directed in 13.1, but substitute 1.00 g of copper
cathode lamps, operated in accordance with manufacturers’
recommendations as sources for the following lines: Cu 324.7, (purity: 99.9 % min) for the bismuth.
E37
13.3 Silver, Standard Solution (1 mL = 1.00 mg Ag)— 16.1.3 Optimize fuel, air, and burner adjustments while
Proceed as directed in 13.1 but substitute 1.00 g of silver aspirating the highest calibration solution.
(purity: 99.9 % min) for the bismuth.
16.1.4 Aspirate water long enough to establish that the
13.4 Zinc, Standard Solution (1 mL = 0.100 mg Zn)— absorbance reading is stable and then set the initial reading
Proceed as directed in 13.1 but substitute 0.100 g of zinc
(approximately zero absorbance or 100 % transmittance).
(purity: 99.9 % min) for the bismuth.
16.2 Photometry:
16.2.1 Aspirate the test solution and note, but do not record
14. Calibration
the reading.
14.1 Dilute Standard Solution—Using pipets, transfer to
NOTE 4—Avoid transferring particles of precipitated lead chloride that
500-mL volumetric flasks the following volumes of each
may clog the aspirator during the measurements of the test solution.
standard solution: bismuth, 20 mL; copper, 10 mL; silver, 5
mL; and zinc, 10 mL. Dilute to volume and mix. Adjust the
16.2.2 Aspirate water until the initial reading is again
concentration of a dilute standard solution if the proper range
obtained.Aspirate the calibration solutions and test solution in
is not obtained when the 5, 10, 15, 20, and 25-mL portions are
order of increasing instrument response, starting with the
diluted to 100 mL and tested.
reagent blank. When a stable response is obtained for each
14.2 Calibration Solutions—Prepare five calibration solu-
solution, record the reading.
tions for each element to be determined. Using pipets, transfer
16.2.3 Proceed as directed in 16.2.2 at least twice more.
5, 10, 15, 20, and 25-mL portions of the appropriate dilute
standard solution to 100-mL volumetric flasks. Add sufficient
17. Calculations
volumes of HCl and HClO to each flask to yield final acid
17.1 Calculate the variability of the readings for water and
concentrations equal to that of the corresponding test solution,
the highest calibration solution as directed in 12.1.3 to deter-
dilute to volume, and mix. Do not use solutions that have stood
mine whether they are less than 1.4 % and 1.8 %, respectively.
more than 24 h.
If they are not, disregard the data, readjust the instrument, and
15. Procedure proceed again as directed in 16.2.
17.2 If necessary, convert the average of the readings for
15.1 Test Solution:
each calibration solution to absorbance. Calculate the net
15.1.1 Transfer a 10.0-g sample, weighed to the nearest 10
absorbanceofthetestsolutionbysubtractingtheabsorbanceof
mg, to a 300-mLErlenmeyer flask (Note 3).Add 3 mLof HNO
the reagent blank solution.
3 and 15 mL of HClO , and heat until dissolution is complete.
17.3 Prepare a calibration curve by plotting the absorbance
Evaporate to strong fumes of perchloric acid and cool.
values for the calibration solutions against milligrams of the
NOTE 3—Due to the limited solubility of silver chloride, the silver
elements per millilitre.
concentration in the sample solution should be less than 1 mg/100 mL. If
17.4 Convert the net absorbance value of the test solution to
the expected silver concentration is higher than 0.01 %, choose a sample
milligrams of the element per millilitre by means of the
weight that limits the silver concentration to less than 1 mg/100 mL.
appropriate calibration curve.
15.1.2 Add 50 mL of water and, while swirling, heat to
17.5 Calculate the percentage of the element as follows
boiling.Add 25 mL of HCl. If less than a 10-g sample is used,
(Note 5):
add 20 mL HCl plus 0.5 mL for each gram of sample used.
Heat again to boiling and cool to room temperature. Element, % 5 @~A 3 B 3 0.977!/C# 3 100 (2)
15.1.3 Transfer the solution and precipitate to a 100-mL
where:
volumetric flask, dilute to volume with water, and mix thor-
A = milligrams of element per millilitre,
oughly. Allow the precipitated lead chloride to settle. Use the
B = final volume of test solution in millilitres, and
supernatant solution, or dilute an appropriate aliquot of the
C = milligrams of sample represented in final volume of
supernatant solution to provide a concentration of the element
test solution.
being measured which lies within the concentration range
determined in Section 10. NOTE 5—The factor 0.977 is used to compensate for the volume error
in the 100 mL of final test solution caused by the 13.1 g of lead chloride
15.2 Reagent Blank Solution—Prepare a reagent blank by
precipitate. If less than 10 g of sample is used, calculate and apply an
adding 3 mL of HNO and 15 mL of HClO to a 300-mL
3 4
appropriate factor.
Erlenmeyer flask and proceed as directed in 15.1.
18. Precision and Bias
16. Photometry
18.1 Seven laboratories cooperated in testing this method,
16.1 Instrument Adjustment—Optimize the response of the
with one laboratory reporting a second pair of values; the data
instrument as directed in 16.1.1-16.1.4.
are summarized in Table 1.
16.1.1 Set the instrument parameters approximately at the
values obtained in 12.1, and light the burner. 18.2 The accuracy of this method could not be evaluated
16.1.2 Adjust the instrument to the approximate wavelength because adequate certified standard reference materials were
for the element to be determined, permit the instrument to unavailable at the time of testing. The user is cautioned to
reach thermal equilibrium, and complete the wavelength ad- verify by the use of certified reference materials, if available,
justment to obtain maximum absorption while aspirating the that the accuracy of this method is adequate for the contem-
highest calibration solution. plated use.
E37
TABLE 1 Statistical Information
phases to separate and discard the aqueous phase. Repeat one
Repe
...
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