ASTM E1277-96
(Test Method)Standard Test Method for Chemical Analysis of Zinc-5% Aluminum-Mischmetal Alloys by ICP Emission Spectrometry
Standard Test Method for Chemical Analysis of Zinc-5% Aluminum-Mischmetal Alloys by ICP Emission Spectrometry
SCOPE
1.1 This test method covers the chemical analysis of zinc alloys having chemical compositions within the following limits: Element Concentration Range, % Aluminum 3.0-8.0 Antimony 0.002 max Cadmium 0.025 max Cerium 0.03-0.10 Copper 0.10 max Iron 0.10 max Lanthanum 0.03-0.10 Lead 0.026 max Magnesium 0.05 max Silicon 0.015 max Tin 0.002 max Titanium 0.02 max Zirconium 0.02 max
1.2 Included are procedures for elements in the following concentration ranges: Element Concentration Range, % Aluminum 3.0-8.0 Cadmium 0.0016-0.025 Cerium 0.005-0.10 Iron 0.0015-0.10 Lanthanum 0.009-0.10 Lead 0.002-0.026
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 establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazards statements are given in Section 9.
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Standards Content (Sample)
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Designation: E 1277 – 96
Standard Test Method for
Chemical Analysis of Zinc-5 % Aluminum-Mischmetal Alloys
by ICP Emission Spectrometry
This standard is issued under the fixed designation E 1277; 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 E 50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals
1.1 This test method covers the chemical analysis of zinc
E 55 Practice for Sampling Wrought Nonferrous Metals for
alloys having chemical compositions within the following
Determination of Chemical Composition
limits:
E 88 Practice for Sampling Nonferrous Metals and Alloys
Element Concentration Range, %
in Cast Form for Determination of Chemical Composition
Aluminum 3.0–8.0
E 173 Practice for Conducting Interlaboratory Studies of
Antimony 0.002 max
Methods for Chemical Analysis of Metals
Cadmium 0.025 max
E 876 Practice for Use of Statistics in the Evaluation of
Cerium 0.03–0.10
Copper 0.10 max
Spectrometric Data
Iron 0.10 max
Lanthanum 0.03–0.10
3. Summary of Test Method
Lead 0.026 max
Magnesium 0.05 max
3.1 The sample is dissolved in mixed acids. The sample
Silicon 0.015 max
solution is introduced into the plasma source of an ICP
Tin 0.002 max
spectrometer and the intensities at selected wavelengths from
Titanium 0.02 max
Zirconium 0.02 max
the plasma emission spectrum are compared to the intensities at
the same wavelengths measured with calibration solutions.
1.2 Included are procedures for elements in the following
concentration ranges:
4. Significance and Use
Element Concentration Range, %
4.1 This test method for the chemical analysis of metals and
Aluminum 3.0–8.0
alloys is primarily intended to test such materials for compli-
Cadmium 0.0016–0.025
ance with compositional specifications. It is assumed that all
Cerium 0.005–0.10
Iron 0.0015–0.10 those who use this test method will be trained analysts capable
Lanthanum 0.009–0.10
of performing common laboratory procedures skillfully and
Lead 0.002–0.026
safely. It is expected that work will be performed in a properly
1.3 This standard does not purport to address all of the
equipped laboratory.
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.1 Inductively-Coupled Argon Plasma (ICP) Atomic Emis-
bility of regulatory limitations prior to use. Specific safety sion Spectrometer—The instrument is equipped with an argon-
hazards statements are given in Section 7. plasma source, a sample transport system for introducing the
test sample and calibration solutions into the plasma. The
2. Referenced Documents
monochromator or polychromator must be capable of isolating
2.1 ASTM Standards: the required wavelengths shown in Table 1 for measurement of
D 1193 Specification for Reagent Water
their intensities by a linear photometer. Multielement pro-
E 29 Practice for Using Significant Digits in Test Data to
grammed analysis including automatic data acquisition and
Determine Conformance With Specifications
computer-controlled calibration and anlaysis calculations may
be used if available, provided that, in addition to calculated
results, the instrument records intensity readings each time a
This test method is under the jurisdiction of ASTM Committee E-1 on test sample or calibration solution is presented to the instru-
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
ment.
responsibility of Subcommittee E01.05 on Zn, Sn, Pb, Be, and Other Metals.
Current edition approved Oct. 10, 1996. Published December 1996. Originally
published as E 1277 – 91. Last previous edition E 1277 – 91.
2 4
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 3.05.
3 5
Annual Book of ASTM Standards, Vol 14.02. Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1277
A
TABLE 1 Wavelengths and Instrument Conditions
6.4 Boric Acid Solution (3 g/100 mL)—Dissolve 3.0 g of
Element Wavelength Time, s No. Integ. BCor1 BCor2 boric acid (H BO ) in 100 mL of boiling water.
3 3
6.5 Cadmium, Standard Solution (1 mL = 1.00 mg Cd)—
Al 3092.7 1.0 3 . .
Cd 2265.02 .5 3 2264.46 2265.58
Transfer 1.000 g of cadmium (purity: 99.95 % min) to a
Ce 4186.6 .5 2 . .
250-mL beaker. Cover and add 40 mL of HNO (1 + 1) and 10
Fe 2599.4 .5 2 . .
La 3988.5 .5 2 3987.54 3989.06 mL of HCl. After dissolution is complete, heat to boiling to
Pb 2832.97 1.0 3 . 2833.36
remove oxides of nitrogen. Cool, transfer to a 1-L volumetric
A
The tabulated conditions were those found satisfactory on one instrument.
flask, add 240 mL of HCl, dilute to volume, and mix. Store in
Wavelengths are expressed in angstroms. Time = seconds for each integration,
a polyethylene bottle.
No. Integ. = number of integrations averaged for each reading, and BCor1 and
BCor2 are off-peak background correction wavelengths. 6.6 Cerium, Standard Solution A (1 mL = 1.00 mg Ce)—
Dry ceric ammonium nitrate ((NH ) Ce(NO ) , also known as
4 2 3 6
ammonium hexanitrato cerate) (purity: 99.95 % min) for4hat
85°C and cool to room temperature in a desiccator. Dissolve
NOTE 1—All elements (including aluminum) are calibrated as linear
3.913 g of dry ceric ammonium nitrate in 100 mL of HCl
functions of intensity. If the instrument cannot be set to measure
aluminum and ignore other elements in calibration solutions No. 1 and No. (1 + 9). Transfer to a 1-L volumetric flask, add 240 mL of HCl
4, then a separate determination of aluminum must be made using
and 20 mL of HNO , dilute to volume, and mix. Store in a
calibration solutions No. 1, No. 2 and No. 4. The other elements can then
polyethylene bottle.
be determined together in another run using only calibration solutions No.
6.7 Cerium, Standard Solution B (1 mL = 0.010 mg Ce)—
2 and No. 3. Use the calibration solutions prepared in 10.1 in determining
Using a pipet, transfer 1.00 mL of Cerium Standard Solution A
the instrument settings for the elements in this matrix. Follow the
to a 100-mL volumetric flask. Dilute to volume with dilution
manufacturer’s instructions to set the wavelengths and parameters to
solution and mix.
provide as large a difference between the intensity readings for the high
6.8 Dilution Solution—Half fill a 2-L volumetric flask with
and low calibration concentrations as is consistent with stable instrument
readings. If there is a question of linearity of the instrument’s response water. Add 500 mL of HCl and 40 mL of HNO , swirl to mix,
over the range of solution concentrations given, a third standard, equidis-
dilute to the mark, and mix.
tant between the two listed standards, must be measured to verify linearity.
6.9 Iron, Standard Solution A (1 mL = 1.00 mg Fe)—
Transfer 1.000 g of iron (purity: 99.95 % min) to a 250-mL
6. Reagents
beaker, cover, and add 100 mL of HCl (1 + 1). Boil gently to
complete dissolution. Cool and transfer to a 1-L volumetric
6.1 Purity of Reagents—Unless otherwise indicated, all
flask, add 200 mL of HCl and 20 mL of HNO , dilute to
reagents used in this test method shall conform to the “Reagent
volume, and mix. Store in the polyethylene bottle.
Grade” Specifications of the American Chemical Society.
6.10 Iron, Standard Solution B (1 mL = 0.010 mg Fe)—
Other chemicals may be used provided that it is first ascer-
Using a pipet, transfer 1.00 mL of Iron Standard Solution A to
tained that the reagent used is of sufficiently high purity to
a 100-mL volumetric flask. Dilute to volume with dilution
permit its use without lessening the accuracy of the determi-
solution and mix.
nation.
6.11 Lanthanum, Standard Solution A (1 mL = 0.010 mg
6.2 Purity of Water—Unless otherwise indicated, references
La)—Ignite lanthanum oxide (La O ) (purity: 99.9 % min) for
2 3
to water shall be understood to mean reagent water as defined
1 h at 1000°C and cool to room temperature in a desiccator.
by Type II of Specification D 1193.
Dissolve 1.173 g of dry lanthanum oxide in 100 mL of HCl
6.3 Aluminum, Standard Solution (1 mL = 20.0 mg Al)—
(1 + 9) and transfer to a 1-L volumetric flask. Add 240 mL of
Transfer 2.0000 g of aluminum (purity: 99.999 % min) to a
HCl and 20 mL of HNO , dilute to volume, and mix. Store in
250-mL beaker. Cover, add 50 mL of HCl (1 + 1) and a small
a polyethylene bottle.
crystal of mercuric nitrate. Heat gently to accelerate the
6.12 Lanthanum, Standard Solution B (1 mL = 0.010 mg
reaction, but avoid temperatures high enough to cause a
La)—Using a pipet, transfer 1.00 mL of Lanthanum Standard
noticeable volume loss. If the reaction slows, add more
Solution A to a 100-mL volumetric flask. Dilute to volume with
mercuric salt as needed. A number of hours may be required to
dilution solution and mix.
complete the dissolution (only a small droplet of mercury will
6.13 Lead, Standard Solution (1 mL = 1.00 mg Pb)—
remain undissolved). Transfer the solution to a 100-mL volu-
Transfer 1.000 g of lead (purity: 99.9 % min) to a 250-mL
metric flask, dilute to volume, and mix. Store in a polyethylene
beaker, cover, and add 40 mL of HNO (1 + 1). Boil gently to
bottle. complete dissolution and to remove oxides of nitrogen. Cool,
transfer to a 1-L volumetric flask, add 250 mL of HCl, dilute to
volume, and mix. Store in a polyethylene bottle.
6.14 Zinc Matrix Solution (50 mL = 3.75 g Zinc Matrix
Reagent Chemicals, American Chemical Society Specifications, American
Standard)—Transfer 18.75 g 6 0.10 g of Zinc Matrix Standard
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
to a 250-mL plastic beaker. Cover and add about 50 mL of
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
water. Add 62.5 mL of HCl and heat enough to maintain the
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
reaction but not enough to evaporate the solution. When most
MD.
of the material has dissolved, add 5.0 mL of HNO . When all
solids have dissolved, remove from the heat and allow to cool.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 1277
A,B
TABLE 4 Concentration Table for Calibration Solutions
Transfer to a 250-mL plastic volumetric flask, dilute to the
mark, and mix. Element No. 1 No. 2 No. 3 No. 4
6.15 Zinc Matrix Standard—Use a zinc reference material
Aluminum 3.00 5.50 . 8.00
Cadmium . .00011 .0251 .
of known composition with respect to the elements listed in the
Cerium . .00050 .1000 .
scope of this test method.
Iron . .00052 .1003 .
Lanthanum . .00050 .1000 .
7. Hazards
Lead . .00104 .0260 .
A
7.1 For precautions to be observed in the use of certain The values in this table assume SRM 728 as zinc matrix, a sample weight of
4.00 g, and results reported in %.
reagents in this test method, refer to Practices E 50.
B
To calculate the concentration table for a different zinc matrix material, add the
parts per million contributed from 3.75 g of that material in a volume of 100 mL to
8. Sampling the parts per million shown in Table 3. Calculate the percent element by dividing
the parts per million by 400.
8.1 For procedures for sampling the material, refer to
Practices E 55 and E 88.
728 as Zinc Matrix Standard. If a different Zinc Matrix
9. Interlaboratory Studies and Rounding of Calculated Standard is used, Table 4 must be revised to reflect the different
composition of that material. Using the calibration solutions,
Values
follow the manufacturer’s procedure to perform the instrument
9.1 Only four laboratories were available to test this
calibration at the wavelengths specified in Table 1. Without
method, therefore, the interlaboratory test does not comply
undue delay, proceed in accordance with 11.2.
with the protocol for Practice E 173. However, the statistics
10.5 Nonautomatic Mode—No separate calibration run is
were calculated according to Practice E 173.
required if intensity readings only are recorded. Set up the
9.2 Calculated values shall be rounded to the desired num-
instrument to measure intensities at the wavelengths specified
ber of places as directed in 3.4 to 3.6 of Practice E 29.
in Table 1 according to the manufacturer’s instructions and
proceed to 11.3 .
10. Calibration
10.1 Prepare calibration and test sample solutions before
A,B
TABLE 2 Standard Solution Volumes Added, mL
calibration measurements are started.
Element No. 1 No. 2 No. 3 No. 4
10.2 Calibration Solutions—All calibration solutions con-
B
Aluminum 6.00 11.0 11.0 16.0
tain the same concentration of zinc as the test sample solutions.
Cadmium . . 1.00 .
The aluminum content of calibration solutions No. 2 and No. 3
Cerium . 2.00(B) 4.00(A) .
must be equal to the midpoint of the calibrated aluminum
Iron . 1.00(B) 4.00(A) .
Lanthanum . 2.00(B) 4.00(A) .
range. Using a pipet, transfer 50.0 mL of the Zinc Matrix
Lead . . 1.00 .
Solution into each of four 100-mL plastic volumetric flasks
A
Use standard solution A or B as indicated in parentheses.
marked Cal No. 1 through Cal No. 4. Add the volumes of
B
Added to match solution No. 2, not for calibration purposes.
standard solutions specified in Table 2 (also see Table 3), dilute
to volume with dilution solution, and mix:
A
TABLE 3 Solution Concentrations Added, mg/L
10.3 Test Sample Solution—Transfer a 3.8 to 4.2-g portion
Element No. 1 No. 2 No. 3 No. 4
of the test sample weighed to the nearest 0.02 g to a 250-mL
Aluminum 1200 2200 . 3200
polytetrafluoroethylene beaker. Add about 30 mL of water,
Cadmium . . 10.0 .
cover, and cautiously add 25 mL of HCl in increments. Heat
Cerium . 0.2 40.0 .
gently to maintain the reaction, if necessary, but do not boil. Iron . 0.1 40.0 .
Lanthanum . 0.2 40.0 .
When most of the material has dissolved, add 2.0 mL of HNO ,
Lead . . 10.0 .
let the solution cool for about 20 min, transfer to a 100-mL
A
Table 4 is derived from this table by adding the trace element contributions
plastic volumetric flask, dilute to volume, and mix.
from the zinc matrix solution t
...
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