ASTM E1834-96(2002)
(Test Method)Standard Test Method for Determination of Lead in Nickel Alloys by Electrothermal Atomic Absorption Spectrometric Method
Standard Test Method for Determination of Lead in Nickel Alloys by Electrothermal Atomic Absorption Spectrometric Method
SIGNIFICANCE AND USE
This test method is intended to be used for the determination of trace levels of lead in nickel and nickel alloys. It is assumed that the procedure will be performed by trained analysts capable of performing common laboratory practices skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and proper waste disposal procedures will be followed.
SCOPE
1.1 This test method covers the determination of lead in nickel and nickel alloys in the concentration range of 0.00005 % to 0.001 % by electrothermal atomic absorption spectrometry.
Note 1—If this test method is used to test materials having contents less than 0.0001 % lead, users in different laboratories will experience more than the usual 5 % risk that their results will differ by more than 50 % relative error.
1.2 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. For specific hazards associated with the use of this practice see Practices E 50.
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Standards Content (Sample)
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Designation:E1834–96 (Reapproved 2002)
Standard Test Method for
Determination of Lead in Nickel Alloys by Electrothermal
Atomic Absorption Spectrometric Method
This standard is issued under the fixed designation E 1834; 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 Trace-Element Content–Electrothermal Atomic Absorp-
tion Spectrometric Method–Part 2: Determination of Lead
1.1 This test method covers the determination of lead in
Content
nickel and nickel alloys in the concentration range of
ISO Guide 5725–Accuracy, Trueness, and Precision of
0.00005 % to 0.001 % by electrothermal atomic absorption
Measurements, Methods and Results
spectrometry.
NOTE 1—If this test method is used to test materials having contents 3. Summary of Test Method
less than 0.0001 % lead, users in different laboratories will experience
3.1 The sample is dissolved in a mixture of nitric acid,
more than the usual 5 % risk that their results will differ by more than
hydrofluoric acid, and water. The sample and a nickel-
50 % relative error.
ammonium phosphate matrix modifier are injected into the
1.2 This standard does not purport to address all of the
electrothermal atomizer of an atomic absorption spectrometer,
safety concerns, if any, associated with its use. It is the
which is provided with a background corrector. Measurement
responsibility of the user of this standard to establish appro-
of the absorbance is made at a wavelength of 283.3 nm. The
priate safety and health practices and determine the applica-
lead concentration is determined from a calibration curve
bility of regulatory limitations prior to use.Forspecifichazards
established with nickel solutions containing a known amount
associated with the use of this practice see Practices E 50.
of lead.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
4.1 This test method is intended to be used for the determi-
E 50 Practices for Apparatus, Reagents, and Safety Precau-
nation of trace levels of lead in nickel and nickel alloys. It is
tions for Chemical Analysis of Metals, Ores, and Related
assumed that the procedure will be performed by trained
Materials
analysts capable of performing common laboratory practices
E 1184 Practice for Electrothermal (Graphite Furnace)
skillfully and safely. It is expected that the work will be
Atomic Absorption Analysis
performed in a properly equipped laboratory and proper waste
E 1452 Practice for Preparation of Calibration Solutions for
disposal procedures will be followed.
Spectrophotometric and Spectroscopic Atomic Analysis
E 1601 Practice for Conducting an Interlaboratory Study to
5. Apparatus
Evaluate the Performance of an Analytical Method
5.1 Atomic Absorption Spectrometer, with electrothermal
E 1770 Practice for Optimization of ElectrothermalAtomic
atomizer,equippedwithanappropriatebackgroundcorrector,a
Absorption Spectrometric Equipment
signal output device, such as a video display screen, a digital
2.2 ISO Standards:
computer, a printer or strip chart recorder, and an autosampler.
ISO Standard 11437–Nickel Alloys–Determination of
5.2 Pyrolytically Coated Graphite Tubes, grooved, con-
forming to the instrument manufacturer’s specifications.
5.3 Pyrolytic Graphite Platforms, L’vov design, fitted to the
This test method is under the jurisdiction of ASTM Committee E01 on
tubes specified in 5.2.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
5.4 Radiation Source, lead hollow cathode lamp, or elec-
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys.
Current edition approved Oct. 10, 1996. Published December 1996.
trodeless discharge lamp with an appropriate power supply.
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 Available from American National Standards Institute, 25 W. 43rd St., 4th
the ASTM website. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1834–96 (2002)
6. Instrument Parameters and Criteria 7.5 Nickel, Solution (5.0 g/L)—Transfer 10.0 mL of the
Nickel Stock Solution to a 100 mL volumetric flask. Dilute to
6.1 The atomic absorption spectrometer and electrothermal
the mark with water and mix.
atomizer are satisfactory if after adjustment of the instruments
7.6 Nickel Nitrate-Ammonium Phosphate Matrix Modifier
and optimization of the furnace heating program as described
Solution—Dissolve 6.0 6 0.1 g high purity ammonium dihy-
in Practice E 1770, they meet the criteria given in 6.4-6.7.
drogenphosphate(NH H PO )in50mLwater.Transferto100
4 2 4
6.2 Calibration solutions S through S prepared in accor-
0 3
mL volumetric flask and add 20 mL of nickel solution (7.5).
dance with 7.9 and summarized in Table 1 shall be used for
Dilute with water and mix. This solution shall be freshly
testing criteria.
prepared.
6.3 The parameters for the determination of lead and the
7.7 Lead Reference Solution (100 mg/L)—Dissolve0.100 6
establishing of the instrument criteria are as follows:
0.001 g of lead metal (99 % minimum purity) in 20 mL nitric
6.3.1 The injection volume is 20 µL.
acid (1:1) in a 250-mL beaker. Heat to assist dissolution. Cool
6.3.2 The peak area absorbance integration measurements
and transfer to 1-L volumetric flask, dilute to mark with water
shall be at a wavelength of 283.3 nm.
and mix. Store in polypropylene or high density polyethylene
6.4 Characteristic Mass—The characteristic mass deter-
bottle.
minedinaccordancewithPracticeE 1770shallbewithin20 %
7.8 Lead Standard Solution (1.0 mg/L)—Pipette 10.0 mLof
of that given in the manufacturer’s literature.
the lead reference solution (7.7) into a 1-L volumetric flask.
6.5 Precision—The variability obtained from calibration
Add 20 mL nitric acid and dilute to volume with water and
solution S shall not exceed 10 % of the mean absorbance of
mix. This solution shall be freshly prepared.
the same solution, and the variability of calibration solution S
7.9 Calibration Solutions—Transfer 10.0 mL nickel solu-
shall not exceed 4 % of the mean absorbance of solution S
tion (50 g/L) to each of six 100 mL volumetric flasks. Add
when determined in accordance with Practice E 1770.
respectively 0, 1.0, 2.0, 3.0, 4.0, and 6.0 mL of lead standard
6.6 Limit of Detection—The limit of detection of lead as
solution (7.8). Dilute with water and mix. These calibration
described in Practice E 1770 shall be less than 20 pg (equiva-
solutions contain 0, 10.0, 20.0, 30.0, 40.0 and 60.0 µg Pb/L.
lent to 1.0 µg/L in the test solution or 0.2 ppm in the original
These calibration solutions shall be identified as calibration
sample).
solutions S through S , respectively (see Table 1).
6.7 Linearity—The linearity of the calibration as deter- 0 5
mined in Practice E 1770 shall not be less than 0.7.
8. Sampling and Sample Preparation
7. Reagents
8.1 Sampling and sample preparation are to be performed
7.1 Purity and Concentration of Reagents—The purity and
by procedures agreed upon between buyer and seller.
concentration of common chemical reagents shall conform to
8.2 The sampling procedure shall not involve any steps or
Practices E 50. The reagents should be free of or contain
procedures that can result in the loss or pick up of lead in the
minimal amounts (<0.01 µg/g) of lead.
sample.
7.2 Dissolution Acid Mixture—To 150 mL water carefully
NOTE 3—Sometimes a heterogeneous scrap composite is homogenized
add 150 mLnitric acid and 150 mLhydrofluoric acid. Mix and
by melting, then milling a laboratory sample from the solid. Arc melting
store in plastic bottle.
of the sample or induction melting of the sample under vacuum can result
7.3 Pure Nickel Metal—99.9 % minimum purity nickel, and
in significant loss of several elements, including lead, that have a low
shall contain less than 0.1 ppm lead. vapor pressure. Arc melting of the sample should be avoided and
induction melting should be performed only with at least a partial inert
7.4 Nickel, Stock Solution (50 g/L)—Dissolve 25 60.1gof
atmosphere.
the pure nickel in 200 mL of nitric acid (1:1) in a 600 mL
beaker. Cool the solution and transfer to a 500 mL volumetric
8.3 In most cases the laboratory sample is in the form of
flask. Dilute to the mark and mix.
homogeneous turnings, millings or drillings and no further
mechanical preparation of the sample is necessary.
NOTE 2—Iflargenickelturningsorchunksareused,gentleheatingmay
be required to complete the disso
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