ASTM E1452-92(1996)
(Practice)Standard Practice for Preparation of Calibration Solutions for Spectrophotometric and for Spectroscopic Atomic Analysis (Withdrawn 2005)
Standard Practice for Preparation of Calibration Solutions for Spectrophotometric and for Spectroscopic Atomic Analysis (Withdrawn 2005)
SCOPE
1.1 This practice covers the preparation, labeling, and storage of calibration solutions employed for calibrating atomic and molecular spectroscopic equipment used for the analysis of metals and alloys.
1.2 This standard does not purport to address all of the safety problems, 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 information, see Section 5.
WITHDRAWN RATIONALE
This practice covers the preparation, labeling, and storage of calibration solutions employed for calibrating atomic and molecular spectroscopic equipment used for the analysis of metals and alloys.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in March 2005 in accordance with section 10.6.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E 1452 – 92 (Reapproved 1996)
Standard Practice for
Preparation of Calibration Solutions for Spectrophotometric
and for Spectroscopic Atomic Analysis
This standard is issued under the fixed designation E 1452; 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 scopic instruments. Therefore, the quality of the analytical
results obtained is directly dependent on the accuracy of the
1.1 This practice covers the preparation, labeling, and stor-
calibration solutions.
age of calibration solutions employed for calibrating atomic
3.2 It is assumed that the users of this practice will be
andmolecularspectroscopicequipmentusedfortheanalysisof
trained analysts capable of performing common laboratory
metals and alloys.
procedures skillfully and safely. It is expected that the work
1.2 This standard does not purport to address all of the
will be performed in a properly equipped laboratory.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Reagents
priate safety and health practices and determine the applica-
4.1 Purity of Reagents—All reagents shall conform to the
bility of regulatory limitations prior to use.Forspecifichazards
specifications of the Committee on Analytical Reagents of the
information, see Section 5.
American Chemical Society, when such specifications are
2. Referenced Documents available. Other grades may be used if it is first ascertained
that the reagent is of sufficient purity to permit its use without
2.1 ASTM Standards:
lessening the accuracy or stability of the calibration solutions
D 1193 Specification for Reagent Water
produced. See PracticesE50.
E50 Practices for Apparatus, Reagents, and Safety Precau-
4.2 Purity of Water—Unless otherwise indicated, all water
tions for Chemical Analysis of Metals
used shall be Type II (distilled water) or water of equivalent
E 288 Specification for Laboratory Glass Volumetric
purity, in accordance with Specification D 1193.
Flasks
E 319 Practice for the Evaluation of Single-Pan Mechanical
5. Hazards
Balances
4 5.1 All safety precautions referenced in PracticeE50 shall
E 969 Specification for Volumetric (Transfer) Pipets
be observed. Generally accepted prudent laboratory practices
2.2 National Institute for Standards and Technology (NIST)
shall be followed.
Documents:
5 5.2 Calibration solutions may be subject to several federal,
Circular 602 Testing of Glass Volumetric Apparatus
state, and local laws and regulations, and may be subject to the
3. Significance and Use regulations of some fire departments.
5.3 Other laws or regulations may be applicable, depending
3.1 Analytical instrumentation is employed extensively
on the nature and concentration of the matrix and the element
throughout industry for quality control, research, and develop-
used to prepare the calibration solutions.
ment purposes. Calibration solutions are required for calibrat-
ing certain types of analytical atomic and molecular spectro-
6. Calibration of Equipment
6.1 Balances and Weights—Calibrate balances and weights
periodically, depending on use, or at least once every twelve
Precision and Bias This practice is under the jurisdiction ofASTM Committee
months. Calibration shall be traceable to NIST. See Method
E-1 on Analytical Chemistry for Metals, Ores, and Related Materials and is the
E 319.
direct responsibility of Subcommittee E01.21 on Reference Materials and Liaison
with S17.
Current edition approved Feb. 15, 1992. Published June 1992.
2 6
Annual Book of ASTM Standards, Vol 11.01. Reagent Chemicals, American Chemical Society Specifications,Am. Chemical
Annual Book of ASTM Standards, Vol 03.05. Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
Annual Book of ASTM Standards, Vol 14.02. American Chemical Society, see Rosen, J. Reagent Chemicals and Standards,D.
Available as Order No. COM 73-10504 from the National Technical Informa- Van Nostrand Co., Inc., New York, NY, and United States Pharmacopeia, United
tion Services, Springfield, VA 22161. States Pharmacopeial Convention, Inc., Rockville, MD.
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. Contact ASTM
International (www.astm.org) for the latest information.
E 1452 – 92 (1996)
6.2 Glass and Plastic Laboratory Ware—All glass and 7.4.3 The minimum weight of the analyte or analyte com-
plastic volumetric flasks and pipets shall be of Class A, pound or aliquot should be within 60.05 % relative standard
precision grade, within the tolerances established by NIST for deviation. The minimum weight of the analyte or analyte
the appropriate type of glassware. See Practices E50, Speci- compound shall be calculated from the number of places to the
fications E 288, and E 969, and NIST Circular 602. right of the decimal point that the balance is capable of
determining. Compute minimum weight, w, as follows:
7. Preparation of Calibration Solutions
2 2 1/2
w 5 [~X 1 X ! /0.05]100 (1)
1 2
7.1 General—Usually when calibrating an instrument, an
where X and X are the balance limitations for two
1 2
analyte stock solution is prepared first. From this solution
weighings.
aliquots are taken by transfer pipets or by weight, and diluted
If the balance weighs to 0.001 g and two weighings, tare and
in volumetric flasks to yield a series of calibration solutions
final, are taken, then:
which are used to calibrate an instrument in the concentration
2 2 1/2
range of interest. w 5 $@~0.001! 1 ~0.001! # /0.05%100 5 ~0.0014/0.05!100 5 2.800 g
(2)
7.1.1 Stock Solution—The concentration of analyte is suffi-
ciently high so that adsorption of the analyte on the container
7.4.4 The solution is diluted in volumetric vessels that meet
walls is negligibly small compared to the concentration of the
the requirements of 6.2.
analyte, and from which the several needed calibration solu-
7.4.5 The solution was made within the last twelve months
tions can be prepared by suitable quantitative dilution.
or within the shelf life interval, whichever is shorter.
7.2 Preparation—Prepare the stock solution by dissolving
7.4.6 The standard stock solution is stored at all times in
an accurately weighed quantity of the element or the appropri-
accordance with Section 8.
atestochiometricquantityofastablecompoundoftheelement,
7.4.7 The concentration has been verified prior to use or
inwater,acid,base,ororganicsolvent,anddilutingtoaknown
sale.
volume or weight in a suitably sized and calibrated volumetric
7.5 Stock solutions that do not meet all the conditions of 7.4
flask.
shall be analyzed prior to use. The analysis shall be performed
7.3 Purity of Analyte—The total of all known impurities in
using an appropriate analytical method, preferably a gravimet-
theelementorcompoundoftheelementshallnotexceed0.1 %
ric or volumetric determination that does not depend on
by weight. If an element is used, its quantity shall be corrected
instrumental comparison with another solution of the same
for the total of the metallic impurities and non-metallic
type.
elements such as carbon, nitrogen, sulfur, and oxygen, and also
7.6 Calibration solutions shall be prepared by quantitative
for the quantity of such insoluble materials as may be present
dilution of the stock or standard solutions as directed in the
(see Note 1). The reagents used for dissolution may also
analytical method for which they are specified. The frequency
contain impurities. If one of the impurities is the analyte, the
of preparation will depend on the shelf life of the calibration
concentration of the analyte in the stock solution shall be
solution. At trace lev
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