ASTM E1009-95(2000)
(Practice)Standard Practice for Evaluating an Optical Emission Vacuum Spectrometer to Analyze Carbon and Low-Alloy Steel
Standard Practice for Evaluating an Optical Emission Vacuum Spectrometer to Analyze Carbon and Low-Alloy Steel
SCOPE
1.1 This practice covers evaluation of an optical emission vacuum spectrometer to analyze carbon and low-alloy steels. It covers instruments used for the analysis of solid samples taken from molten metal for production control or from products to confirm the composition. Both pre-installation and post-installation precision and accuracy are included in the evaluation.
1.2 While Tables 1-3 are specific for plain carbon and low-alloy steel, they could be supplemented by similar tables for other materials.
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.
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Designation:E1009 –95 (Reapproved 2000)
Standard Practice for
Evaluating an Optical Emission Vacuum Spectrometer to
Analyze Carbon and Low-Alloy Steel
This standard is issued under the fixed designation E 1009; 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 3.2.1 accuracy—the closeness of a spectrochemical deter-
mination to an accepted reference; it is affected by imprecision
1.1 This practice covers evaluation of an optical emission
and bias.
vacuum spectrometer to analyze carbon and low-alloy steels. It
3.2.2 standard error (SE)—although primarily a calculation
covers instruments used for the analysis of solid samples taken
thatmeasureshowwellacalibrationhasbeendefined,standard
from molten metal for production control or from products to
error (SE) is used in this practice as an indicator of accuracy.
confirm the composition. Both pre-installation and post-
It is CRM-dependent and instrument-operator dependent.
installation precision and accuracy are included in the evalua-
Some expected maximum SE values are listed, but compari-
tion.
sons between instrument calibrations can strictly be done only
1.2 While Tables 1-3 are specific for plain carbon and
when identical suites of calibrants are used.
low-alloy steel, they could be supplemented by similar tables
for other materials.
4. Summary of Practice
1.3 This standard does not purport to address all of the
4.1 After the spectrometer is calibrated, use this practice to
safety concerns, if any, associated with its use. It is the
evaluate the instrument and its calibration. Certified reference
responsibility of the user of this standard to establish appro-
materials are run as unknowns and precision is compared to
priate safety and health practices and determine the applica-
Table 1. Before comparing standard errors to those in Table 2,
bility of regulatory limitations prior to use.
ascertain that the calibration does not include unrealistic
2. Referenced Documents inflections. Values equal to or less than those in Tables 1 and 2
indicate that the instrument is acceptable.
2.1 ASTM Standards:
E 135 Terminology Relating to Analytical Chemistry for
5. Significance and Use
Metals, Ores, and Related Materials
5.1 Periodically throughout the useful life of an optical
E 305 Practice for Establishing and Controlling Spectro-
2 emission spectrometer it becomes necessary to evaluate its
chemical Analytical Curves
performance. This is especially true at manufacture and during
E 406 Practice for Using Controlled Atmospheres in Spec-
2 installation. The objective at this time is to establish whether
trochemical Analysis
the instrument meets design specifications and performs to
E 528 Practices for Grounding Basic Optical Emission
3 customer specifications. A manufacturer’s objective may be to
Spectrochemical Equipment
compare production line instruments. With data on many
E 876 Practice for Use of Statistics in the Evaluation of
2 instruments, such an evaluation procedure would be a valuable
Spectrometric Data
contribution to the manufacturer’s quality control plan.
3. Terminology 5.2 Use of this procedure at installation can tell the manu-
facturer or user whether there has been a significant change in
3.1 Definitions—For definitions of terms used in this prac-
performance due to faulty shipping or handling of the instru-
tice, refer to Terminology E 135 and Practice E 876.
ment. At this time, the procedure could be the beginning of a
3.2 Definitions of Terms Specific to This Standard:
quality control plan for the user. Once established, the data
from the procedure provide a base for comparison of future
This practice is under the jurisdiction of ASTM Committee E01 on Analytical runs, enabling operators to detect changes in performance.
Chemistry for Metals, Ores and Related Materials and is the direct responsibility of
5.3 Data produced by this practice make possible a com-
Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
parisonofdifferentinstruments,forexample,X-rayandoptical
Current edition approved March 15, 1995. Published May 1995. Originally
emission or optical emission and atomic absorption. While the
published as E 1009 – 90. Last previous edition E 1009 – 90.
Annual Book of ASTM Standards, Vol 03.05.
Discontinued 1999; see 1998 Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1009
TABLE 1 (a) Revised Data
data in the Tables 1-3 are valid for optical emission spectrom-
eters, other instruments may produce better or worse perfor- Approximate Standard
Element
Concentration, % Deviation
mance values. In this manner, the data could be used by
C 0.015 0.0009
management to determine the suitability of a given instrument
C 1.03 0.012
to perform a given determination with an acceptable precision
MN 0.067 0.0006
and accuracy.
Mn 2.00 0.023
P 0.0032 0.0007
S 0.0024 0.0001
TABLE 1 Recommended Precision Requirements For Steel Using
Si 0.01 0.0002
A
An Optical Emission Vacuum Spectrometer
Ni 0.021 0.0004
Ni 2.00 0.005
Approximate Standard
CR 1.48 0.009
Element
Concentration, % Deviation
Mo 0.005 0.0004
Mo 0.50 0.002
C 0.06 60.002
Cu 0.015 0.0003
0.15 0.004
Cu 0.30 0.0007
0.50 0.010
Ti 0.0055 0.0004
0.90 0.015
Al 0.004 0.0004
Mn 0.35 0.007
Al 0.04 0.0007
0.60 0.015
Nb 0.01 0.0005
1.00 0.02
Nb 0.1 0.002
1.50 0.03
B 0.001 0.0001
P 0.006 0.0007
B 0.005 0.0001
0.04 0.0015
Zr 0.013 0.0007
S 0.005 0.0015
Pb 0.002 0.0004
0.04 0.002
As 0.01 0.0003
0.06 0.004
As 0.055 0.002
Si 0.02 0.004
0.30 0.006
A
0.50 0.010
These precisions were generated from data that were collected on newer
Ni 0.03 0.002
instruments than the original data.
0.10 0.003
0.70 0.007
1.60 0.03
Cr 0.04 0.002 5.4 While this practice is directed towards optical emission
0.30 0.007
vacuum spectrometers in the analysis of carbon and low-alloy
0.80 0.015
steel, its use is not restricted to that instrument or that matrix.
Sn 0.003 0.0006
0.02 0.0015
0.05 0.002 6. Instrumentation
V 0.01 0.0015
6.1 The vacuum spectrometer shall be equipped with an
0.03 0.002
0.25 0.007 argon-flushed sample stand for point-to-plane excitation.
Mo 0.03 0.003
6.2 The excitation parameters and radiations measured shall
0.30 0.008
be selected to meet the specified performance.
Cu 0.02 0.0007
0.15 0.003
NOTE 1—Ordinarily this selection is made by the vendor, or instrument
Ti 0.02 0.002
manufacturer, based on experience.
0.20 0.008
Al 0.006 0.002
6.3 Provision shall be made to compensate for spectral
0.02 0.003
interferences. More than one spectral line may be provided for
0.07 0.004
Nb 0.02 0.0015
an element, depending on element concentration or the exci-
0.07 0.003
tation used, but switching of lines shall be done automatically.
B 0.001 0.00015
0.07 0.003
7. Analysis Time
Zr 0.05 0.002
Pb 0.01 0.0015
7.1 Analysis time, excluding sample preparation, shall not
Se 0.02 0.002
exceed 30 s for single burns, or 60 s for multiple burns.
A
These precisions were generated from actual data in one laboratory; as such,
they represent what has been done with proven, homogeneous materials. NOTE 2—This requirement may be waived if speed of analysis is not
E1009
TABLE 2 Elements, Concentration Ranges, and Recommended
9. Purpose of Analytical Performance Tests
Acceptable Standard Error (SE) for Steel
9.1 Pre-Shipment Precision:
Approximate Concentration
Max Allowable Standard
9.1.1 Perform the tests in 10.1 to verify performance before
Element Range, %, as Covered by the
A
Error, %
Certified Standards
shipment so that any necessary adjustments can be made at the
C 0.02 to 1.00 0.009 factory. Preliminary calibration of the spectrometer is required
Mn 0.01 to 1.50 0.012
to assure that the concentration range specified for each
P 0.001 to 0.07 0.0
...
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