Designation: E3047 − 16

Standard Test Method for

Analysis of Nickel Alloys by Spark Atomic Emission
Spectrometry1
This standard is issued under the fixed designation E3047; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope Quantification
Element Range (Mass
1.1 This method describes the spark atomic emission spec- Fraction, %)
trometric (Spark-AES) analysis of nickel alloys, such as those Phosphorous 0.005-0.020
specified by committee B02, having chemical compositions Silicon 0.07-0.6
Sulfur 0.002-0.005
within the following limits: Tantalum 0.025-0.15
Application Tin 0.001-0.02
Element Range (Mass Titanium 0.025-3.2
Fraction, %) Tungsten 0.02-0.10
Aluminum 0.005-6.00 Vanadium 0.005-0.25
Boron 0.001-0.10 Zirconium 0.01-0.05
Carbon 0.005-0.15 1.3 This method has been interlaboratory tested for the
Chromium 0.01-33.00
Copper 0.01-35.00 elements and quantification ranges specified in section 1.2. The
Cobalt 0.01-25.00 ranges in section 1.2 indicate intervals within which results
Iron 0.05-55.00 have been demonstrated to be quantitative. It may be possible
Magnesium 0.001-0.020
Manganese 0.01-1.00 to extend this method to other elements or different composi-
Molybdenum 0.01-35.00 tion ranges provided that a method validation study as de-
Niobium 0.01-6.0 scribed in Guide E2857 is performed and that the results of this
Nickel 25.00-100.0
Phosphorous 0.001-0.025 study show that the method extension is meeting laboratory
Silicon 0.01-1.50 data quality objectives. Supplemental data on other elements
Sulfur 0.0001-0.01 not included in the scope are found in the supplemental data
Titanium 0.0001-6.0
Tantalum 0.01-0.15 tables of the Precision and Bias section.
Tin 0.001-0.020 1.4 This standard does not purport to address all of the
Tungsten 0.01-5.0
Vanadium 0.0005-1.0 safety concerns, if any, associated with its use. It is the
Zirconium 0.01-0.10 responsibility of the user of this standard to establish appro-
1.2 The following elements may be determined using this priate safety and health practices and determine the applica-
method. bility of regulatory limitations prior to use. Specific safety
Quantification hazard statements are given in Section 9.
Element Range (Mass
Fraction, %) 2. Referenced Documents
Aluminum 0.010-1.50
Boron 0.004-0.025 2.1 ASTM Standards:2
Carbon 0.014-0.15 E29 Practice for Using Significant Digits in Test Data to
Chromium 0.09-20.0
Cobalt 0.05-14.00
Determine Conformance with Specifications
Copper 0.03-0.6 E135 Terminology Relating to Analytical Chemistry for
Iron 0.17-20 Metals, Ores, and Related Materials
Magnesium 0.001-0.03
Manganese 0.04-0.6
E177 Practice for Use of the Terms Precision and Bias in
Molybdenum 0.07-5.0 ASTM Test Methods
Niobium 0.02-5.5 E305 Practice for Establishing and Controlling Atomic
Emission Spectrochemical Analytical Curves
1
This test method is under the jurisdiction of ASTM Committee E01 on
2
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 1, 2016. Published May 2016. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
E3047–16. the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 E3047 − 16
E406 Practice for Using Controlled Atmospheres in Spec- 5.3 It is expected that laboratories using this method will
trochemical Analysis prepare their own work instructions. These work instructions
E691 Practice for Conducting an Interlaboratory Study to will include detailed operating instructions for the specific
Determine the Precision of a Test Method laboratory including information such as applicable analytical
E1257 Guide for Evaluating Grinding Materials Used for methods, drift correction (standardization) protocols, verifiers,
Surface Preparation in Spectrochemical Analysis and performance acceptance criteria.
E1329 Practice for Verification and Use of Control Charts in
Spectrochemical Analysis 6. Interferences
E1601 Practice for Conducting an Interlaboratory Study to 6.1 When possible, select analytical lines which are free
Evaluate the Performance of an Analytical Method from spectral interferences. However, this is not always
E2857 Guide for Validating Analytical Methods possible, and it may be necessary to apply interelement
E2972 Guide for Production, Testing, and Value Assignment corrections to account mathematically for the effect of the
of In-House Reference Materials for Metals, Ores, and interference on the measured intensities. If interference correc-
Other Related Materials tions are necessary, refer to Practice E305 for detailed infor-
2.2 ISO Standard:3 mation on the various techniques used to calculate interference
ISO/IEC Guide 98-3:2008 Uncertainty of Measurement— corrections.
Part 3: Guide to the Expression of Uncertainty in Mea- 6.2 Table 1 lists analytical lines routinely used for analysis
surement (GUM:1995) of nickel alloys. For consistency of expression, the wave-
lengths are all listed as stated in the National Institute of
3. Terminology
Standards and Technology (NIST) Atomic Spectroscopy Data-
3.1 Definitions—For definitions of terms used in this base.4 In the NIST wavelength table, wavelengths < 200 nm
Practice, refer to Terminology E135. are as determined in a vacuum and wavelengths of ≥ 200 nm
are as determined in air. Interference corrections, as reported
4. Summary of Test Method by the interlaboratory study participants, are also indicated. It
4.1 A controlled electrical discharge is produced in an argon is not implied that analyses using this standard test method
atmosphere between the prepared flat surface of a specimen must be made with the same atmospheric conditions as stated
and the tip of a counter electrode. The energy of the discharge for the NIST stated wavelengths. Performance of the analytical
is sufficient to ablate material from the surface of the specimen, line selected should be evaluated during method development
break the chemical or physical bonds, and cause the resulting for sensitivity and potential interferences.
atoms or ions to emit radiant energy. The radiant energy is
dispersed by a grating and energies of selected analytical lines 7. Apparatus
and the internal standard line(s) are converted into electrical 7.1 Spark Atomic Emission Spectrometer, containing the
signals by either photomultiplier tubes (PMTs) or a suitable following basic components.
solid state detector. The detected analyte signals are integrated 7.1.1 Spark Source—The excitation source uses computer
and converted to an intensity value. A ratio of the detected software which typically produces: (1) a high-energy pre-spark
analyte intensity and the internal standard signal may be made. (of some preset duration), (2) a spark-type discharge (of some
A calibration is made using a suite of reference materials with preset duration), (3) an arc type discharge (of some preset
compositional similarity to the specimens being analyzed. duration), and (4) a spark-type discharge, during which, time
Calibration curves plotting analyte intensity (intensity ratio) resolved measurements are made for improved detection
versus analyte mass fraction are developed. Specimens are limits, (this may be optional on some instruments). The
measured for analyte intensity and results in mass fraction are counter-electrode serves as a conduction path for the high
determined using the calibration curves. voltage discharge. The counter-electrode configuration/
composition is typically specified by the instrument manufac-
5. Significance and Use turer.
5.1 This test method for the chemical analysis of nickel 7.1.2 Analytical Stand—Capable of supporting the speci-
alloys is primarily intended to test material for compliance with men and counter-electrode in a manner such that the discharge
compositional specifications such as those under jurisdiction of of the spark source may conduct through the flat, uniform
ASTM committee B02. It may also be used to test compliance surface of a prepared specimen. Additionally, the stand is
with other specifications that are compatible with the test designed to work in conjunction with the gas flow system.
method. 7.1.3 Gas Flow System—Designed to deliver pure argon gas
to the spark discharge, specimen interface region. Use the
5.2 It is assumed that all who use this method will be trained
minimum argon purity specified by the instrument manufac-
analysts capable of performing common laboratory procedures
turer. Refer to Practice E406 for practical guidance on the use
skillfully and safely, and that the work will be performed in a
of controlled atmospheres.
properly equipped laboratory.

4
Kramida, A., Ralchenko, Yu., Reader, J., and NIST ASD Team (2014). NIST
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., Atomic Spectra Database (ver. 5.2), [Online]. Available: http://physics.nist.gov/asd
4th Floor, New York, NY 10036, http://www.ansi.org. [2015, July 29]. National Institute of Standards and Technology, Gaithersburg, MD.

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 E3047 − 16
TABLE 1 Analytical Lines for the Analysis of Nickel Alloys and Potential Interferences
Element Wavelength, nm Potential Interference Element Wavelength, nm Potential Interference
Aluminum 308.22 Cr, Mo,, Nb, Ti Nickel 150.00
Aluminum 309.28 Cu, Fe, Mo, Nb, Nickel 166.66
Aluminum 394.40 Co, Cr, Cu, Fe, Mo, Nickel 182.31
Nb, Si, W
Aluminum 616.43 Nickel 208.08
Arsenic 189.04 Fe Nickel 210.58
Boron 182.64 Co, Cr, Fe, Mn, Mo, Nickel 214.78
Ti, W
Boron 345.13 Nickel 218.55
Calcium 396.85 Nickel 226.14
Calcium 393.37 Fe Nickel 232.27
Carbon 193.09 Al, Fe Nickel 243.79
Carbon 165.70 Fe Nickel 282.13
Cobalt 228.62 Cr, Fe, Mo, Nb, W, Ti, Nickel 301.91
Cobalt 258.03 Fe, Mo,Nb, W Nickel 304.50
Cobalt 345.35 Cr, Fe, ,Mo,Nb,Ti, W, Nickel 309.71
Cobalt 384.55 Cr,Fe,Mo,Ti,,W Nickel 310.55
Cobalt 184.59 Al, Fe Ti, Nickel 346.95
Chromium 267.72 Cu, Mo, Nb Nickel 376.95
Chromium 298.92 Al,Co,Fe,Ti,W Nickel 380.71
Copper 199.97 Fe, Mo, Nb Nickel 471.44
Copper 212.30 Co, Mn, Ti, Si, Sn Phosphorous 177.49 Cu, Mo, Nb, W
Copper 224.26 Ni, W Phosphorous 178.28 Cr, Fe, Mo, Nb, W
Copper 282.44 Silver 338.29 Co, Cr
Copper 324.75 Fe, Nb, W Silver 328.07 Mo
Copper 510.55 Co, Cr,Mo,Nb, W, Silicon 212.41 Cr, Co, Fe, Mo, Nb,W
Iron 260.02 Co, Cr, Cu, W Silicon 288.16 Al, Cr
Iron 273.07 Co,Cr,Ti,W,Mo, Nb Sulfur 180.73 Al, Co, Cr, Mn, Mo,
Nb, Ni, Ti, W
Iron 275.57 Al, Co, Cu,Mn, Mo, Nb Tantalum 240.06 Co
Ti, W,
Iron 371.99 Tantalum 293.27 Cr, Nb, Ni, W
Iron 492.39 Tantalum 331.12 Cr, Nb, W, Zr
Magnesium 279.08 Fe Tin 189.99 Cr, Mo,Nb, Ti,V
Manganese 263.82 Al, Cr, Fe, Mo, W Tin 300.91 Cr, Fe, Mo
Manganese 273.09 Cr, Fe, Ti Tin 317.50 Fe
Manganese 293.93 Titanium 308.81 Co, Cu, Fe, Mo, W,
Molybdenum 202.03 Cr, Mn, Ni, W Titanium 324.20 Co, Cr, Fe, Mo,Nb,W
Molybdenum 281.61 Al, Co, Cr, Fe Vanadium 311.07 Al, Co, Cr, Cu, Fe,
Mo, Nb, Ti,
Molybdenum 290.91 Cr, Fe, W Tungsten 220.45 Al, Co, Cr, Mo
Molybdenum 308.76 Cr, Fe, W Tungsten 400.90 Co, Cr, Fe, Mo, Nb, Ti
Molybdenum 369.26 Fe Zirconium 343.82 Co, Cr, Fe, Mo, Ta, Ti,
W
Niobium 319.50 W Zirconium 349.62 Co, Cr, Mn, Mo
Zirconium 468.84

7.1.4 Spectrometer—Having acceptable dispersion, analytical method conditions, source operation, data
resolution, and wavelength coverage for the determination of acquisition, and the conversion of intensity data to mass
nickel alloys. Table 1 provides guidance on the wavelengths fraction.
that may be required. 7.1.7 Other Software—Designed to coordinate instrument
7.1.5 Optional Optical Path Purge or Vacuum System— function. At a minimum, the instrument’s software should
Designed to enhance ultraviolet wavelength sensitivity by include functions for calibration, routine instrument drift cor-
either purging the optical path with a UV-transparent gas or by rection (standardization) and routine measurement. Additional
evacuating the optical path to remove air. The UV-transparent software features may include functionality for tasks such as
gas shall meet the manufacturer’s minimum suggested purity control charting.
requirements. Typically, the sum of the residual O2 and H2O 7.2 Specimen Preparation Equipment—A grinder or lathe
impurities in the UV-transparent gas should not exceed 2 capable of machining nickel alloy specimens to produce a
µmol/mol (ppm). clean, flat analytical surface.
7.1.6 Measuring and Control Systems—Designed to convert
emitted light intensities to a measurable electrical signal. These 8. Reagents and Materials
systems will consist of either a series of photomultiplier tubes 8.1 Reference Materials (RMs):
(PMT) or solid-state photosensitive arrays ((Charge Coupled 8.1.1 Certified Reference Materials (CRMs) should be used
Device (CCD) or Charge Injection Device (CID)) and integrat- as calibration reference materials (RMs), if available. These
ing electronics. Dedicated computer software is used to control certified reference materials should be of similar composition

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 E3047 − 16
to the alloys being analyzed. In cases where CRMs are not 9.2 Exhaust gas containing fine metallic dust generated by
available for the element and/or alloy being analyzed or if the excitation process may be a health hazard. Therefore, the
available CRMs do not adequately cover the intended analyti- instrument should be designed with an exhaust system to
cal range, it is acceptable to use other reference materials for remove this dust in a safe manner. Some instruments are
calibration. equipped with a filtration system designed for this purpose. An
8.1.2 In-house RMs—Some laboratories may have the re- acceptable alternative to the filtration system would be a
sources to produce in-house RMs for nickel alloys. It is ventilation system that exhausts the powder to a “safe” area
acceptable to use these RMs for calibration of Spark-AES outside of the laboratory. If a filtration system is used, it should
instruments provided that the in-house RMs have been devel- be maintained according to the manufacturer’s recommenda-
oped following technically sound development protocols, such tions.
as those described in Practice E2972. 9.3 If the filtration system includes filters, the filters used to
8.1.3 Instrument Manufacturer Provided RMs—Some collect the internal dust are likely exposed to an oxygen-
manufacturers perform factory calibrations which may include depleted atmosphere. Sudden exposure of the filter to air may
reference materials owned by the manufacturer. The laboratory create a fire hazard. The lab should assess the risks associated
should make reasonable attempts to secure certificates of with used filter disposal.
analysis for each of these RMs and to evaluate the acceptability
of these certificates in conjunction with the laboratory’s quality 10. Sampling, Test Specimens, Test Specimen Preparation
policies. 10.1 Laboratories should follow written practices for sam-
8.2 Grinding Media—If grinding is used as the specimen pling and preparation of test specimens.
preparation technique, belts or disks of appropriate grit shall be 10.2 Test specimens should be free of porosity or inclusions.
provided. Aluminum oxide and silicon carbide based abrasive
materials have been found to be acceptable for grinding nickel 10.3 The test specimen must fit the specimen stand being
alloys. Typically 60 grit or finer abrasive materials are found to used and must be large enough to cover the specimen orifice on
be acceptable. Guide E1257 may be consulted for guidance in the analytical stand of the instrument.
evaluating grinding materials. 10.4 The test specimen configuration must be compatible
with the selected specimen preparation equipment.
8.3 Lathe Tooling—If lathe turning is used for specimen
preparation then tools appropriate for cutting nickel alloys shall 10.5 Prepare the specimen surface by either grinding or
be provided. lathe turning to produce a clean, flat analytical surface. A visual
inspection for flatness is acceptable. Prepare the specimens,
8.4 Drift Correction (Standardization) Samples—Select a drift correction (standardization) samples, and calibration RMs
suite of drift correction samples. This suite of samples should using the same procedure.
be of similar composition to the alloys being analyzed and
should contain analyte levels near the extremes of the calibra- 11. Preparation of Apparatus/Method Development
tion range for each analyte. Drift correction involves a calcu-
lated adjustment to calibration slope and intercept based on 11.1 Analytical instrumentation and specimen preparation
intensity changes observed for the analyzed drift correction equipment shall be installed in a manner consistent with
samples. Although in some cases reference materials may be manufacturer recommendations.
used for this purpose, it is not necessary that reference 11.2 Specify the following parameters into the instrument
materials be used, as drift correction does not involve calibra- software.
tion. Refer to Practices E305 and E1329 for a more detailed 11.2.1 The excitation source conditions.
discussion of the use of drift correction (standardization) 11.2.2 The analytical lines and measurement conditions to
samples in Spark-AES analysis. be used for measurement.
11.2.3 The internal standards and associated measurement
8.5 Verifiers—The verifiers should be of similar composi-
parameters, if intensity ratio is to be used as the expression for
tion to the unknowns. Additionally, they should contain ana-
the measurement response. Nickel is typically used as the
lytes in sufficient quantity as to display a significant intensity
internal standard for the analysis of nickel alloys.
response when ablated, in order that calibration drift may be
11.2.4 Drift correction (standardization) sample identifica-
quantified. Refer to Practices E305 and E1329 for a more
tion and associated measurement parameters. If possible, each
detailed discussion of the use of verifiers in Spark-AES
analyte should be assigned a drift correction (standardization)
analysis.
sample containing analyte mass fractions near the anticipated
calibration extremes. If the software supports the use of
9. Hazards
multiple point drift correction (standardization), specify addi-
9.1 The excitation sources present a potential electrical tional drift correction (standardization) samples, as necessary.
shock hazard. The sample stand shall be provided with a safety 11.2.5 Calibration reference material (RM) identification,
interlock system to prevent energizing the source whenever analyte mass fractions and associated measurement param-
contact with the electrode is possible. The instrument should be eters.
designed so access to the power supply is also restricted by the 11.2.6 Appropriate reporting parameters such as result
use of safety interlocks. format, unit of measure, reporting order, report destination, etc.

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 E3047 − 16
11.2.7 Optimize source operating conditions, analyte lines, method quantification range will typically exhibit < 3 % RSD
and measuring conditions by performing test burns on calibra- for the average of the burns.
tion RMs in order to assess the sensitivity and precision of the 12.6 Calibration curves are calculated by plotting an expres-
selected measuring conditions. sion of intensity (raw intensity or raw intensity to internal
11.2.8 A cursory examination of intensity data from the test standard intensity ratio) versus analyte mass fraction for the
burns should suggest that the selected measurement conditions calibration RMs. Creation of the calibration curves will involve
are acceptable. Examine the intensity data for these attributes. multivariate regression analysis, including correction for po-
11.2.8.1 There is a change in response for increasing analyte tential interferences. As necessary, apply interelement correc-
mass fraction. tions to mathematically correct for interferences. Refer to
11.2.8.2 The % RSD of the intensity multiplied by the Practice E305 for a detailed discussion on calculating calibra-
analyte concentration of a standard in the analytical range tion curves for Spark-AES.
yields an estimated analyte standard deviation that is consistent
with the laboratories measurement quality objectives. 13. Procedure
11.2.8.3 Ultimately, the acceptability of the selected mea- 13.1 Place a prepared specimen over the orifice in the
surement method parameters will be demonstrated by the instrument analytical stand. There should be no gaps at the
method validation study. edge of the specimen. Choose the location for measurement to
11.2.9 The laboratory should make a copy of the analytical be approximately 6 mm from the edge of the specimen. If
parameters offline in order to recover in the event of instrument burns are to be made near the center of the specimen, consider
database corruption. the metallurgical condition of the specimen, since chill-cast
specimens may have a shrinkage cavity near the center of the
12. Calibration casting.
12.1 Select calibration RMs which adequately define the 13.2 Perform a minimum of two separate burns on the
instrument response across the range of expected analyte mass specimen, re-positioning the specimen between burns so that
fractions. Practice E305 provides general guidance about the ablated areas of the burns do not overlap.
selection of reference materials for calibration. The quality and 13.3 Examine the calculated % RSD for the average of the
number of these calibration RMs will have bearing on the burns. The scope elements listed in the method quantification
quality of the calibration curves obtained. The interlaboratory range will typically exhibit < 3 % RSD for the average of the
study made during the development of this method demon- burns. The lab may choose to make additional burns in order to
strated cases where laboratories clearly did not have robust get a better estimate of the average and its variance.
calibrations covering the full range of specimen compositions
which caused significant calibration biases and outlying data 14. Verification/Drift Correction (Standardization)
for some elements. 14.1 The laboratory shall establish procedures for control of
12.2 Prepare the drift correction (standardization) samples instrument response drift. These procedures should involve the
and calibration RMs using the same technique. use of a verifier and control chart to monitor drift. Refer to
Practice E1329 for guidance in the preparation and use of
12.3 Measure the drift correction (standardization) samples. control charts. Use control chart limits equal to 2 s (two times
Measure each sample for a minimum of three excitation cycles the standard deviation) or 3 s to indicate the need for drift
(burns), re-positioning the sample between burns so that the correction (standardization).
ablated areas of the burns do not overlap. Burns should be
made approximately 6 mm from the edge of the sample. If 14.2 If the instrument software allows, it is acceptable to
burns are to be made near the center of the sample, consider the apply the control strategy using the software. Calculate control
metallurgical condition of the sample, since chill-cast samples limits for the verifier as described in Practice E1329 and enter
may have a shrinkage cavity near the center of the casting. into the software.
Observe the % Relative Standard Deviation (% RSD) obtained 14.3 Prepare control charts/control limits for each verifier/
for the burns. The scope elements listed in the method element combination.
quantification range will typically exhibit < 3 % RSD for the 14.4 The laboratory shall establish a frequency of analysis
average of the burns. for the verifier. Once a verifier control strategy is established,
12.4 Prepare the calibration RMs and test specimens using analyze the verifier periodically to evaluate instrument re-
the same technique. sponse drift.
12.5 Measure each calibration reference material for a 14.5 Drift correct (standardize) the instrument when the
minimum of three burns, re-positioning the calibration RM verifier measurement indicates that the spectrometer has drifted
between burns so that the ablated areas of the burns do not to the point that one or more elements exceed the established
overlap. Burns should be made approximately 6 mm from the 2 s or 3 s control limits. Update the drift correction (standard-
edge of the calibration RM. If burns are to be made near the ization) using the drift correction (standardization) samples
center of the calibration RM, consider the metallurgical con- established in 12.3.
dition of the RM, since chill-cast RMs may have a shrinkage 14.6 Users of this method are discouraged from using
cavity near the center of the casting. Observe the % RSD certified reference materials as drift correction samples or
calculated for the three burns. The scope elements listed in the routine verifiers.

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 E3047 − 16
15. Method Validation include all significant sources of uncertainty in their estimate of
15.1 A laboratory using this method for the first time shall the combined uncertainty. Express the value of U with 2
provide method validation data to demonstrate that the method significant digits. Then, express the reported result to the same
as applied in their laboratory is yielding repeatable, unbiased number of decimal places.
results. 18. Precision and Bias
15.2 Guide E2857 should be consulted for guidance in 18.1 The precision of this test method is based on an
performing the method validation study. It suggests multiple interlaboratory study conducted in 2014. Ten laboratories
means of validating analytical methods. For this Spark-AES participated in this study, testing thirteen total materials of five
validation study, the minimum expectation is that the labora- different alloys for specified elemental contents. One labora-
tory will prepare and analyze solid CRMs and/or RMs using tory submitted two datasets, making eleven datasets available
the method to obtain the necessary validation data. Ideally for statistical analysis in some cases. Not every laboratory was
these will be reference materials that are independent of the able to submit results for every alloy/element combination,
calibration. The precision and bias data obtained for these however each “test result” reported represents an individual
reference materials must then be compared to the precision and determination, and all participants were asked to report tripli-
bias data stated in this method. The interlaboratory study cate test results for each alloy/element pairing. Practice E691
associated with development of this test method clearly was followed for the design and analysis of the data; the details
showed biases related to measurement of specimens with are given in RR:E01-1124.5
analyte composition near the extremes of available calibration 18.1.1 Repeatability (r)—The difference between repetitive
materials. The laboratory should verify calibration robustness results obtained by the same operator in a given laboratory
by analyzing reference materials near the extremes of the applying the same test method with the same apparatus under
working range of calibration. constant operating conditions on identical test material within
15.3 If the validation exercise yields precision and bias data short intervals of time would in the long run, in the normal and
worse than given in the Precision and Bias section of this correct operation of the test method, exceed the following
Method, the laboratory should attempt to identify and correct values only in one case in 20.
any problems associated with their application of this method. 18.1.1.1 Repeatability can be interpreted as maximum dif-
15.4 Ultimately, the method user must weigh customer ference between two results, obtained under repeatability
requirements and the laboratory’s data quality objectives in conditions, that is accepted as plausible due to random causes
order to justify acceptance of the method validation data. under normal and correct operation of the test method.
18.1.1.2 Repeatability limits are listed in Tables 2-25 below.
15.5 The method validation study shall be documented. 18.1.2 Reproducibility (R)—The difference between two
16. Calculations single and independent results obtained by different operators
applying the same test method in different laboratories using
16.1 Analyte results for the unknowns are determined by different apparatus on identical test material would, in the long
comparing the intensity (raw intensity or ratio of raw intensity run, in the normal and correct operation of the test method,
to internal standard intensity) obtained for the specimen exceed the following values only in one case in 20.
measurements to the calibration curve. 18.1.2.1 Reproducibility limits are listed in Tables 2-25
16.2 All calculations may be performed using the instru- below.
ment software. Calculate the mean of the results of the 18.1.3 The above terms (repeatability limit and reproduc-
individual measurements of each specimen and report the ibility limit) are used as specified in Practice E177.
result as a mass fraction, either in % or mg/kg. 18.1.4 Except in cases where fewer than six laboratories
reported usable data, any judgment in accordance with state-
16.3 Rounding of test results obtained using this Test
ments 18.1.1 and 18.1.2 would have an approximate 95%
Method shall be performed in accordance with Practice E29,
probability of being correct.
Rounding Method, unless an alternative rounding method is
specified by the customer or applicable material specification. 18.2 Bias—Using the certified or reference values reported
by the manufacturers and distributors of the tested materials,
17. Report biases were calculated and reported in Tables 2-21.
17.1 Results shall be reported in a manner consistent with 18.3 The precision statement was determined through sta-
laboratory internal requirements. tistical examination of usable test results, submitted by ten
17.2 When uncertainty estimates are required, results may laboratories (up to eleven datasets), measuring twenty
be reported in accordance with the guidance provided in the elements, in thirteen test materials.
ISO/IEC Guide 98-3:2008. In this document, it is explained 18.4 To judge the equivalency of two test results, it is
that the analyst must obtain an estimate of the overall uncer- recommended to choose the alloy material that is closest in
tainty of the result and express that uncertainty as an expanded characteristics to the test material.
uncertainty U = kuc, where uc is a combined uncertainty
expressed at the level of 1 s (one standard deviation), and k is 5
Supporting data have been filed at ASTM International Headquarters and may
an expansion factor typically chosen as k = 2 to approximate a be obtained by requesting Research Report RR:E01-1124. Contact ASTM Customer
95 % level of confidence. It is suggested that the laboratory Service at service@astm.org.

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 E3047 − 16
TABLE 2 Aluminum (wt%)
NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.181 0.0013 0.038 0.0036 0.11
WN53 (718 Alloy) 11 0.456 0.0030 0.012 0.0085 0.034
NIST1249 (718 Alloy) 11 0.566 0.5682 -0.4% 0.0031 0.017 0.0086 0.047
NIST1244 (600 Alloy) 10 0.251 0.252 -0.6% 0.0022 0.016 0.0061 0.044
Brammer BS600-4 (600 10 0.0528 0.060 -11.9% 0.00047 0.0098 0.0013 0.028
Alloy)
WT71 (600 Alloy) 10 1.253 0.020 0.097 0.055 0.27
WASP79 (Waspaloy) 10 1.431 0.014 0.094 0.038 0.26
NIST1243 (Waspaloy) 10 1.241 1.23 0.9% 0.017 0.060 0.048 0.17
ARMI62B (Waspaloy) 10 1.354 1.38 -1.9% 0.013 0.063 0.037 0.18
NIST1230 (A286 Alloy) 10 0.244 0.249 -2.0% 0.0034 0.029 0.0095 0.080
ARMI26C (A286 Alloy) 10 0.121 0.12 0.5% 0.0014 0.015 0.0038 0.042
A286-48 (A286 Alloy) 10 0.469 0.0045 0.039 0.013 0.11
Brammer BS200-4 10 0.0076 0.0057 33.1% 0.00036 0.0018 0.0010 0.0049
A
The average of the laboratories’ calculated averages.

TABLE 3 Boron (wt%)

NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 11 0.0171 0.0010 0.0040 0.0028 0.011
WN53 (718 Alloy) 9 0.00059 0.00004 0.00074 0.00010 0.0021
NIST1249 (718 Alloy) 10 0.00234 0.0023 1.6% 0.00003 0.00036 0.00007 0.0010
NIST1244 (600 Alloy) 9 0.00346 0.00283 22.2% 0.00010 0.00080 0.00028 0.0022
Brammer BS600-4 (600 9 0.0066 0.0060 10.5% 0.00012 0.0021 0.00035 0.0059
Alloy)
WT71 (600 Alloy) 8 0.00091 0.00003 0.00057 0.00008 0.0016
WASP79 (Waspaloy) 8 0.00225 0.00004 0.00043 0.00012 0.0012
NIST1243 (Waspaloy) 8 0.00512 0.00494 3.7% 0.00009 0.00020 0.00024 0.00056
ARMI62B (Waspaloy) 8 0.00488 0.005 -2.3% 0.00016 0.00025 0.00046 0.00071
NIST1230 (A286 Alloy) 9 0.0058 0.00519 12.3% 0.00020 0.0012 0.00055 0.0032
ARMI26C (A286 Alloy) 9 0.0077 0.0074 3.6% 0.00015 0.0012 0.00043 0.0034
A286-48 (A286 Alloy) 7 0.00063 0.00005 0.00065 0.00013 0.0018
Brammer BS200-4 8 0.0034 0.0037 -8.0% 0.00004 0.0022 0.00010 0.0061
A
The average of the laboratories’ calculated averages.

18.5 For several elements, the interlaboratory study did not 19. Keywords
yield the number of datasets required by Practice E1601 for 19.1 nickel; nickel alloys; Spark-AES; spark atomic emis-
inclusion of the element in the Method scope. For this reason, sion; spark atomic emission spectrometry
these elements are not included in the Method scope. These
supplemental data are, however, summarized Tables 22-25.

7
 E3047 − 16
TABLE 4 Carbon (wt%)
NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.0242 0.0015 0.0031 0.0041 0.0088
WN53 (718 Alloy) 9 0.0095 0.00077 0.0024 0.0022 0.0067
NIST1249 (718 Alloy) 10 0.0380 0.0014 0.0026 0.0040 0.0074
NIST1244 (600 Alloy) 9 0.0625 0.063 -0.8% 0.0016 0.0040 0.0046 0.011
Brammer BS600-4 (600 Alloy) 9 0.0345 0.034 1.4% 0.00084 0.0024 0.0024 0.0068
WT71 (600 Alloy) 6 0.0085 0.0011 0.0050 0.0030 0.014
WASP79 (Waspaloy) 7 0.0056 0.00081 0.0033 0.0023 0.0093
NIST1243 (Waspaloy) 9 0.0246 0.00094 0.0022 0.0026 0.0063
ARMI62B (Waspaloy) 9 0.0277 0.028 -1.0% 0.00062 0.0023 0.0018 0.0064
NIST1230 (A286 Alloy) 9 0.0437 0.0428 2.0% 0.0022 0.0071 0.0062 0.020
ARMI26C (A286 Alloy) 9 0.0307 0.028 9.5% 0.0010 0.0049 0.0028 0.014
A286-48 (A286 Alloy) 8 0.0261 0.00090 0.0058 0.0025 0.016
Brammer BS200-4 7 0.1066 0.107 -0.4% 0.00094 0.0053 0.0026 0.015
A
The average of the laboratories’ calculated averages.

TABLE 5 Chromium (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 16.05 0.056 0.33 0.16 0.93
WN53 (718 Alloy) 10 17.87 0.10 0.14 0.28 0.40
NIST1249 (718 Alloy) 10 18.38 18.472 -0.5% 0.061 0.14 0.17 0.39
NIST1244 (600 Alloy) 8 15.724 15.74 -0.1% 0.052 0.096 0.14 0.27
Brammer BS600-4 (600 Alloy) 8 14.73 14.72 0.1% 0.047 0.23 0.13 0.64
WT71 (600 Alloy) 8 16.43 0.13 0.25 0.36 0.71
WASP79 (Waspaloy) 9 19.51 0.077 0.16 0.22 0.44
NIST1243 (Waspaloy) 9 19.32 19.05 1.4% 0.067 0.24 0.19 0.66
ARMI62B (Waspaloy) 9 19.18 19.06 0.6% 0.099 0.20 0.28 0.57
NIST1230 (A286 Alloy) 8 14.77 14.65 0.8% 0.064 0.35 0.18 0.98
ARMI26C (A286 Alloy) 8 13.73 13.7 0.2% 0.071 0.41 0.20 1.15
A286-48 (A286 Alloy) 8 14.43 0.060 0.32 0.17 0.90
Brammer BS200-4 9 0.133 0.132 0.5% 0.00085 0.015 0.0024 0.043
A
The average of the laboratories’ calculated averages.

TABLE 6 Cobalt (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.982 0.0032 0.079 0.0089 0.22
WN53 (718 Alloy) 9 0.023 0.00065 0.015 0.0018 0.042
NIST1249 (718 Alloy) 10 0.336 0.3371 -0.5% 0.0020 0.010 0.0056 0.028
NIST1244 (600 Alloy) 9 0.0621 0.0602 3.2% 0.00078 0.0034 0.0022 0.0094
Brammer BS600-4 (600 Alloy) 9 0.0941 0.09 4.5% 0.00099 0.0064 0.0028 0.018
WT71 (600 Alloy) 9 0.0114 0.0012 0.0093 0.0033 0.026
WASP79 (Waspaloy) 9 14.02 0.58 0.58 1.62 1.62
NIST1243 (Waspaloy) 9 12.51 12.39 1.0% 0.054 0.14 0.15 0.40
ARMI62B (Waspaloy) 9 13.02 12.95 0.6% 0.028 0.21 0.079 0.58
NIST1230 (A286 Alloy) 8 0.1446 0.151 -4.3% 0.0015 0.0051 0.0042 0.014
ARMI26C (A286 Alloy) 8 0.0541 0.052 4.1% 0.0012 0.0081 0.0034 0.023
A286-48 (A286 Alloy) 8 0.0462 0.00080 0.0080 0.0022 0.022
Brammer BS200-4 8 0.080 0.0911 -12.3% 0.00055 0.014 0.0015 0.039
A
The average of the laboratories’ calculated averages.

8
 E3047 − 16
TABLE 7 Copper (wt%)
NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 0.557 0.0078 0.058 0.022 0.16
WN53 (718 Alloy) 9 0.0065 0.00037 0.0055 0.0010 0.016
NIST1249 (718 Alloy) 10 0.1403 0.1402 0.1% 0.0020 0.0063 0.0055 0.018
NIST1244 (600 Alloy) 10 0.249 0.255 -2.5% 0.0028 0.032 0.0078 0.089
Brammer BS600-4 (600 Alloy) 10 0.0756 0.08 -5.6% 0.00083 0.0073 0.0023 0.021
WT71 (600 Alloy) 10 0.2901 0.0050 0.034 0.014 0.096
WASP79 (Waspaloy) 9 0.0607 0.0024 0.0062 0.0067 0.017
NIST1243 (Waspaloy) 10 0.0082 0.0063 30.4% 0.00018 0.0034 0.00051 0.0096
ARMI62B (Waspaloy) 9 0.0219 0.024 -8.9% 0.00030 0.0044 0.00084 0.012
NIST1230 (A286 Alloy) 8 0.1367 0.137 -0.2% 0.0019 0.0042 0.0052 0.012
ARMI26C (A286 Alloy) 8 0.1463 0.144 1.6% 0.0016 0.0082 0.0043 0.023
A286-48 (A286 Alloy) 8 0.254 0.0031 0.019 0.0086 0.053
Brammer BS200-4 9 0.038 0.0482 -20.6% 0.00020 0.014 0.00055 0.039
A
The average of the laboratories’ calculated averages.

TABLE 8 Iron (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 16.26 0.050 0.25 0.14 0.70
WN53 (718 Alloy) 10 18.20 0.063 0.17 0.18 0.48
NIST1249 (718 Alloy) 10 17.62 17.693 -0.4% 0.057 0.13 0.16 0.37
NIST1244 (600 Alloy) 8 9.55 9.63 -0.9% 0.022 0.13 0.063 0.36
Brammer BS600-4 (600 Alloy) 8 8.39 8.40 -0.1% 0.025 0.21 0.071 0.58
WT71 (600 Alloy) 8 9.03 0.044 0.14 0.12 0.39
WASP79 (Waspaloy) 8 0.172 0.0042 0.030 0.012 0.084
NIST1243 (Waspaloy) 9 0.801 0.776 3.2% 0.0082 0.041 0.023 0.11
ARMI62B (Waspaloy) 9 0.786 0.79 -0.5% 0.011 0.041 0.031 0.12
NIST1230 (A286 Alloy) 6 54.78 55.6 -1.5% 0.10 1.80 0.28 5.03
ARMI26C (A286 Alloy) 6 56.67 0.19 1.59 0.53 4.46
A286-48 (A286 Alloy) 6 54.82 0.15 1.54 0.42 4.31
Brammer BS200-4 9 0.282 0.297 -5.2% 0.0042 0.038 0.012 0.11
A
The average of the laboratories’ calculated averages.

TABLE 9 Manganese (wt%)

NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.313 0.0033 0.039 0.0093 0.11
WN53 (718 Alloy) 6 0.0097 0.00024 0.0096 0.00067 0.027
NIST1249 (718 Alloy) 11 0.1076 0.108 -0.3% 0.0018 0.0058 0.0051 0.016
NIST1244 (600 Alloy) 10 0.299 0.288 3.8% 0.0032 0.015 0.0090 0.042
Brammer BS600-4 (600 Alloy) 10 0.204 0.20 2.1% 0.0028 0.012 0.0077 0.034
WT71 (600 Alloy) 10 0.463 0.0029 0.020 0.0080 0.057
WASP79 (Waspaloy) 9 0.0316 0.00025 0.0057 0.00070 0.016
NIST1243 (Waspaloy) 9 0.0133 0.00730 82.8% 0.00013 0.0066 0.00036 0.018
ARMI62B (Waspaloy) 9 0.0306 0.026 17.5% 0.00033 0.0046 0.00093 0.013
NIST1230 (A286 Alloy) 9 0.615 0.652 -5.6% 0.0035 0.067 0.0097 0.19
ARMI26C (A286 Alloy) 9 0.262 0.25 4.7% 0.0012 0.025 0.0033 0.069
A286-48 (A286 Alloy) 9 0.486 0.0021 0.031 0.0060 0.088
Brammer BS200-4 9 0.312 0.310 0.5% 0.0019 0.032 0.0054 0.089
A
The average of the laboratories’ calculated averages.

9
 E3047 − 16
TABLE 10 Magnesium (wt%)
NOTE 1—Data from up to N=9 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 0.0216 0.00071 0.0082 0.0020 0.023
WN53 (718 Alloy) 8 0.00097 0.00007 0.00063 0.00019 0.0018
NIST1249 (718 Alloy) 9 0.00137 0.0012 14.0% 0.00012 0.00062 0.00032 0.0017
NIST1244 (600 Alloy) 8 0.0134 0.01383 -3.3% 0.00034 0.0030 0.00096 0.0085
Brammer BS600-4 (600 Alloy) 8 0.0197 0.020 -1.7% 0.00038 0.0045 0.0011 0.013
WT71 (600 Alloy) 7 0.0041 0.00023 0.0067 0.00064 0.019
WASP79 (Waspaloy) 7 0.00138 0.00001 0.00085 0.00003 0.0024
NIST1243 (Waspaloy) 7 0.00062 0.00001 0.00051 0.00004 0.0014
ARMI62B (Waspaloy) 7 0.00087 0.00016 0.00041 0.00046 0.0011
NIST1230 (A286 Alloy) 5 0.00046 0.00002 0.00025 0.00006 0.00069
ARMI26C (A286 Alloy) 5 0.00045 0.00001 0.00026 0.00003 0.00074
A286-48 (A286 Alloy) 5 0.0112 0.00058 0.0029 0.0016 0.0080
Brammer BS200-4 7 0.027 0.0312 -14.7% 0.00031 0.012 0.00088 0.034
A
The average of the laboratories’ calculated averages.

TABLE 11 Molybdenum (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 3.385 0.030 0.093 0.084 0.26
WN53 (718 Alloy) 10 2.886 0.017 0.062 0.047 0.17
NIST1249 (718 Alloy) 10 3.117 3.112 0.2% 0.016 0.046 0.046 0.13
NIST1244 (600 Alloy) 9 0.202 0.204 -0.8% 0.0040 0.016 0.011 0.045
Brammer BS600-4 (600 Alloy) 7 0.0090 0.0016 0.0090 0.0043 0.025
WT71 (600 Alloy) 9 0.020 0.0012 0.015 0.0035 0.043
WASP79 (Waspaloy) 9 4.981 0.028 0.085 0.079 0.24
NIST1243 (Waspaloy) 9 4.240 4.226 0.3% 0.019 0.058 0.053 0.16
ARMI62B (Waspaloy) 9 4.157 4.17 -0.3% 0.031 0.057 0.087 0.16
NIST1230 (A286 Alloy) 9 1.161 1.15 0.9% 0.0073 0.059 0.021 0.17
ARMI26C (A286 Alloy) 9 1.094 1.09 0.4% 0.0036 0.096 0.010 0.27
A286-48 (A286 Alloy) 9 1.146 0.024 0.089 0.068 0.25
Brammer BS200-4 6 0.006 0.0013 368.8% 0.00061 0.011 0.0017 0.032
A
The average of the laboratories’ calculated averages.

TABLE 12 Niobium (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 4.83 0.089 0.23 0.25 0.64
WN53 (718 Alloy) 9 5.431 0.052 0.067 0.14 0.19
NIST1249 (718 Alloy) 9 5.214 5.196 0.3% 0.024 0.064 0.067 0.18
NIST1244 (600 Alloy) 9 0.119 0.126 -5.4% 0.0013 0.010 0.0037 0.029
Brammer BS600-4 (600 Alloy) 6 0.0082 0.00037 0.0032 0.0010 0.0089
WT71 (600 Alloy) 8 0.0104 0.00017 0.0024 0.00048 0.0067
WASP79 (Waspaloy) 10 0.0162 0.00047 0.0055 0.0013 0.015
NIST1243 (Waspaloy) 10 0.0301 0.0286 5.3% 0.00039 0.0057 0.0011 0.016
ARMI62B (Waspaloy) 10 0.0508 0.050 1.6% 0.00050 0.0073 0.0014 0.021
NIST1230 (A286 Alloy) 10 0.054 0.06700 -18.8% 0.0014 0.014 0.0040 0.039
ARMI26C (A286 Alloy) 9 0.016 0.002 722.7% 0.00043 0.014 0.0012 0.040
A286-48 (A286 Alloy) 9 0.028 0.00032 0.013 0.00089 0.037
Brammer BS200-4 7 0.0012 0.0010 19.6% 0.00006 0.0073 0.00017 0.020
A
The average of the laboratories’ calculated averages.

10
 E3047 − 16
TABLE 13 Phosphorus (wt%)
NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 11 0.0187 0.00086 0.0027 0.0024 0.0076
WN53 (718 Alloy) 10 0.00268 0.00027 0.00086 0.00076 0.0024
NIST1249 (718 Alloy) 11 0.0121 0.0134 -9.4% 0.00023 0.0017 0.00063 0.0047
NIST1244 (600 Alloy) 10 0.0106 0.011 -3.2% 0.00032 0.0016 0.00088 0.0044
Brammer BS600-4 (600 Alloy) 10 0.0074 0.007 5.5% 0.00015 0.0017 0.00041 0.0048
WT71 (600 Alloy) 7 0.0038 0.00011 0.0024 0.00032 0.0069
WASP79 (Waspaloy) 10 0.0022 0.00012 0.0010 0.00034 0.0029
NIST1243 (Waspaloy) 10 0.00291 0.00317 -8.3% 0.00020 0.00091 0.00056 0.0026
ARMI62B (Waspaloy) 10 0.00315 0.0028 12.5% 0.00041 0.00094 0.0012 0.0026
NIST1230 (A286 Alloy) 9 0.0199 0.0239 -16.7% 0.00075 0.0037 0.0021 0.010
ARMI26C (A286 Alloy) 9 0.0169 0.017 -0.7% 0.00048 0.0034 0.0014 0.0095
A286-48 (A286 Alloy) 9 0.0056 0.00039 0.0023 0.0011 0.0064
Brammer BS200-4 8 0.00214 0.0023 -6.8% 0.00009 0.00077 0.00026 0.0022
A
The average of the laboratories’ calculated averages.

TABLE 14 Silicon (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 8 0.523 0.0032 0.078 0.0090 0.22
WN53 (718 Alloy) 9 0.019 0.00088 0.014 0.0025 0.038
NIST1249 (718 Alloy) 9 0.1135 0.120 -5.4% 0.00082 0.0057 0.0023 0.016
NIST1244 (600 Alloy) 10 0.1228 0.114 7.7% 0.0028 0.0098 0.0077 0.028
Brammer BS600-4 (600 Alloy) 10 0.204 0.22 -7.2% 0.0017 0.013 0.0048 0.036
WT71 (600 Alloy) 9 0.572 0.0035 0.070 0.0097 0.20
WASP79 (Waspaloy) 9 0.0384 0.0033 0.0096 0.0091 0.027
NIST1243 (Waspaloy) 9 0.023 0.0192 17.9% 0.00070 0.010 0.0020 0.028
ARMI62B (Waspaloy) 9 0.0625 0.073 -14.4% 0.0017 0.0095 0.0048 0.027
NIST1230 (A286 Alloy) 9 0.434 0.411 5.5% 0.0125 0.046 0.035 0.13
ARMI26C (A286 Alloy) 9 0.093 0.08 16.4% 0.0015 0.016 0.0043 0.044
A286-48 (A286 Alloy) 9 0.477 0.0046 0.052 0.013 0.15
Brammer BS200-4 9 0.077 0.101 -23.6% 0.00053 0.036 0.0015 0.10
A
The average of the laboratories’ calculated averages.

TABLE 15 Sulfur (wt%)

NOTE 1—Data from up to N=8 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 8 0.00057 0.00015 0.00052 0.00042 0.0014
WN53 (718 Alloy) 5 0.00043 0.00009 0.00018 0.00025 0.00051
NIST1249 (718 Alloy) 7 0.00055 0.00064 -14.4% 0.00012 0.00023 0.00035 0.00064
NIST1244 (600 Alloy) 9 0.0027 0.0028 -4.2% 0.00042 0.0012 0.0012 0.0033
Brammer BS600-4 (600 Alloy) 8 0.0030 0.004 -25.4% 0.00023 0.0011 0.00064 0.0032
WT71 (600 Alloy) 8 0.0016 0.00014 0.0011 0.00041 0.0030
WASP79 (Waspaloy) 8 0.0013 0.00015 0.0011 0.00042 0.0031
NIST1243 (Waspaloy) 6 0.0023 0.00217 7.1% 0.00024 0.0014 0.00066 0.0039
ARMI62B (Waspaloy) 6 0.00099 0.0003 230.6% 0.00032 0.00087 0.00088 0.0024
NIST1230 (A286 Alloy) 6 0.0012 0.00095 27.1% 0.00024 0.0016 0.00067 0.0046
ARMI26C (A286 Alloy) 4 0.00017 0.0004 -58.1% 0.00033 0.00071 0.00091 0.0020
A286-48 (A286 Alloy) 5 0.0012 0.00021 0.0019 0.00059 0.0054
Brammer BS200-4 6 0.0040 0.0076 -47.0% 0.00032 0.0031 0.00090 0.0087
A
The average of the laboratories’ calculated averages.

11
 E3047 − 16
TABLE 16 Tantalum (wt%)
NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.0096 0.00070 0.0045 0.0020 0.013
WN53 (718 Alloy) 11 0.084 0.0034 0.033 0.0095 0.092
NIST1249 (718 Alloy) 10 0.0058 0.0027 114.0% 0.0024 0.0036 0.0068 0.010
NIST1244 (600 Alloy) 4 0.029 0.0013 0.037 0.0036 0.10
Brammer BS600-4 (600 Alloy) 4 0.025 0.0024 0.031 0.0068 0.088
WT71 (600 Alloy) 6 0.022 0.0011 0.031 0.0032 0.086
WASP79 (Waspaloy) 8 0.136 0.0046 0.047 0.013 0.13
NIST1243 (Waspaloy) 5 0.023 0.00099 0.017 0.0028 0.048
ARMI62B (Waspaloy) 6 0.020 0.0030 0.017 0.0083 0.047
NIST1230 (A286 Alloy) 7 0.0040 0.00049 0.0041 0.0014 0.011
ARMI26C (A286 Alloy) 6 0.0040 0.002 98.8% 0.00091 0.0048 0.0026 0.014
A286-48 (A286 Alloy) 7 0.0111 0.0012 0.0035 0.0033 0.0097
Brammer BS200-4 2 0.00444 0.0003 1380% 0.00018 0.00058 0.00051 0.0016
A
The average of the laboratories’ calculated averages.

TABLE 17 Tin (wt%)

NOTE 1—Data from up to N=9 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 0.0193 0.00030 0.0067 0.00085 0.019
WN53 (718 Alloy) 6 0.00115 0.00026 0.00068 0.00074 0.0019
NIST1249 (718 Alloy) 8 0.00249 0.0024 3.7% 0.00015 0.00082 0.00042 0.0023
NIST1244 (600 Alloy) 4 0.0017 0.00074 130.5% 0.00008 0.0024 0.00022 0.0068
Brammer BS600-4 (600 Alloy) 4 0.0026 0.00005 0.0025 0.00015 0.0071
WT71 (600 Alloy) 5 0.0033 0.00018 0.0022 0.00049 0.0062
WASP79 (Waspaloy) 4 0.00209 0.00012 0.00089 0.00035 0.0025
NIST1243 (Waspaloy) 4 0.00062 0.00009 0.00031 0.00025 0.00088
ARMI62B (Waspaloy) 4 0.00103 0.00008 0.00037 0.00023 0.0010
NIST1230 (A286 Alloy) 7 0.0130 0.0013 0.0028 0.0038 0.0077
ARMI26C (A286 Alloy) 7 0.0122 0.011 10.9% 0.0012 0.0068 0.0034 0.019
A286-48 (A286 Alloy) 6 0.0014 0.00050 0.0013 0.0014 0.0037
Brammer BS200-4 3 0.00021 0.00020 3.9% 0.00002 0.00013 0.00007 0.00036
A
The average of the laboratories’ calculated averages.

TABLE 18 Titanium (wt%)

NOTE 1—Data from up to N=11 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 10 0.485 0.0072 0.027 0.020 0.077
WN53 (718 Alloy) 11 1.011 0.0065 0.041 0.018 0.11
NIST1249 (718 Alloy) 10 0.969 0.959 1.0% 0.0049 0.041 0.014 0.12
NIST1244 (600 Alloy) 9 0.2592 0.251 3.3% 0.0038 0.0086 0.011 0.024
Brammer BS600-4 (600 Alloy) 9 0.1970 0.20 -1.5% 0.0019 0.0047 0.0054 0.013
WT71 (600 Alloy) 9 0.1002 0.0011 0.0065 0.0030 0.018
WASP79 (Waspaloy) 9 3.180 0.021 0.047 0.059 0.13
NIST1243 (Waspaloy) 9 3.074 3.054 0.7% 0.022 0.037 0.062 0.10
ARMI62B (Waspaloy) 9 3.039 3.02 0.6% 0.023 0.034 0.065 0.096
NIST1230 (A286 Alloy) 8 2.23 2.18 2.5% 0.042 0.14 0.12 0.40
ARMI26C (A286 Alloy) 9 1.906 1.87 1.9% 0.013 0.080 0.037 0.22
A286-48 (A286 Alloy) 9 2.01 0.046 0.10 0.13 0.29
Brammer BS200-4 9 0.0219 0.0191 14.6% 0.00044 0.0044 0.0012 0.012
A
The average of the laboratories’ calculated averages.

12
 E3047 − 16
TABLE 19 Tungsten (wt%)
NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 7 0.025 0.0023 0.020 0.0065 0.056
WN53 (718 Alloy) 10 0.078 0.0022 0.015 0.0062 0.041
NIST1249 (718 Alloy) 10 0.086 0.0846 1.0% 0.0020 0.018 0.0056 0.051
NIST1244 (600 Alloy) 5 0.0078 0.0019 0.0064 0.0052 0.018
Brammer BS600-4 (600 Alloy) 5 0.0115 0.0011 0.0047 0.0031 0.013
WT71 (600 Alloy) 9 0.017 0.0038 0.029 0.011 0.081
WASP79 (Waspaloy) 8 0.051 0.0025 0.033 0.0069 0.091
NIST1243 (Waspaloy) 7 0.034 0.00091 0.028 0.0025 0.078
ARMI62B (Waspaloy) 7 0.079 0.068 16.8% 0.0028 0.030 0.0080 0.084
NIST1230 (A286 Alloy) 7 0.0689 0.0695 -0.9% 0.0016 0.0093 0.0044 0.026
ARMI26C (A286 Alloy) 9 0.0165 0.01 64.9% 0.0012 0.0093 0.0034 0.026
A286-48 (A286 Alloy) 9 0.042 0.00083 0.016 0.0023 0.045
Brammer BS200-4 4 0.0047 0.00095 390.3% 0.00049 0.0042 0.0014 0.012
A
The average of the laboratories’ calculated averages.

TABLE 20 Vanadium (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 0.086 0.00041 0.014 0.0012 0.038
WN53 (718 Alloy) 9 0.0109 0.00018 0.0065 0.00051 0.018
NIST1249 (718 Alloy) 10 0.0333 0.0338 -1.4% 0.00037 0.0060 0.0010 0.017
NIST1244 (600 Alloy) 9 0.0305 0.0327 -6.7% 0.00021 0.0056 0.00059 0.016
Brammer BS600-4 (600 Alloy) 9 0.0242 0.023 5.3% 0.00026 0.0035 0.00074 0.0098
WT71 (600 Alloy) 7 0.0092 0.00017 0.0048 0.00048 0.013
WASP79 (Waspaloy) 9 0.0177 0.00037 0.0034 0.0010 0.0096
NIST1243 (Waspaloy) 9 0.0996 0.1043 -4.5% 0.00069 0.0088 0.0019 0.025
ARMI62B (Waspaloy) 9 0.0227 0.022 3.2% 0.00047 0.0038 0.0013 0.011
NIST1230 (A286 Alloy) 9 0.225 0.229 -1.8% 0.0016 0.035 0.0044 0.098
ARMI26C (A286 Alloy) 9 0.237 0.238 -0.2% 0.020 0.028 0.055 0.079
A286-48 (A286 Alloy) 9 0.158 0.0045 0.024 0.013 0.067
Brammer BS200-4 5 0.00253 0.0024 5.5% 0.00005 0.00083 0.00013 0.0023
A
The average of the laboratories’ calculated averages.

TABLE 21 Zirconium (wt%)

NOTE 1—Data from up to N=10 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N x̄ Reference
% Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 9 0.0096 0.00053 0.0029 0.0015 0.0080
WN53 (718 Alloy) 9 0.0314 0.00060 0.0068 0.0017 0.019
NIST1249 (718 Alloy) 10 0.0036 0.0029 25.0% 0.00025 0.0020 0.00071 0.0056
NIST1244 (600 Alloy) 6 0.0018 0.00037 396.1% 0.00025 0.0026 0.00071 0.0072
Brammer BS600-4 (600 Alloy) 5 0.0017 0.00014 0.0025 0.00039 0.0070
WT71 (600 Alloy) 6 0.0230 0.00061 0.0052 0.0017 0.015
WASP79 (Waspaloy) 9 0.0220 0.00079 0.0037 0.0022 0.010
NIST1243 (Waspaloy) 9 0.0527 0.053 -0.6% 0.00060 0.0021 0.0017 0.0060
ARMI62B (Waspaloy) 8 0.0377 0.036 4.6% 0.00036 0.0025 0.0010 0.0071
NIST1230 (A286 Alloy) 5 0.0039 0.00013 0.0037 0.00036 0.010
ARMI26C (A286 Alloy) 5 0.00135 0.00013 0.00068 0.00036 0.0019
A286-48 (A286 Alloy) 5 0.0133 0.00056 0.0068 0.0016 0.019
Brammer BS200-4 2 0.0054 0.00010 0.0070 0.00027 0.020
A
The average of the laboratories’ calculated averages.

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 E3047 − 16
TABLE 22 Arsenic (wt%)
NOTE 1—Data from up to N=4 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 4 0.00025 NA NA 0.00010 0.00085 0.00028 0.0024
WN53 (718 Alloy) 4 0.00031 NA NA 0.00029 0.00072 0.00082 0.0020
NIST1249 (718 Alloy) 4 0.00114 .0013 NA 0.00007 0.00051 0.00020 0.0014
NIST1244 (600 Alloy) 3 0.00152 NA NA 0.00010 0.00089 0.00027 0.0025
Brammer BS600-4 (600 Alloy) 3 0.00079 NA NA 0.00024 0.00092 0.00067 0.0026
WT71 (600 Alloy) 3 0.00161 NA NA 0.00024 0.00081 0.00068 0.0023
WASP79 (Waspaloy) 1 -0.00003 NA NA 0.00029 0.00029 0.00080 0.00080
NIST1243 (Waspaloy) 1 0.00040 NA NA 0.00010 0.00010 0.00028 0.00028
ARMI62B (Waspaloy) 1 0.00055 NA NA 0.00039 0.00039 0.0011 0.0011
NIST1230 (A286 Alloy) 2 0.0048 NA NA 0.00026 0.0029 0.00072 0.0080
ARMI26C (A286 Alloy) 2 0.00274 NA NA 0.00050 0.00050 0.0014 0.0014
A286-48 (A286 Alloy) 2 0.00134 NA NA 0.00023 0.00062 0.00066 0.0017
A
The average of the laboratories’ calculated averages.

TABLE 23 Silver (wt%)

NOTE 1—Data from up to N=3 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 3 0.00114 NA NA 0.00002 0.00008 0.00005 0.00024
WN53 (718 Alloy) 3 0.00007 NA NA 0.00001 0.00006 0.00003 0.00016
NIST1249 (718 Alloy) 3 0.00007 NA NA 0.00001 0.00008 0.00002 0.00021
NIST1244 (600 Alloy) 1 0.00046 NA NA 0.00001 0.00001 0.00003 0.00003
Brammer BS600-4 (600 Alloy) 1 0.00028 NA NA 0.00002 0.00002 0.00006 0.00006
WT71 (600 Alloy) 1 0.00054 NA NA 0.00002 0.00002 0.00004 0.00004
WASP79 (Waspaloy) 2 0.00043 NA NA 0.00002 0.00010 0.00005 0.00029
NIST1243 (Waspaloy) 1 0.00008 NA NA 0.00001 0.00001 0.00003 0.00003
ARMI62B (Waspaloy) 1 0.00004 NA NA 0.00001 0.00001 0.00003 0.00003
NIST1230 (A286 Alloy) 3 0.00020 NA NA 0.00002 0.00009 0.00005 0.00025
ARMI26C (A286 Alloy) 3 0.00011 NA NA 0.00001 0.00004 0.00002 0.00011
A286-48 (A286 Alloy) 3 0.00361 NA NA 0.00012 0.00035 0.00033 0.00099
A
The average of the laboratories’ calculated averages.

TABLE 24 Calcium (wt%)

NOTE 1—Data from up to N=4 datasets utilized.

Repeatability Reproducibility
Certified or
Material N AverageA Reference
Bias Standard Standard Repeatability Reproducibility
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 4 0.00206 NA NA 0.00007 0.00036 0.00021 0.00102
WN53 (718 Alloy) 4 0.00043 NA NA 0.00009 0.00019 0.00024 0.00054
NIST1249 (718 Alloy) 4 0.00032 NA NA 0.00009 0.00023 0.00024 0.00064
NIST1244 (600 Alloy) 2 0.00065 NA NA 0.00003 0.00065 0.00010 0.00181
Brammer BS600-4 (600 Alloy) 2 0.00053 NA NA 0.00001 0.00059 0.00003 0.00165
WT71 (600 Alloy) 2 0.00059 NA NA 0.00005 0.00060 0.00014 0.00169
WASP79 (Waspaloy) 3 0.00012 NA NA 0.00002 0.00005 0.00006 0.00013
NIST1243 (Waspaloy) 3 0.00010 NA NA 0.00002 0.00005 0.00005 0.00014
ARMI62B (Waspaloy) 3 0.00010 NA NA 0.00002 0.00006 0.00007 0.00017
NIST1230 (A286 Alloy) 2 0.00025 NA NA 0.00001 0.00001 0.00003 0.00004
ARMI26C (A286 Alloy) 2 0.00022 NA NA 0.00001 0.00003 0.00003 0.00009
A286-48 (A286 Alloy) 3 0.00068 NA NA 0.00003 0.00025 0.00007 0.00071
A
The average of the laboratories’ calculated averages.

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 E3047 − 16
TABLE 25 Nitrogen (wt%)
NOTE 1—Data from up to N=4 datasets utilized.
Repeatability Reproducibility
Certified or
AverageA Bias Standard Standard Repeatability Reproducibility
Material N Reference
x̄ % Deviation Deviation Limit Limit
Value
sr sR r R
WT48 (718 Alloy) 4 0.0030 NA NA 0.00031 0.0041 0.00086 0.011
WN53 (718 Alloy) 4 0.013 NA NA 0.017 0.023 0.049 0.066
NIST1249 (718 Alloy) 4 0.0077 NA NA 0.00061 0.0038 0.0018 0.011
NIST1244 (600 Alloy) 3 0.0116 NA NA 0.0018 0.0029 0.0050 0.0080
Brammer BS600-4 (600 Alloy) 3 0.0186 0.021 NA 0.00052 0.0057 0.0014 0.016
WT71 (600 Alloy) 3 0.00198 NA NA 0.00039 0.00092 0.0011 0.0026
WASP79 (Waspaloy) 2 0.0062 NA NA 0.00019 0.0046 0.00052 0.013
NIST1243 (Waspaloy) 2 0.0086 NA NA 0.00097 0.0044 0.0027 0.012
ARMI62B (Waspaloy) 2 0.0127 0.0022 NA 0.0020 0.0068 0.0056 0.019
NIST1230 (A286 Alloy) 3 0.008 NA NA 0.012 0.012 0.033 0.033
ARMI26C (A286 Alloy) 3 0.00452 0.0045 NA 0.00035 0.00040 0.00098 0.0011
A286-48 (A286 Alloy) 3 0.0059 NA NA 0.00039 0.0054 0.0011 0.015
Brammer BS200-4 1 0.00051 0.00031 NA 0.00008 0.00008 0.00022 0.00022
A
The average of the laboratories’ calculated averages.

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