ASTM D4927-14
(Test Method)Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
Standard Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
SIGNIFICANCE AND USE
4.1 Some oils are formulated with organo-metallic additives which act as detergents, antioxidants, antiwear agents, and so forth. Some of these additives contain one or more of these elements: barium, calcium, phosphorus, sulfur, and zinc. These test methods provide a means of determining the concentration of these elements which in turn provides an indication of the additive content of these oils.
4.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (see Table 2).
SCOPE
1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at element concentration ranges shown in Table 1. The range can be extended to higher concentrations by dilution of sample specimens. Additives can also be determined after dilution. Two different methods are presented in these test methods.
1.2 Test Method A (Internal Standard Procedure)—Internal standards are used to compensate for interelement effects of X-ray excitation and fluorescence (see Sections 8 through 13).
1.3 Test Method B (Mathematical Correction Procedure)—The measured X-ray fluorescence intensity for a given element is mathematically corrected for potential interference from other elements present in the sample (see Sections 14 through 19).
1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.
1.5 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: D4927 − 14
StandardTest Methods for
Elemental Analysis of Lubricant and Additive Components—
Barium, Calcium, Phosphorus, Sulfur, and Zinc by
Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D4927; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* 3. Summary of the Test Methods
1.1 These test methods cover the determination of barium,
3.1 Asample specimen is placed in the X-ray beam and the
calcium,phosphorus,sulfur,andzincinunusedlubricatingoils intensity of the appropriate fluorescence lines of barium,
at element concentration ranges shown in Table 1. The range
calcium,phosphorus,sulfur,andzincaremeasured.Instrument
can be extended to higher concentrations by dilution of sample response factors related to the concentration of standards
specimens. Additives can also be determined after dilution.
enable the determination of the concentration of elements in
Two different methods are presented in these test methods. thetestedsamplespecimens.Enhancementordepressionofthe
X-ray fluorescence of a given element by an interfering
1.2 Test Method A (Internal Standard Procedure)—Internal
element in the sample may occur. Two test methods (A and B)
standards are used to compensate for interelement effects of
are described for compensating any interference effect.
X-ray excitation and fluorescence (see Sections 8 through 13).
3.2 Test Method A (Internal Standard Procedure)—Internal
1.3 Test Method B (Mathematical Correction Procedure)—
standards are used with the standards and sample specimens to
The measured X-ray fluorescence intensity for a given element
compensate for the potential interelement effects.
is mathematically corrected for potential interference from
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample
other elements present in the sample (see Sections 14 through
specimen that has been blended with a single internal standard
19).
solution (containing tin or titanium for barium and calcium,
1.4 The preferred concentration units are mass % barium,
zirconium for phosphorus, and nickel for zinc) is poured into
calcium, phosphorus, sulfur, or zinc.
an X-ray cell. Total net counts (peak intensity—background)
1.5 This standard does not purport to address all of the
for each element and its respective internal standard are
safety concerns, if any, associated with its use. It is the
collected at their appropriate wavelengths. The ratios between
responsibility of the user of this standard to establish appro-
elemental and internal standard counts are calculated and
priate safety and health practices and determine the applica-
converted into barium, calcium, phosphorus, or zinc
bility of regulatory limitations prior to use.
concentrations, or a combination thereof, from calibration
curves.
2. Referenced Documents
3.2.2 Sulfur—A sample specimen is mixed with a lead
internal standard solution and analyzed as described in 3.2.1.
2.1 ASTM Standards:
D6299 Practice for Applying Statistical Quality Assurance
3.3 Test Method B (Mathematical Correction Procedure)—
and Control Charting Techniques to Evaluate Analytical
The measured intensity for a given element is mathematically
Measurement System Performance
corrected for the interference from other elements in the
sample specimen. This requires that intensities from all ele-
ments in the specimen be obtained.
These test methods are under the jurisdiction of ASTM Committee D02 on
3.3.1 The sample specimen is placed in the X-ray beam and
Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility
the intensities of the fluorescence lines of barium, calcium,
of Subcommittee D02.03 on Elemental Analysis.
phosphorus, sulfur, and zinc are measured.Asimilar measure-
Current edition approved Dec. 1, 2014. Published January 2015. Originally
ment is made away from the fluorescence lines in order to
approved in 1989. Last previous edition approved in 2010 as D4927 – 10. DOI:
10.1520/D4927-14.
obtainabackgroundcorrection.Concentrationsoftheelements
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
of interest are determined by comparison of net signals against
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
appropriate interelement correction factors developed from
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. responses of calibration standards.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4927 − 14
TABLE 1 Range of Applicability
mass % due to the heavier elements to 1 mass % for the lighter
Element Range, Mass % elements. The measured intensity for a given element can be
Barium 0.04-8.5
mathematically corrected for the absorption of the emitted
Calcium 0.01-1.0
radiationbytheotherelementspresentinthesamplespecimen.
Phosphorus 0.01-0.5
Sulfur 0.1-4.0 Suitable internal standards can also compensate for X-ray
Zinc 0.01-0.6
inter-element effects. If an element is present at significant
concentrations and an interelement correction for that element
is not employed, the results can be low due to absorption or
3.3.2 The X-ray fluorescence spectrometer is initially cali-
high due to enhancement.
brated with a suite of standards in order to determine by
regression analysis, interelement correction factors and instru- 6. Apparatus
ment response factors.
6.1 X-Ray Spectrometer, equipped for soft X-ray detection
3.3.3 Subsequent calibration is achieved using a smaller
˚
of radiation in the range from 1 to 10 A. For optimum
number of standards since only the instrument response factors
sensitivity, the spectrometer is equipped with the following:
needtoberedetermined.Oneofthesestandards(oranoptional
6.1.1 X-Ray Generating Tube, with chromium, rhodium, or
syntheticpellet)canbeusedtomonitorinstrumentaldriftwhen
scandium target. Other targets can also be employed.
performing a high volume of analyses.
6.1.2 Helium, purgeable optical path.
3.4 Additivesandadditivepackagescanbedeterminedafter 6.1.3 Interchangeable Crystals, germanium, lithium fluo-
ride (LiF ), graphite, or pentaerythritol (PET), or a combi-
dilution with base oil to place the elemental concentrations in
the range described in 1.1. nation thereof. Other crystals can also be used.
6.1.4 Pulse-Height Analyzer, or other means of energy
4. Significance and Use
discrimination.
6.1.5 Detector, flow proportional, or scintillation, or flow
4.1 Some oils are formulated with organo-metallic additives
proportional and scintillation counter.
which act as detergents, antioxidants, antiwear agents, and so
forth. Some of these additives contain one or more of these
6.2 Shaker, Mechanical Stirrer, or Ultrasonic Bath, capable
elements: barium, calcium, phosphorus, sulfur, and zinc.These
of handling from 30-mL to 1-L bottles.
test methods provide a means of determining the concentration
6.3 X-Ray Disposable Plastic Cells, with suitable film
of these elements which in turn provides an indication of the
window. Suitable films include Mylar, polypropylene, or
additive content of these oils.
polyimidwithfilmthicknessesbetween0.25to0.35mil(6.3to
4.2 Several additive elements and their compounds are
8.8 µm).
addedtothelubricatingoilstogivebeneficialperformance(see
NOTE 1—Some films contain contamination of the elements of interest
Table 2).
(Mylar in particular). The magnitude of the contamination is assessed and
the same film batch used throughout the entire analysis.
5. Interferences
5.1 The additive elements found in lubricating oils will 7. Purity of Reagents
affect the measured intensities from the elements of interest to
7.1 Reagent grade chemicals shall be used in all tests.
avaryingdegree.Ingeneralforlubricatingoils,theX-radiation
Unless otherwise indicated, it is intended that all reagents shall
emitted by the element of interest is absorbed by the other
conform to the specifications of the Committee on Analytical
elements in the sample matrix. Also, the X-radiation emitted
from one element can further excite another element. These
effects are significant at concentrations varying from 0.03 A registered trademark of E. I. du Pont de Nemours and Co.
TABLE 2 Lubricants and Additive Materials
Element Compounds Purpose/Application
Barium Sulfonates, Phenates Detergent inhibitors, corrosion inhibitors, detergents, rust inhibitors,
automatic transmission fluids
Calcium Sulfonates, Phenates Detergent inhibitors, dispersants
Phosphorus Dithiophosphates, Phosphates phosphites Anti-rusting agents, extreme pressure additives, anti-wear
Sulfur Base oils, sulfonates, thiophosphates, polysulfides Detergents, extreme pressure additives, anti-wear
and other sulfurized components
Zinc Dialkyldithiophosphates, Dithiocarbamates, Anti-oxidant, corrosion inhibitors, anti-wear additives, detergents,
Phenolates Carboxylates crankcase oils, hypoid gear lubricants, aircraft piston engine oils, turbine
oils, automatic transmission fluids, railroad diesel engine oils, brake
lubricants
D4927 − 14
Reagents of the American Chemical Society, where such ratory needs to evaporate away the petroleum solvent to yield
specifications are available. Other grades may be used, pro- a solution that contains 12.0 6 0.1 mass % zirconium. Other
vided it is first ascertained that the reagent is of sufficiently zirconium containing organic matrices (free of other metals,
high purity to permit its use without lessening the accuracy of sulfur, and phosphorus) may be substituted, provided the
the determination. zirconium is stable in solution and the concentration is known
and does not exceed 12.0 6 0.1 mass % zirconium. If the
TEST METHOD A (INTERNAL STANDARD
zirconium concentration is <12.0 6 0.1 mass %, the laboratory
PROCEDURE)
needs to evaporate away the petroleum solvent to yield a
solution that contains 12.0 6 0.1 mass % zirconium.
8. Reagents and Materials
8.4.4 Lead Naphthenate, containing 24.0 6 0.1 mass %
8.1 Helium, for optical path of spectrometer.
lead.
8.2 P-10 Ionization Gas,90volume%argonand10volume
8.5 Calibration Standard Materials:
% methane for the flow proportional counter.
NOTE 3—In addition to calibration standards identified in 8.5.1 – 8.5.5,
single-elementormultielementcalibrationstandardsmayalsobeprepared
8.3 Diluent Solvent, a suitable solvent free of metals, sulfur,
from materials similar to the samples being analyzed, provided the
and phosphorus (for example, kerosine, white oil, or xylenes).
calibration standards to be used have previously been characterized by
8.4 Internal Standard Materials :
independent primary (for example, gravimetric or volumetric) analytical
techniques to establish the elemental concentration mass % levels.
8.4.1 Nickel Octoate, preferably containing 5.0 6 0.1
mass % nickel. If the nickel concentration is higher or lower
8.5.1 Barium 2-Ethylhexoide or Sulfonate, with concentra-
(minimum concentration that can be used is 2.5 6 0.1 mass %
tions ≥4 mass % barium and certified to better than 60.1 %
nickel), the laboratory needs to adjust the amount of sample
absolute (95 % confidence limit), so that calibration standards
taken in 9.1 to yield an equivalent nickel concentration level in
can be prepared as stated in 10.1.1 and 10.1.2.
the internal standard. Other nickel-containing organic matrices
8.5.2 Calcium Octoate or Sulfonate,withconcentrations≥4
(free of other metals, sulfur, and phosphorus) may be substi-
mass % calcium and certified to better than 60.1 % absolute
tutedprovidedthenickelisstableinsolution,theconcentration
(95 % confidence limit), so that calibration standards can be
is known (≥2.5 6 0.1 mass % nickel), and the laboratory can
prepared as stated in 10.1.1 and 10.1.2.
adjust the amount of sample taken in 9.1 to yield an equivalent
8.5.3 Bis(2-Ethylhexyl)Hydrogen Phosphate, 97 % purity
nickel concentration level in the internal standard if the nickel
(9.62 mass % phosphorus). Other phosphorus containing or-
concentration does not initially contain 5.0 6 0.1 mass %
ganic matrices (free of other metals) may be substituted
nickel.
provided the phosphorus is stable in solution and the concen-
tration is ≥4 mass % phosphorus and certified to better than
NOTE 2—Many X-ray tubes emit copper X rays which increase in
60.1 % absolute (95 % confidence limit), so that calibration
intensity with age. This does not present a problem when using copper as
an internal standard for zinc providing that frequent calibrations are
standards can be prepared as stated in 10.1.1 and 10.1.2.
performed. No problem exists when using nickel as internal for zinc and
8.5.4 Zinc Sulfonate or Octoate, with concentration ≥4
nickel is the preferred internal standard material.
mass %zincandcertifiedtobetterthan 60.1 %absolute(95 %
8.4.2 Titanium 2-Ethylhexoide or Tin Octoate, preferably
confidence limit), so that calibration standards can be prepared
containing 8.0 6 0.1 mass % titanium or tin. If the titanium or
as stated in 10.1.1 and 10.1.2.
tin concentration is higher or lower (minimum concentration
8.5.5 Di-n-Butyl Sulfide, 97 % purity, (21.9 mass % sulfur).
that can be used is 4.0 6 0.1 mass % titanium or tin), the
Other sulfur containing organic matrices (free of metals) may
laboratory needs to adjust the amount of sample taken in 9.1 to
be substituted, provided the sulfur is stable in solution and the
yield an equivalent titanium or tin concentration level in the
concentration is ≥2 mass % sulfur and certified to better than
internal standard. Other titanium or tin containing organic
60.1% absolute (95 % confidence limit), so that calibration
matrices (free of other metals, sulfur, and phosphorus) may be
standards can be prepared as stated in 10.1.2.
substituted, provided the titanium or tin is stable in solution,
8.6 Quality Control (QC) Samples, preferably are portions
the concentration is known (≥4.0 6 0.1 mass % titanium or
of one or more lubricating oils or additives that are stable and
tin), and the laboratory can adjust the amount of sample taken
representative of the samples of interest. These QC samples
in 9.1 to yield an equivalent titanium or tin concentration level
can be used to check the validity of the testing process and
in the internal standard if the titanium or tin concentration does
performance of the instrument as
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4927 − 10 D4927 − 14
Standard Test Methods for
Elemental Analysis of Lubricant and Additive Components—
Barium, Calcium, Phosphorus, Sulfur, and Zinc by
Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
This standard is issued under the fixed designation D4927; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*
1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at
element concentration ranges shown in Table 1. The range can be extended to higher concentrations by dilution of sample
specimens. Additives can also be determined after dilution. Two different methods are presented in these test methods.
1.2 Test Method A (Internal Standard Procedure)—Internal standards are used to compensate for interelement effects of X-ray
excitation and fluorescence (see Sections 8 through 13).
1.3 Test Method B (Mathematical Correction Procedure)—The measured X-ray fluorescence intensity for a given element is
mathematically corrected for potential interference from other elements present in the sample (see Sections 14 through 19).
1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
3. Summary of the Test Methods
3.1 A sample specimen is placed in the X-ray beam and the intensity of the appropriate fluorescence lines of barium, calcium,
phosphorus, sulfur, and zinc are measured. Instrument response factors related to the concentration of standards enable the
determination of the concentration of elements in the tested sample specimens. Enhancement or depression of the X-ray
fluorescence of a given element by an interfering element in the sample may occur. Two test methods (A and B) are described for
compensating any interference effect.
3.2 Test Method A (Internal Standard Procedure)—Internal standards are used with the standards and sample specimens to
compensate for the potential interelement effects.
3.2.1 Barium, Calcium, Phosphorus, and Zinc—A sample specimen that has been blended with a single internal standard
solution (containing tin or titanium for barium and calcium, zirconium for phosphorus, and nickel for zinc) is poured into an X-ray
cell. Total net counts (peak intensity—background) for each element and its respective internal standard are collected at their
appropriate wavelengths. The ratios between elemental and internal standard counts are calculated and converted into barium,
calcium, phosphorus, or zinc concentrations, or a combination thereof, from calibration curves.
3.2.2 Sulfur—A sample specimen is mixed with a lead internal standard solution and analyzed as described in 3.2.1.
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and are the direct responsibility
of Subcommittee D02.03 on Elemental Analysis.
Current edition approved July 1, 2010Dec. 1, 2014. Published July 2010January 2015. Originally approved in 1989. Last previous edition approved in 20052010 as
D4927D4927 – 10.–05. DOI: 10.1520/D4927-10.10.1520/D4927-14.
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 the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4927 − 14
TABLE 1 Range of Applicability
Element Range, Mass %
Barium 0.04-8.5
Calcium 0.01-1.0
Phosphorus 0.01-0.5
Sulfur 0.1-4.0
Zinc 0.01-0.6
3.3 Test Method B (Mathematical Correction Procedure)—The measured intensity for a given element is mathematically
corrected for the interference from other elements in the sample specimen. This requires that intensities from all elements in the
specimen be obtained.
3.3.1 The sample specimen is placed in the X-ray beam and the intensities of the fluorescence lines of barium, calcium,
phosphorus, sulfur, and zinc are measured. A similar measurement is made away from the fluorescence lines in order to obtain a
background correction. Concentrations of the elements of interest are determined by comparison of net signals against appropriate
interelement correction factors developed from responses of calibration standards.
3.3.2 The X-ray fluorescence spectrometer is initially calibrated with a suite of standards in order to determine by regression
analysis, interelement correction factors and instrument response factors.
3.3.3 Subsequent calibration is achieved using a smaller number of standards since only the instrument response factors need
to be redetermined. One of these standards (or an optional synthetic pellet) can be used to monitor instrumental drift when
performing a high volume of analyses.
3.4 Additives and additive packages can be determined after dilution with base oil to place the elemental concentrations in the
range described in 1.1.
4. Significance and Use
4.1 Some oils are formulated with organo-metallic additives which act as detergents, antioxidants, antiwear agents, and so forth.
Some of these additives contain one or more of these elements: barium, calcium, phosphorus, sulfur, and zinc. These test methods
provide a means of determining the concentration of these elements which in turn provides an indication of the additive content
of these oils.
4.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (see Table
2).
5. Interferences
5.1 The additive elements found in lubricating oils will affect the measured intensities from the elements of interest to a varying
degree. In general for lubricating oils, the X-radiation emitted by the element of interest is absorbed by the other elements in the
sample matrix. Also, the X-radiation emitted from one element can further excite another element. These effects are significant at
concentrations varying from 0.03 mass % due to the heavier elements to 1 mass % for the lighter elements. The measured intensity
for a given element can be mathematically corrected for the absorption of the emitted radiation by the other elements present in
the sample specimen. Suitable internal standards can also compensate for X-ray inter-element effects. If an element is present at
significant concentrations and an interelement correction for that element is not employed, the results can be low due to absorption
or high due to enhancement.
TABLE 2 Lubricants and Additive Materials
Element Compounds Purpose/Application
Barium Sulfonates, Phenates Detergent inhibitors, corrosion inhibitors, detergents, rust inhibitors,
automatic transmission fluids
Calcium Sulfonates, Phenates Detergent inhibitors, dispersants
Phosphorus Dithiophosphates, Phosphates phosphites Anti-rusting agents, extreme pressure additives, anti-wear
Sulfur Base oils, sulfonates, thiophosphates, polysulfides Detergents, extreme pressure additives, anti-wear
and other sulfurized components
Zinc Dialkyldithiophosphates, Dithiocarbamates, Anti-oxidant, corrosion inhibitors, anti-wear additives, detergents,
Phenolates Carboxylates crankcase oils, hypoid gear lubricants, aircraft piston engine oils, turbine
oils, automatic transmission fluids, railroad diesel engine oils, brake
lubricants
D4927 − 14
6. Apparatus
6.1 X-Ray Spectrometer, equipped for soft X-ray detection of radiation in the range from 1 to 10 A˚. For optimum sensitivity,
the spectrometer is equipped with the following:
6.1.1 X-Ray Generating Tube, with chromium, rhodium, or scandium target. Other targets can also be employed.
6.1.2 Helium, purgeable optical path.
6.1.3 Interchangeable Crystals, germanium, lithium fluoride (LiF ), graphite, or pentaerythritol (PET), or a combination
thereof. Other crystals can also be used.
6.1.4 Pulse-Height Analyzer, or other means of energy discrimination.
6.1.5 Detector, flow proportional, or scintillation, or flow proportional and scintillation counter.
6.2 Shaker, Mechanical Stirrer, or Ultrasonic Bath, capable of handling from 30-mL to 1-L bottles.
6.3 X-Ray Disposable Plastic Cells, with suitable film window. Suitable films include Mylar, polypropylene, or polyimid with
film thicknesses between 0.25 to 0.35 mil (6.3 to 8.8 μm).
NOTE 1—Some films contain contamination of the elements of interest (Mylar in particular). The magnitude of the contamination is assessed and the
same film batch used throughout the entire analysis.
7. Purity of Reagents
7.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
TEST METHOD A (INTERNAL STANDARD PROCEDURE)
8. Reagents and Materials
8.1 Helium, for optical path of spectrometer.
8.2 P-10 Ionization Gas, 90 volume % argon and 10 volume % methane for the flow proportional counter.
8.3 Diluent Solvent, a suitable solvent free of metals, sulfur, and phosphorus (for example, kerosine, white oil, or xylenes).
8.4 Internal Standard Materials :
8.4.1 Nickel Octoate, preferably containing 5.0 6 0.1 mass % nickel. If the nickel concentration is higher or lower (minimum
concentration that can be used is 2.5 6 0.1 mass % nickel), the laboratory needs to adjust the amount of sample taken in 9.1 to
yield an equivalent nickel concentration level in the internal standard. Other nickel-containing organic matrices (free of other
metals, sulfur, and phosphorus) may be substituted provided the nickel is stable in solution, the concentration is known (≥2.5 6
0.1 mass % nickel), and the laboratory can adjust the amount of sample taken in 9.1 to yield an equivalent nickel concentration
level in the internal standard if the nickel concentration does not initially contain 5.0 6 0.1 mass % nickel.
NOTE 2—Many X-ray tubes emit copper X rays which increase in intensity with age. This does not present a problem when using copper as an internal
standard for zinc providing that frequent calibrations are performed. No problem exists when using nickel as internal for zinc and nickel is the preferred
internal standard material.
8.4.2 Titanium 2-Ethylhexoide or Tin Octoate, preferably containing 8.0 6 0.1 mass % titanium or tin. If the titanium or tin
concentration is higher or lower (minimum concentration that can be used is 4.0 6 0.1 mass % titanium or tin), the laboratory
needs to adjust the amount of sample taken in 9.1 to yield an equivalent titanium or tin concentration level in the internal standard.
Other titanium or tin containing organic matrices (free of other metals, sulfur, and phosphorus) may be substituted, provided the
titanium or tin is stable in solution, the concentration is known (≥4.0 6 0.1 mass % titanium or tin), and the laboratory can adjust
the amount of sample taken in 9.1 to yield an equivalent titanium or tin concentration level in the internal standard if the titanium
or tin concentration does not initially contain 8.0 6 0.1 mass % titanium or tin.
8.4.3 Zirconium Octoate, preferably containing 12.0 6 0.1 mass % zirconium. If the laboratory uses zirconium octoate with a
lower mass % zirconium concentration level, the laboratory needs to evaporate away the petroleum solvent to yield a solution that
contains 12.0 6 0.1 mass % zirconium. Other zirconium containing organic matrices (free of other metals, sulfur, and phosphorus)
may be substituted, provided the zirconium is stable in solution and the concentration is known and does not exceed 12.0 6 0.1
mass % zirconium. If the zirconium concentration is <12.0 6 0.1 mass %, the laboratory needs to evaporate away the petroleum
solvent to yield a solution that contains 12.0 6 0.1 mass % zirconium.
8.4.4 Lead Naphthenate, containing 24.0 6 0.1 mass % lead.
A registered trademark of E. I. du Pont de Nemours and Co.
Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D4927 − 14
8.5 Calibration Standard Materials:
NOTE 3—In addition to calibration standards identified in 8.5.1 – 8.5.5, single-element or multielement calibration standards may also be prepared from
materials similar to the samples being analyzed, provided the calibration standards to be used have previously been characterized by independent primary
(for example, gravimetric or volumetric) analytical techniques to establish the elemental concentration mass % levels.
8.5.1 Barium 2-Ethylhexoide or Sulfonate, with concentrations ≥4 mass % barium and certified to better than 60.1 % absolute
(95 % confidence limit), so that calibration standards can be prepared as stated in 10.1.1 and 10.1.2.
8.5.2 Calcium Octoate or Sulfonate, with concentrations ≥ 4 mass % calcium and certified to better than 60.1 % absolute (95 %
confidence limit), so that calibration standards can be prepared as stated in 10.1.1 and 10.1.2.
8.5.3 Bis(2-Ethylhexyl)Hydrogen Phosphate, 97 % purity (9.62 mass % phosphorus). Other phosphorus cont
...
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