ASTM C1271-99(2006)
(Test Method)Standard Test Method for X-ray Spectrometric Analysis of Lime and Limestone
Standard Test Method for X-ray Spectrometric Analysis of Lime and Limestone
SIGNIFICANCE AND USE
This procedure is suitable for manufacturing control and verifying that the product meets specifications. It provides rapid, multi-element determinations with sufficient accuracy to ensure product quality and minimize production delays. The analytical performance data included may be used as a benchmark to determine whether similar X-ray spectrometers provide equivalent precision and accuracy, or whether the performance of a particular X-ray spectrometer has changed.
SCOPE
1.1 This test method covers the X-ray emission spectrometric analysis of limestone, quicklime, hydrated lime, and hydraulic lime using wavelength dispersive instruments.
1.2 The values stated in SI units are to be regarded as the standard.
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. Specific precautionary statements are given in Section .
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: C1271 − 99(Reapproved 2006)
Standard Test Method for
X-ray Spectrometric Analysis of Lime and Limestone
This standard is issued under the fixed designation C1271; 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 E1361 Guide for Correction of Interelement Effects in
X-Ray Spectrometric Analysis
1.1 This test method covers the X-ray emission spectromet-
2.2 NIST Documents:
ric analysis of limestone, quicklime, hydrated lime, and hy-
ANSI-NIST Handbook 114
draulic lime using wavelength dispersive instruments.
NIST Standards Catalog
1.2 The values stated in SI units are to be regarded as the
standard.
3. Terminology
1.3 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 emission spectroscopy—unless otherwise specified,
responsibility of the user of this standard to establish appro-
for definitions of terms used in this test method pertaining to
priate safety and health practices and determine the applica-
emission spectroscopy, refer to Terminology E135.
bility of regulatory limitations prior to use. Specific precau-
3.1.2 lime—unless otherwise specified, for definitions of
tionary statements are given in Section 10.
terms used in this test method pertaining to lime, refer to
2. Referenced Documents
Terminology C51.
3.1.3 statistical—unless otherwise specified, for definitions
2.1 ASTM Standards:
C25 Test Methods for Chemical Analysis of Limestone, of terms used in this test method pertaining to statistics, refer
to Terminology E456.
Quicklime, and Hydrated Lime
C50 Practice for Sampling, Sample Preparation, Packaging,
4. Summary of Test Method
and Marking of Lime and Limestone Products
C51 Terminology Relating to Lime and Limestone (as used
4.1 A briquetted powder specimen or a fused-glass disk
by the Industry)
specimen is irradiated by a high-energy X-ray beam. The
E50 Practices for Apparatus, Reagents, and Safety Consid-
secondary X rays produced are dispersed by means of crystals,
erations for Chemical Analysis of Metals, Ores, and
and the intensities are measured by suitable detectors at
Related Materials
selected wavelengths. Data are collected based on the time
E135 Terminology Relating to Analytical Chemistry for
required to reach a fixed number of counts, total count for a
Metals, Ores, and Related Materials
fixed time, or integration of voltage for a fixed time. Concen-
E305 Practice for Establishing and Controlling Atomic
trations of the elements are determined by relating the mea-
Emission Spectrochemical Analytical Curves
sured radiation of unknown specimens to analytical curves
E456 Terminology Relating to Quality and Statistics
prepared from reference materials of known composition.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
5. Significance and Use
E1060 Practice for Interlaboratory Testing of Spectrochemi-
5.1 Thisprocedureissuitableformanufacturingcontroland
cal Methods of Analysis (Withdrawn 1997)
verifying that the product meets specifications. It provides
rapid, multi-element determinations with sufficient accuracy to
This test method is under the jurisdiction of ASTM Committee C07 on Lime
ensure product quality and minimize production delays. The
and is the direct responsibility of Subcommittee C07.05 on Chemical Tests.
analytical performance data included may be used as a bench-
Current edition approved Feb. 15, 2006. Published March 2006. Originally
mark to determine whether similar X-ray spectrometers pro-
approved in 1994. Last previous edition approved in 1999 as C1271 – 99. DOI:
vide equivalent precision and accuracy, or whether the perfor-
10.1520/C1271-99R06.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
mance of a particular X-ray spectrometer has changed.
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.
3 4
The last approved version of this historical standard is referenced on Available from National Institute of Standards and Technology (NIST), 100
www.astm.org. Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1271 − 99 (2006)
6. Interferences radiation of the specimen for the elements specified. The
generator may be equipped with a line voltage regulator and
6.1 Interelementeffectsormatrixeffectsmayexistforsome
current stabilizer.
of the elements listed. One way to compensate for these effects
7.4.2 X-Ray Tubes, with targets of various high-purity
is to prepare a series of calibration curves to cover the
elements, capable of continuous operation at required poten-
designated concentration ranges.The composition of the speci-
tials and currents, and that will excite the elements to be
men being analyzed must match closely the composition of the
determined.
reference materials used to prepare the calibration curve.
Mathematicalcorrections,derivedfromempiricalrelationships 7.5 Spectrometer, designed for X-ray emission analysis and
or fundamental parameter calculations, may be used alterna- equipped with specimen holders and a specimen chamber. The
tively.Anyoftheseareacceptable,providingthattheanalytical chamber may contain a specimen spinner, and it must be
accuracy required by this test method is achieved. equipped for vacuum operation.
7.5.1 Analyzing Crystals—Flat or curved crystals with op-
6.2 Calcium is the primary component of the matrix ana-
timizedcapabilityfordiffractionofthewavelengthsofinterest.
lyzed by this test method. The analyst must be aware of all
7.5.2 Collimator, for limiting the characteristic X rays to a
possible interferences and matrix effects of this element.
parallel bundle when flat crystals are used in the instrument.A
Ordersofallwavelengthsmaycauseinterference,forexample,
collimator is not necessary for curved crystal optics.
the effect of CaKβ1 (2nd order) on PKα1.
7.5.3 Detectors, sealed or gas flow, proportional type, Gei-
6.3 Contamination from the grinding apparatus is an ever-
ger counters, scintillation counters or equivalent.
presentsourceofinterferenceofwhichtheanalystmustalways
7.5.4 Vacuum System, providing for the determination of
be cognizant. For example, stainless steel will impart iron,
elements whose radiation is absorbed by air (atomic number
chrome, and nickel to the prepared sample.
below 20). The system shall consist of at least one vacuum
pump, gage, and electrical controls to provide automatic
6.4 Spectral interferences from the X-ray tube may also
pumpdown of the optical path and maintain a controlled
occur, for example, line overlap from CrKβ1onMnKα1
pressure, usually 13 Pa or less.
caused by a chrome target tube.
7.6 Measuring System, consisting of electronic circuits ca-
7. Apparatus
pable of counting or integrating pulses received from the
detectors.Thecounts,countrate,orintegratedvoltagesmaybe
7.1 Specimen Preparation Equipment:
displayed on meters, recorders, digital counters, or voltmeters.
7.1.1 Jaw Crusher, for initial crushing of lumps.
The counts, count rates, or integrated voltages can also be
7.1.2 Plate Grinder or Pulverizer, with one static and one
presented to a computer or programmable calculator for
rotating disk for further grinding.
conversion to percent concentration. Pulse height analyzers
7.1.3 Rotary Disk Mill or Shatter Box, with hardened
may be required to provide more accurate measurements for
grinding containers and timer control for final grinding.
some measurements.
7.2 Briquetting Equipment:
7.2.1 Briquetting Press, capable of providing pressures up
8. Reagents and Materials
to 550 MPa (80 000 psi). The press shall be equipped with a
8.1 Purity and Concentration of Reagents—The purity and
mold assembly that provides a briquet compatible with the
concentration of chemical reagents shall conform to the re-
X-ray specimen holder.
quirements prescribed in Practices E50.
7.3 Fusion Equipment:
8.2 Binders—Various binders have been used successfully
7.3.1 Furnace or Gas Burners, with a timer, capable of
topreparebriquettessuitableforpresentationtotheinstrument.
heating the sample and flux to at least 1000 °C and homog-
Asageneralrule,thebindershouldnotcontainanelementthat
enizing the melt.
will be determined. In addition, the sample to binder ratio must
7.3.2 Fusion Crucibles:
be present in the analytical sample as in the reference materials
7.3.2.1 Vitreous Carbon or Graphite, 20 to 30-mLcapacity,
that were used to establish the calibration.
with a flat bottom 30 to 35 mm in diameter.
8.3 Fluxes—Various fluxes have been used successfully to
7.3.2.2 Platinum/Gold, 95 % platinum/5 % gold alloy, 30 to
prepare fusion disks.The flux must be capable of dissolving or
35-mL capacity.
dispersing the analyzed elements in an homogeneous and
7.3.2.3 Platinum/Gold Casting Dish, 95 % platinum/5 %
reproducible fashion in the melt. The prepared disks must then
gold alloy, 30 to 35-mL capacity, with a flat bottom 30 to 35
be suitable for presentation to the instrument.
mm in diameter.
7.3.3 Polishing Wheel, suitable for polishing the fusion disk 8.4 Detector Gas (P-10), consisting of a mixture of 90 %
to obtain a uniform surface for irradiation. The analyst should
argon and 10 % methane for use with gas flow proportional
be aware at all times of possible contamination from the counters only.
polishing media used for surfacing the disk (6.3).
9. Reference Materials
7.4 Excitation Source:
7.4.1 X-Ray Tube Power Supply, providing constant poten- 9.1 Certified reference materials are available from the
tialorrectifiedpowerofsufficientenergytoproducesecondary National Institute for Standards and Technology (NIST) and
C1271 − 99 (2006)
other international certification agencies. Refer to Test Meth- given in Table 1. Once established, control all instrument
ods C25 for a current listing. parameters closely to ensure repeatable analyses.
9.2 Reference materials with matrixes similar to that of the
14. Calibration and Standardization
test specimen and containing varying amounts of the elements
14.1 Calibration (Preparation of Analytical Curves)—
to be determined may be used provided that they have been
Select a sufficient number of reference materials to cover the
analyzed in accordance with ASTM standard test methods.
concentration ranges of the elements sought.Average duplicate
9.3 Standard additions method or spiked samples may also
intensity measurements of each reference material, and estab-
be used to create standards for which appropriate reference
lish a calibration curve for each element in accordance with
materials are not available for an element desired to be
Practice E305. Establish the curve by a least squares or
analyzed. The matrix material must match that of the test
multiple regression fit of the X-ray intensity measurements
specimen.
versus the corresponding weight percent concentrations of the
element in the reference materials.
10. Safety Precautions
14.2 Standardization (Analytical Curve Adjustment)—
10.1 Occupational health and safety standards for ionizing
Verify that the calibration curve for each element has not
radiation shall be observed at all X-ray emission spectrometer
drifted using a control reference material. Drift is indicated by
installations. It is also recommended that operating and main-
a change in counts that exceeds the normal variation of counts
tenance personnel follow the guidelines of safe operating
for that element. A change of 1 % or greater usually signifies
procedures given in current handbooks and publications from
that the calibration curve for that element has drifted and
the original equipment manufacturer, NIST, U.S. Government
should thus be adjusted. Re-measure the reference materials to
Printing Office, or similar handbooks on radiation safety. See
verify that acceptable analyses are obtained after the adjust-
NIST Standards Catalog and ANSI-NIST Handbook 114.
ments are made.
10.2 Personnel—X-ray equipment shall be used only under
theguidanceandsupervisionofaresponsible,qualifiedperson.
15. Procedure
10.3 Monitoring Devices—Either film badges or dosimeters
15.1 Excitation—Introduce the specimen into the specimen
shall be worn by all operating and maintenance personnel.
chamber, using care not to contaminate the surface to be
Periodic radiation surveys of the equipment for leaks and
excited. Produce the secondary fluorescence using the equip-
excessive scattered radiation shall be made by a qualified
ment used in 7.4.
person using an ionization chamber detector to meet local,
15.2 Radiation Measurements—Obtain and record the
state, and federal radiation standards. The personal film badge
countingratemeasurementforeachelement.Eitherfixedcount
survey record, the radiation survey record, and an equipment
or fixed time modes may be used. A predetermined minimum
maintenance record shall be available upon request.
count rate is obtainable only after unacceptable long counting
10.4 Special precautions for operators and maintenance
timesforlimematerials,withtheexceptionofthemajoroxides
personnel shall be posted at the equipment site.
(Si, Fe, Al, Ca, and Mg). A minimum counting time of 60 s is
acceptable.
10.5 Radiation caution signs shall be posted near the X-ray
equipment and at all entrances to the radiation area.
15.3 Spectral Interferences—Some X-ray spectrometers
will not resolve radiation completely from several line over-
10.6 Fail-Safe “X-ray on” warning lights shall be used on
laps. Care must therefore be exercised in these cases.Alternate
the equipment.
wavelengths without interference may be used. Otherwise,
11. Sampling
mathematical calculations must be used to correct for the
interferences.
11.1 Gross sample is to be taken in accordance with
Methods C50.
11.2 Sample preparation is to be performed in accordance
TABLE 1 Analytical Lines and Crystals
with Methods C50 and Test Methods C25.
Element Wavelength, A Crystals
11.3 Special preparation may be required to grind the
Sodium 11.91 TLAP, multilayer
Magnesium 9.889 ADP, TLAP, RAP, multilayer
analytical sample finer than is required in 11.2.
Aluminum 8.338 PET, EDdT, RAP
Silicon 7.126 PET, EDdT, RAP, InSb
12. Preparation of Reference Materials and Test
Phosphorus 6.155 Ge, PET
Specimens Sulfur 5.373 Ge, PET, NaCl
Chlorine 4.729 PET, Ge
12.1 Treat reference materials and specimens exactly the
Potass
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