ASTM C1271-99
(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
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 10.
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Designation:C1271–99
Standard Test Method for
X-ray Spectrometric Analysis of Lime and Limestone
This standard is issued under the fixed designation C 1271; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 NIST Documents:
ANSI-NIST Handbook 114
1.1 This test method covers the X-ray emission spectromet-
NIST Standards Catalog
ric analysis of limestone, quicklime, hydrated lime, and hy-
draulic lime using wavelength dispersive instruments.
3. Terminology
1.2 The values stated in SI units are to be regarded as the
3.1 Definitions:
standard.
3.1.1 emission spectroscopy—unless otherwise specified,
1.3 This standard does not purport to address all of the
for definitions of terms used in this test method pertaining to
safety concerns, if any, associated with its use. It is the
emission spectroscopy, refer to Terminology E 135.
responsibility of the user of this standard to establish appro-
3.1.2 lime—unless otherwise specified, for definitions of
priate safety and health practices and determine the applica-
terms used in this test method pertaining to lime, refer to
bility of regulatory limitations prior to use. Specific precau-
TerminologyC51.
tionary statements are given in Section 10.
3.1.3 statistical—unless otherwise specified, for definitions
2. Referenced Documents of terms used in this test method pertaining to statistics, refer
to Terminology E 456.
2.1 ASTM Standards:
C25 Test Methods for Chemical Analysis of Limestone,
4. Summary of Test Method
Quicklime, and Hydrated Lime
4.1 A briquetted powder specimen or a fused-glass disk
C50 Methods for Sampling, Inspection, Packing, and
specimen is irradiated by a high-energy X-ray beam. The
Marking of Lime and Limestone Products
secondary X rays produced are dispersed by means of crystals,
C51 Terminology Relating to Lime and Limestone (As
and the intensities are measured by suitable detectors at
Used by the Industry)
selected wavelengths. Data are collected based on the time
E50 Practices for Apparatus, Reagents, and Safety Precau-
required to reach a fixed number of counts, total count for a
tions for Chemical Analysis of Metals
fixed time, or integration of voltage for a fixed time. Concen-
E 135 Terminology Relating to Analytical Chemistry for
3 trations of the elements are determined by relating the mea-
Metals, Ores, and Related Materials
sured radiation of unknown specimens to analytical curves
E 305 Practice for Establishing and Controlling Spectro-
3 prepared from reference materials of known composition.
chemical Analytical Curves
E 456 Terminology Relating to Quality and Statistics
5. Significance and Use
E 691 Practice for Conducting an Interlaboratory Study to
5.1 This procedure is suitable for manufacturing control and
Determine the Precision of a Test Method
verifying that the product meets specifications. It provides
E 1060 Practice for Interlaboratory Testing of Spectro-
rapid, multi-element determinations with sufficient accuracy to
chemical Methods of Analysis
ensure product quality and minimize production delays. The
E 1361 Guide for Correction of Interelement Effects in
analytical performance data included may be used as a bench-
X-Ray Spectrometric Analysis
mark to determine whether similar X-ray spectrometers pro-
vide equivalent precision and accuracy, or whether the perfor-
mance of a particular X-ray spectrometer has changed.
This test method is under the jurisdiction of ASTM Committee C-7 on Lime
6. Interferences
and is the direct responsibility of Subcommittee C07.05 on Chemical Tests.
Current edition approved June 10, 1999. Published July 1999. Originally
6.1 Interelement effects or matrix effects may exist for some
published as C 1271 – 94. Last previous edition C 1271 – 94a.
of the elements listed. One way to compensate for these effects
Annual Book of ASTM Standards, Vol 04.01.
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 03.06.
Available from National Institute for Standards and Technology (NIST),
Gaithersburg, MD 20899.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1271–99
is to prepare a series of calibration curves to cover the 7.5 Spectrometer, designed for X-ray emission analysis and
designated concentration ranges.The composition of the speci- equipped with specimen holders and a specimen chamber. The
men being analyzed must match closely the composition of the chamber may contain a specimen spinner, and it must be
reference materials used to prepare the calibration curve. equipped for vacuum operation.
Mathematicalcorrections,derivedfromempiricalrelationships
7.5.1 Analyzing Crystals—Flat or curved crystals with op-
or fundamental parameter calculations, may be used alterna-
timizedcapabilityfordiffractionofthewavelengthsofinterest.
tively.Anyoftheseareacceptable,providingthattheanalytical
7.5.2 Collimator, for limiting the characteristic X rays to a
accuracy required by this test method is achieved.
parallel bundle when flat crystals are used in the instrument.A
6.2 Calcium is the primary component of the matrix ana-
collimator is not necessary for curved crystal optics.
lyzed by this test method. The analyst must be aware of all
7.5.3 Detectors, sealed or gas flow, proportional type, Gei-
possible interferences and matrix effects of this element.
ger counters, scintillation counters or equivalent.
Ordersofallwavelengthsmaycauseinterference,forexample,
7.5.4 Vacuum System, providing for the determination of
the effect of CaKb1 (2nd order) on PKa1.
elements whose radiation is absorbed by air (atomic number
6.3 Contamination from the grinding apparatus is an ever-
below 20). The system shall consist of at least one vacuum
presentsourceofinterferenceofwhichtheanalystmustalways
pump, gage, and electrical controls to provide automatic
be cognizant. For example, stainless steel will impart iron,
pumpdown of the optical path and maintain a controlled
chrome, and nickel to the prepared sample.
pressure, usually 13 Pa or less.
6.4 Spectral interferences from the X-ray tube may also
7.6 Measuring System, consisting of electronic circuits ca-
occur, for example, line overlap from CrKb1onMnKa1
pable of counting or integrating pulses received from the
caused by a chrome target tube.
detectors.Thecounts,countrate,orintegratedvoltagesmaybe
displayed on meters, recorders, digital counters, or voltmeters.
7. Apparatus
The counts, count rates, or integrated voltages can also be
7.1 Specimen Preparation Equipment:
presented to a computer or programmable calculator for
7.1.1 Jaw Crusher, for initial crushing of lumps.
conversion to percent concentration. Pulse height analyzers
7.1.2 Plate Grinder or Pulverizer, with one static and one
may be required to provide more accurate measurements for
rotating disk for further grinding.
some measurements.
7.1.3 Rotary Disk Mill or Shatter Box, with hardened
grinding containers and timer control for final grinding.
8. Reagents and Materials
7.2 Briquetting Equipment:
7.2.1 Briquetting Press, capable of providing pressures up
8.1 Purity and Concentration of Reagents—The purity and
to 550 MPa (80 000 psi). The press shall be equipped with a
concentration of chemical reagents shall conform to the re-
mold assembly that provides a briquet compatible with the
quirements prescribed in PracticesE50.
X-ray specimen holder.
8.2 Binders—Various binders have been used successfully
7.3 Fusion Equipment:
topreparebriquettessuitableforpresentationtotheinstrument.
7.3.1 Furnace or Gas Burners, with a timer, capable of
As a general rule, the binder should not contain an element that
heating the sample and flux to at least 1000°C and homogeniz-
will be determined. In addition, the sample to binder ratio must
ing the melt.
be present in the analytical sample as in the reference materials
7.3.2 Fusion Crucibles:
that were used to establish the calibration.
7.3.2.1 Vitreous Carbon or Graphite, 20 to 30-mL capacity,
8.3 Fluxes—Various fluxes have been used successfully to
with a flat bottom 30 to 35 mm in diameter.
prepare fusion disks. The flux must be capable of dissolving or
7.3.2.2 Platinum/Gold, 95 % platinum/5 % gold alloy, 30 to
dispersing the analyzed elements in an homogeneous and
35-mL capacity.
reproducible fashion in the melt. The prepared disks must then
7.3.2.3 Platinum/Gold Casting Dish, 95 % platinum/5 %
be suitable for presentation to the instrument.
gold alloy, 30 to 35-mL capacity, with a flat bottom 30 to 35
8.4 Detector Gas (P-10), consisting of a mixture of 90 %
mm in diameter.
argon and 10 % methane for use with gas flow proportional
7.3.3 Polishing Wheel, suitable for polishing the fusion disk
counters only.
to obtain a uniform surface for irradiation. The analyst should
be aware at all times of possible contamination from the
9. Reference Materials
polishing media used for surfacing the disk (6.3).
9.1 Certified reference materials are available from the
7.4 Excitation Source:
National Institute for Standards and Technology (NIST) and
7.4.1 X-Ray Tube Power Supply, providing constant poten-
other international certification agencies. Refer to Test Meth-
tialorrectifiedpowerofsufficientenergytoproducesecondary
odsC25 for a current listing.
radiation of the specimen for the elements specified. The
9.2 Reference materials with matrixes similar to that of the
generator may be equipped with a line voltage regulator and
test specimen and containing varying amounts of the elements
current stabilizer.
to be determined may be used provided that they have been
7.4.2 X-Ray Tubes, with targets of various high-purity
analyzed in accordance with ASTM standard test methods.
elements, capable of continuous operation at required poten-
tials and currents, and that will excite the elements to be 9.3 Standard additions method or spiked samples may also
determined. be used to create standards for which appropriate reference
C1271–99
TABLE 1 Analytical Lines and Crystals
materials are not available for an element desired to be
analyzed. The matrix material must match that of the test Element Wavelength, A Crystals
specimen.
Sodium 11.91 TLAP, multilayer
Magnesium 9.889 ADP, TLAP, RAP, multilayer
Aluminum 8.338 PET, EDdT, RAP
10. Safety Precautions
Silicon 7.126 PET, EDdT, RAP, InSb
Phosphorus 6.155 Ge, PET
10.1 Occupational health and safety standards for ionizing
Sulfur 5.373 Ge, PET, NaCl
radiation shall be observed at all X-ray emission spectrometer
Chlorine 4.729 PET, Ge
installations. It is also recommended that operating and main-
Potassium 3.742 LiF 200, PET
Calcium 3.359 LiF 200, PET
tenance personnel follow the guidelines of safe operating
Titanium 2.750 LiF 200, LiF 220
procedures given in current handbooks and publications from
Manganese 2.103 LiF 200, LiF 220
the original equipment manufacturer, NIST, U.S. Government
Iron 1.937 LiF 200, LiF 220
Printing Office, or similar handbooks on radiation safety. See Strontium 0.8766 LiF 200, LiF 220
Barium 2.775 LiF 200, LiF 220
NIST Standards Catalog and ANSI-NIST Handbook 114.
Lead 1.175 LiF 200, LiF 220
10.2 Personnel—X-ray equipment shall be used only under
theguidanceandsupervisionofaresponsible,qualifiedperson.
10.3 Monitoring Devices—Either film badges or dosimeters
shall be worn by all operating and maintenance personnel. versus the corresponding weight percent concentrations of the
Periodic radiation surveys of the equipment for leaks and
element in the reference materials.
excessive scattered radiation shall be made by a qualified 14.2 Standardization (Analytical Curve Adjustment)—
person using an ionization chamber detector to meet local, Verify that the calibration curve for each element has not
state, and federal radiation standards. The personal film badge drifted using a control reference material. Drift is indicated by
survey record, the radiation survey record, and an equipment a change in counts that exceeds the normal variation of counts
maintenance record shall be available upon request. for that element. A change of 1 % or greater usually signifies
10.4 Special precautions for operators and maintenance that the calibration curve for that element has drifted and
personnel shall be posted at the equipment site. should thus be adjusted. Re-measure the reference materials to
10.5 Radiation caution signs shall be posted near the X-ray verify that acceptable analyses are obtained after the adjust-
equipment and at all entrances to the radiation area. ments are made.
10.6 Fail-Safe “X-ray on” warning lights shall be used on
15. Procedure
the equipment.
15.1 Excitation—Introduce the specimen into the specimen
11. Sampling
chamber, using care not to contaminate the surface to be
11.1 Gross sample is to be taken in accordance with excited. Produce the secondary fluorescence using the equip-
MethodsC50.
ment used in 7.4.
11.2 Sample preparation is to be performed in accordance 15.2 Radiation Measurements—Obtain and record the
with MethodsC50 and Test MethodsC25.
countingratemeasurementforeachelement.Eitherfixedcount
11.3 Special preparation may be required to grind the or fixed time modes may be used. A predetermined minimum
analytical sample finer than is required in 11.2.
count rate is obtainable only after unacceptable long counting
timesforlimematerials,withtheexceptionofthemajoroxides
12. Preparation of Reference Materials and Test
(Si, Fe, Al, Ca, and Mg). A minimum counting time of 60 s is
Specimens
acceptable.
15.3 Spectral Interferences—Some X-ray spectrometers
12.1 Treat reference materials and specimens exactly the
will not resolve radiation completely from several line over-
same way throughout the procedure. Either briquetted powder
laps. Care must therefore be exercised in these cases.Alternate
or fused disk specimens may be used.
wavelengths without interference may be used. Otherwise,
mathematical calculations must be used to correct for the
13. Preparation of Apparatus
interferences.
13.1 Prepare and operate the spectrometer in accordance
with the manufacturer’s instructions, using the parameters
NOTE 1—If a goniometer is used, the setting for the 2 u peak must be
given in Table 1. Once established, control all instrument determined experimentally within each laboratory. Periodic checks to
verify the setting are advisable.
parameters closely to ensure repeatable analyses.
15.4 Replicate Measurements—Make a minimum of two
14. Calibration and Standardization
measureme
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