ASTM C1301-1995(2009)e1 Standard Test Method for Major and Trace Elements in Limestone and Lime by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP) and Atomic Absorpti.pdf
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1、Designation: C 1301 95 (Reapproved 2009)1Standard Test Method forMajor and Trace Elements in Limestone and Lime byInductively Coupled Plasma-Atomic Emission Spectroscopy(ICP) and Atomic Absorption (AA)1This standard is issued under the fixed designation C 1301; the number immediately following the d
2、esignation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEA units statement was added editor
3、ially as new paragraph 1.3 and subsequent paragraphs were renumbered in June2009.1. Scope1.1 The following test method covers the use of inductivelycoupled plasma-atomic emission spectroscopy (ICP) andatomic absorption spectroscopy (AA) in the analysis of majorand trace elements in limestone and lim
4、e (calcined limestone).1.2 Table 1 lists some of the elements that can be analyzedby this test method and the preferred wavelengths. Also seeU.S. EPA Methods 200.7 and 200.9.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.
5、4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Doc
6、uments2.1 ASTM Standards:2C51 Terminology Relating to Lime and Limestone (as usedby the Industry)D 1193 Specification for Reagent WaterE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 863 Practice for Describing Atomic Absorption Spectro-metric Equipment3E 1
7、479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission Spectrometers2.2 U.S. EPA Standards:Methods for the Determination of Metals in EnvironmentalSamples; U.S. EPA Methods 200.2, 200.7, and200.9; Smoley, C. K., 19924Method 6010, Inductively Coupled Plasma Method, SW-8
8、46, Test Methods for Evaluating Solid Waste51This test method is under the jurisdiction of ASTM Committee C07 on Limeand is the direct responsibility of Subcommittee C07.05 on Chemical TestsCurrent edition approved June 1, 2009. Published September 2009. Originallyapproved in 1995. Last previous edi
9、tion approved in 2001 as C 1301 95(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last
10、 approved version of this historical standard is referencedon www.astm.org.4Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL33431.5Available from U.S. Government Printing Office, Washington, DC 20402.TABLE 1 Elements and Some Suggested WavelengthsAMajor Elements ICP Wavelength,
11、nm AA Wavelength, nmCalcium 317.933 (315.887)B422.7Magnesium 279.079 (285.213) 285.2Silicon 251.611 (288.160) 251.6Aluminum 308.215 (309.271) 309.3Iron 259.940 248.3Manganese 257.610 279.5Sodium 588.995 (589.59) 589.0Potassium 766.491 766.5Phosphorus 214.914 (213.618) .CStrontium 421.552 460.7Trace
12、Elements ICP Wavelength, nm AA Wavelength, nmAntimony 206.833 217.6Arsenic 193.696 193.7Barium 455.403 (493.409) 553.6Beryllium 313.042 234.9Boron 249.773 249.8Cadmium 226.502 (228.80) 228.8Chromium 267.716 (205.552) 357.9Cobalt 228.616 240.7 (242.5)Copper 324.754 324.8Lead 220.353 217.0 (283.3)Moly
13、bdenum 202.030 (203.844) 313.3Nickel 231.604 (221.647) 232.0Selenium 196.090 196.0Silver 328.068 328.1Sulfur 180.731 (180.669) .CThallium 190.864 276.8Tin 189.989 235.5 (286.3)Vanadium 292.402 318.4Zinc 213.856 (202.551) 213.9AThe suggested wavelengths may vary for your particular instrument.BNumber
14、s in parentheses are alternate wavelengths.CNot recommended or not used.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3. Terminology3.1 DefinitionsDefinitions for terms used in this testmethod can be found in Terminologies C 51 and
15、 E 135.3.2 Additional Definitions:3.2.1 total recoverable, ntrace element concentration inan unfiltered sample after heating in acid.3.2.2 total digestion, ncomplete digestion of a sample,including silica and silicate minerals, using the fusion-fluxmethod.4. Summary of Test Method4.1 A sample, diges
16、ted by either fusion or acid, is atomizedand passed into an excitation medium (a plasma in the case ofICP; a flame in the case ofAA). The resulting ions are analyzedby atomic spectroscopy. Elemental concentrations are deter-mined by graphically relating the emission/absorption at spe-cific wavelengt
17、hs for an unknown sample to analytical curvesmade from reference standards of known composition.5. Significance and Use5.1 The presence and concentration of elements in lime andlimestone is important in determining product quality and itssuitability for various uses. This test method provides a mean
18、sof measuring the major and trace element concentration in limeand limestone.6. Interferences6.1 ChemicalChemical interferences, most common inAA, arise from the formation of molecular compounds thatcause absorbances at the wavelength of interest. This molecu-lar band spectral overlap can be minimiz
19、ed by buffering thesample with matrix modifiers (a Lanthanum additive, forexample), using standard additions techniques, matrix match-ing or by careful selection of operating conditions (for ex-ample, using a hotter nitrous oxide/acetylene flame, selectingan alternate wavelength).6.2 PhysicalPhysica
20、l interferences are the result of theinconsistencies in the introduction of the sample into theinstrument, namely the transport and atomization/nebulizationof the sample. These inconsistencies are a function of changingviscosity and surface tension, and are found primarily insamples of high-dissolve
21、d solids or high-acid concentrations.Physical interferences can be reduced by diluting the sampleand by the use of a peristaltic pump.6.3 SpectralSpectral interference, most common in ICP,consists of overlapping and unresolved peaks. Computer soft-ware, along with the analysis of the suspected inter
22、feringelement, can compensate for this effect. Using an alternatewavelength is also a solution. Another spectral interference iscaused by background, both stray light and continuous spec-trum (continuous argon spectrum, for example). Backgroundcorrection adjacent to the analyte line will correct bac
23、kgroundspectral interference.7. Apparatus7.1 Spectrometer.7.1.1 Inductively Coupled Plasma Emission Spectrometer(ICP)Either a scanning sequential or multi-element simulta-neous type ICP, with resolution appropriate for the elements tobe analyzed. The optical path may be in air, vacuum or an inertgas
24、. A detailed description of an ICP is given in PracticeE 1479.7.1.2 Atomic Absorption Spectrometer (AA)An atomicabsorption spectrometer consisting of single or double beamoptics, a monochromator, photomultiplier detector, adjustableslits, a wavelength range from 190 to 800 nm, and provisionsfor inte
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