ASTM_D_2332_-_13.pdf

Designation:D233213Standard Practice forAnalysis of Water-Formed Deposits by Wavelength-Dispersive X-Ray Fluorescence1This standard is issued under the fixed designation D2332;the number immediately following the designation 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.1.Scope1.1 This practice covers X-ray spectrochemical analysis ofwater-formed deposits.1.2 The practice is applicable to the determination ofelements of atomic number 11 or higher that are present insignificant quantity in the sample(usually above 0.1%).1.3 The values stated in SI units are to be regarded asstandard.1.4 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 Documents2.1 ASTM Standards:2D887 Practices for Sampling Water-Formed DepositsD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Terminology3.1 For definitions of terms used in this practice,refer toTerminology D1129.4.Summary of Practice4.1 The sample or its fusion with a suitable flux is powderedand the powder is compacted(mounted).The mount is thenirradiated by an X-ray beam of short wavelength(high energy).The characteristic X rays of the atom that are emitted orfluoresced upon absorption of the primary or incident X raysare dispersed,and intensities at selected wavelengths aremeasured by sensitive detectors.Detector output is related toconcentration by calibration curves or charts.4.2 The K spectral lines are used for elements of atomicnumbers 11 to 50.Whether the K or L lines are used for theelements numbered 51 or higher depends on the availableinstrumentation.5.Significance and Use5.1 Certain elements present in water-formed deposits areidentified.Concentration levels of the elements are estimated.5.2 Deposit analysis assists in providing proper water con-ditioning.5.3 Deposits formed from or by water in all its phases maybe further classified as scale,sludge,corrosion products,orbiological deposits.The overall composition of a deposit orsome part of a deposit may be determined by chemical orspectrographic analysis;the constituents actually present aschemical substances may be identified by microscope or X-raydiffraction studies.Organisms may be identified by micro-scopical or biological methods.6.Apparatus6.1 Sample Preparation Equipment:6.1.1 Fusion Crucibles,prepared from 25-mm(1-in.)commercial-grade graphite rods.The dimensions shall be 29mm(118in.)high,an inside diameter of 19 mm(34in.),and acavity 22 mm(78in.)deep.6.1.2 Pulverizers,including an agate or mullite mortar andpestle,minimum capacity 25 ml.6.1.3 SievesNo.100(150-m)and No.270(53-m)asspecified in Specification E11.6.1.4 CompactorsA press,equipped with a gauge en-abling reproducible pressure,is recommended.6.2 Excitation Source(X-ray Tube):6.2.1 Stable Electrical Power Supply(61%).6.2.2 Source of high-intensity,short-wave-length X rays.6.3 Sample Housing(Turret).1This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.03 on Sampling Water andWater-Formed Deposits,Analysis of Water for Power Generation and Process Use,On-Line Water Analysis,and Surveillance of Water.Current edition approved Jan.1,2013.Published February 2013.Originallyapproved in 1965.Last previous edition approved in 2008 as D2332 08.DOI:10.1520/D2332-13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.4 SpectrometerBest resolution of the spectrometer andbest sensitivity are not simultaneously attainable;a compro-mise is effected to give adequate values for each.6.4.1 Collimating System.6.4.2 Spectrogoniometer.6.4.3 Analyzing Crystal and HolderThe choice of theanalyzing crystal is made on the basis of what elements mustbe determined;for example,a gypsum or an ammoniumdihydrogen phosphate crystal can be used for determiningmagnesium but lithium fluoride is much superior for copperand iron(high-intensity diffracted secondary rays and conse-quently greater sensitivity and potential precision).A salt,sodium chloride(NaCl),crystal is frequently employed forgeneral use,being applicable over a broad range and producingintense lines and medium broadening.6.4.4 Counter-Tube Support.6.5 Evacuating or Flushing System.6.6 Measuring System:6.6.1 Detector(of which the principal t