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analyte concentrations also listed In Table 3 At present, information on the listed Silver and potassium wavelengths are not available but It has been reported that second order energy from the magnesium 383 231 nm wavelength Interferes with the listed potassium line at 766491 nm 5.1.2 Physical mterferences are generally considered to be effects associated with the sample nebuliza- tion and transport processes Such properties as change In VISCOSity and surface tension can cause Significant inaccuracies especially In samples which may contain high dissolved solids and/or acid concentrations The use of a penstaltlc pump may lessen these Interferences If these types of Interferences are operative. they must be reduced by dilution of the sample and/or utilization of standard addition techniques Another problem which can occur from high dissolved solids is salt bUildup at the tiP of the nebulizer This affects aersol flow-rate causing Instrumental dnft Wetting the argon prior to nebulization, the use of a tip washer, or sample dilution have been used to control this problem. Also. It has been reported that better control of the argon flow rate Improves instrument performance This IS accomplished with the use of mass flow controllers 5 1.3 procedures These types of Interferences can be hIghly dependent on matrix type and the speCifiC analyte erement 6.2 It IS recommended that whenever a new or unusual sample matrix is encountered, a senes of tests be performed pnor to reporting concentration data for analyte elements These tests. as outlined In 5 2 1 through 5 2 4, Will ensure the analyst that neither POSitive nor negatlve interference effects are operative on any of the analyte el- ements thereby dIstorting the accuracy of the reported values 5 2 1 Sertal dIlutIon-If the analyte concentration IS suffiCiently high (mln- Imally a factor of 10 above the instru- mental detection limit after dilutIon), an analySIS of a dilution should agree Within 5 % of the onglnal determina- tion (or Within some acceptable con- trol limit (143) that has been estab- lished for that matnx) If not. a chemical or phYSical Interference ef- fect should be sl,lspected 5 2 2 Spike additIOn-The recovery of a spike addition added at a mInimum level of lOX the in- strumental detectIOn limit (maximum 100X) to the onglnal determinatIOn should be recovered to Within 90 to 110 percent or Within the established control limit for that matnx If not, a matnx effect should be suspected The use of a standard addition analySIS procedure can usually compensate for thiS effect Caution The standard ad- dition technique does not detect COin- Cident spectral overlap If suspected, use of computenzed compensatIon, an alternate wavelength, or companson With an alternate method IS recom- mended (See 5 2 3) responsibility of the analyst to venfy that the Instrument configuration and operating conditions used satIsfy the analytical reqUirements and to maintain quality control data confirming Instrument performance and analytical results 7 Reagents and standards 7 1 ACids used In the preparation of standards and for sample processing must be ultra-high punty grade or eqUivalent Redistilled aCids are acceptable 711 AcetiCaCid,conc(spgr106) ChemIcal Interferences are charactenzed by molecular compound formation, Ionization effects and solute vaponzatlOn effects Normally these effects are not pronounced With the lCP technique, however, If observed they can be minimized by careful selection of operating conditions (that IS, mCldent power, observation pOSitIOn. and so forth). by buffering of the sample, by matnx matching, and by standard additIOn 5 2 4 analyte Ime region-If the appropnate equIpment IS available, wavelength scanning can be performed to detect potential spectral Interferences 5 2 3 method of analySis-When investi- gating a new sample matnx, compan- son tests may be performed With other analytical techniques such as atomic absorption spectrometry, or other approved methodology Apparatus Inductively Coupled Plasma- AtomiC EmiSSion Spectrometer 6 Standard stock solutions may be 6 1 Compaffson With alternate Wavelength scannmg of Computer controlled atomic emiSSion spectrometer With background correction 6 1 1 6 1 2 Radlofrequency generator 6 1 3 Argon gas supply, welding grade or better 6 2 Operating conditIons - of the differences between vanous makes and models of satisfactory Instruments. no detailed operating instructIOns can be prOVided Instead, the analyst should follow the instructions prOVided by the manufacturer of the particular Instrument Sensitivity. Instrumental detection limit, preCISion, linear dy- namIc range, and Interference effects must be investigated and established for each indIVIdual analyte line on that particular Instrument It IS the Metals-22 Dec 1982 Because Hydrochloflc aCid conc (sp gr 7 1 3 500 mL conc HCI (sp gr 1 19) to 400 mL deiOnized, dlstnlled water and dilute to 1 liter 7 14 NItric aCid conc (sp gr 141) 715 NltflCaCId,(1+1)Add500mL conc HN03 (sp gr 1 41) to 400 mL deiOnized, distilled water and dilute to 1 liter 7 2 Dlomzed distilled water Prepare by passing distilled water through a mixed bed of catIon and anion ex- change resins Use deionized, distilled water for the preparation of all reagents, calibration standards and as dilution water The punty of thiS water must be eqUivalent to ASTM Type II reagent water of SpeCification D 1193 (146) 7 1 2 1 19) Hydrochloflc aCId, (1+1) Add 7 3 purchased or prepared from ultra high punty grade chemicals or metals All salts must be dned for 1 h at 105°C unless otherWise speCified (CAUTION Many metal salts are ex- tremely tOXIC and may be fatal ,f swal- lowed Wash hands thoroughly after handling) TYPical stock solution pre- paration procedures follow 7 3 1 Aluminum solutIOn, stock, 1 mL = 100 /1g AI Dissolve a 100 g of aluminum metal In an aCid mixture of 4 mL of (1+1) HCI and 1 mL of conc HN03 In a beaker Warm gently to effect solution When solution IS complete, transfer quantitatively to a liter flask, add an additional 10 mL of (1+ 1) HCI and dilute to 1 000 mL With deiOnized, distilled water 7 3 2 Antimony solutIOn stock, 1 mL = 100 /1g Sb Dissolve a 2669 g K(SbO) C4H40 S In deionized distilled water, add 10 mL (1+1) HCl and dilute to 1000 mL With deionized, distilled waterPDF Image | Methods for Chemical Analysis of Water and Wastes
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