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Published by: jljimenez1969 on Jul 02, 2013
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CD-ROM8000B - 1Revision 2December 1996METHOD 8000BDETERMINATIVE CHROMATOGRAPHIC SEPARATIONS1.0SCOPE AND APPLICATION1.1Method 8000 is not a determinative method but instead provides guidance on analyticalchromatography and describes calibration and quality control requirements that are common to allSW-846 chromatographic methods. Apply Method 8000 in conjunction with all SW-846determinative chromatographic methods. The methods include, but are not limited to, the following:MethodChromatographicNumberAnalytesTechnique (see Sec. 1.5)Detecto7580White phosphorus (P)GC, capillary columnNPD
8011EDB, DBCPGC, capillary columnECD8015Nonhalogenated volatilesGC, packed & capillaryFIDcolumn8021VolatilesGC, capillary columnPID, ELCD8031AcrylonitrileGC, packed columnNPD8032AcrylamideGC, packed columnECD8033AcetonitrileGC, capillary columnNPD8041PhenolsUnderivatized orFID, ECDderivatized, GC, capillarycolumn8061PhthalatesGC, capillary columnECD8070NitrosaminesGC, packed columnNPD, ELCD, TED8081Organochlorine pesticides GC, capillary columnECD, ELCD8082Polychlorinated biphenylsGC, capillary columnECD, ELCD8091Nitroaromatics and cyclicGC, capillary columnECDketones8100PAHsGC, packed & capillaryFIDcolumn8111HaloethersGC, capillary columnECD8121Chlorinated hydrocarbonsGC, capillary columnECD
MethodChromatographicNumberAnalytesTechnique (see Sec. 1.5)DetectoCD-ROM8000B - 2Revision 2December 19968131Aniline and selected derivativesGC, capillary columnNPD8141Organophosphorus pesticidesGC, capillary columnFPD, NPD, ELCD8151Acid herbicidesDerivatize; GC, capillaryECDcolumn8260VolatilesGC, capillary columnMS8270SemivolatilesGC, capillary columnMS8275SemivolatilesThermal extraction/GCMS8280Dioxins and DibenzofuransGC, capillary columnLow resolution MS8290Dioxins and DibenzofuransGC, capillary columnHigh resolution MS8310PAHsHPLC, reverse phaseUV, Fluorescence8315Carbonyl compoundsDerivatize; HPLCFluorescence8316Acrylamide, acrylonitrile,HPLC, reverse phaseUVacrolein8318N-Methyl carbamatesDerivatize; HPLCFluorescence8321Extractable nonvolatilesHPLC, reverse phaseTS/MS, UV8325Extractable nonvolatilesHPLC, reverse phasePB/MS, UV8330Nitroaromatics and nitraminesHPLC, reverse phaseUV8331TetrazeneHPLC, ion pair, reverseUVphase8332NitroglycerineHPLC, reverse phaseUV8410SemivolatilesGC, capillary columnFT-IR8430Bis(2-chloroethyl) etherGC, capillary columnFT-IRhydrolysis products
DBCP=DibromochloropropaneMS=Mass spectrometryECD=Electron capture detectorNPD=Nitrogen/phosphorous detectoEDB=Ethylene dibromidePAHs=Polynuclear aromatic hydrocarbonsELCD=Electrolytic conductivity detectorPB/MS=Particle beam mass spectrometryFID=Flame ionization detectorPID=Photoionization detectoFPD=Flame photometric detectorTED=Thermionic emission detectoFT-IR=Fourier transform-infraredTS/MS=Thermospray mass spectrometryGC=Gas chromatographyUV=UltravioletHPLC=High performance liquid chromatography
CD-ROM8000B - 3Revision 2December 19961.2Analytical chromatography is used to separate target analytes from co-extractedinterferences in samples. Chromatographic methods can be divided into two major categories: gaschromatography (GC) and high performance liquid chromatography (HPLC).1.2.1Gas chromatography (more properly called gas-liquid chromatography) is theseparation technique of choice for organic compounds which can be volatilized without beingdecomposed or chemically rearranged.1.2.2High performance liquid chromatography (HPLC) is a separation technique usefulfor semivolatile and nonvolatile chemicals or for analytes that decompose upon heating.Successful liquid chromatographic separation requires that the analyte(s) of interest be solublein the solvent(s) selected for use as the mobile phase. Because the solvents are deliveredunder pressure, the technique was originally designated as high pressure liquidchromatography, but now is commonly referred to as high performance liquid chromatography.1.3All chromatographic processes achieve separation by passing a mobile phase over astationary phase. Constituents in a mixture are separated because they partition differently betweenthe mobile and stationary phases and thus have different retention times. Compounds that interactstrongly with the stationary phase elute slowly (i.e., long retention time), while compounds thatremain in the mobile phase elute quickly (i.e., short retention time).1.3.1The mobile phase for GC is an inert gas, usually helium, and the stationary phaseis generally a silicone oil or similar material.1.3.2In "normal phase" HPLC, the mobile phase is less polar than the stationary phase.In "reverse phase" HPLC, the converse is true. Reverse phase HPLC is the technique of choice for environmental and waste analyses of non-volatile organic target analytes.1.4A number of specific GC and LC techniques are used for environmental and wasteanalyses. The specific techniques are distinguished by the chromatographic hardware or by thechemical mechanisms used to achieve separations.1.4.1GC methods, including those in SW-846, can be categorized on the basis of thechromatographic columns employed. columns are typically made from glass or stainless steel tubingand generally are 1.5 - 3 m long with a 2 - 4 mm ID, and filled with small particles (60-100mesh diatomaceous earth or carbon) coated with a liquid phase. columns are typically made from open tubular glass capillarycolumns that are 15 - 100 m long with a 0.2 - 0.75 mm ID, and coated with a liquidphase. Most capillary columns are now made of fused silica, although glass columns arestill sold for the analysis of volatiles. Capillary columns are inherently more efficient thanpacked columns and have replaced packed columns for most SW-846 applications.1.4.2SW-846 HPLC methods are categorized on the basis of the mechanism of separation. chromatography is the basis of reverse phase HPLCseparations. Analytes are separated on a hydrophobic column using a polar mobilephase pumped at high pressure (800 - 4000 psi) through a stainless steel column 10 -

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