人人文库网 > 行业资料 > 各类标准 > AOAC Official 968.04 Heptachlor in Pesticide ulations Gas Chromatographic First Action 1968 Final Action 1969_AOAC.rar
AOAC Official 968.04 Heptachlor in Pesticide ulations Gas Chromatographic First Action 1968 Final Action 1969_AOAC.rar
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AOAC Official 968.04 Heptachlor in Pesticide ulations Gas Chromatographic Fi
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AOAC Official 968.04 Heptachlor in Pesticide ulations Gas Chromatographic First Action 1968 Final Action 1969_AOAC.rar,AOAC Official 968.04 Heptachlor in Pesticide ulations Gas Chromatographic Fi
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7.6.42AOAC Official Method 968.04Heptachlorin Pesticide FormulationsGas Chromatographic MethodFirst Action 1968Final Action 1969A. Apparatus(a) Gas chromatograph.With Hflameionization detector;capa-bleofacceptingglasscolumnandglass-linedsampleintroductionsys-tem or on-column injection. Use following conditions: Temperatures(C): column 175, detector 175190, sample inlet 190; N2carrier gaspressure 30 psig; recorder chart speed 2.5 cm/min.(b) Glass-stoppered tubes.Approximately 25 and 75 mLcapacity.(c) Microliter syringe.10 L.B. Reagents(a) Heptachlor.Reference grade (Velsicol Chemical Corp.,5600 N. River Rd, Rosemont, IL 60018-5119, USA).(b) Aldrin.Referencegrade(Sandoz,Inc.,480CaminodelRioSoth, Suite 204, San Diego, CA 92108, USA).C. Preparation of ColumnTo 9.5 g 100120 mesh Gas Chrom Q in vacuum flaskadd0.50gsilicone GE Versilube F-50 (available from Alltech-Applied Sci-ence Laboratories, Inc.) dissolved in 50 mL CH2Cl2. Shake slurrywell to wet solid thoroughly. Connect flask to H2O aspirator andevaporate solvent with frequent shaking. When solids appear dry,complete drying by placing flask in steam bath and connecting tovacuumpumpuntilca4mmpressureisattained.Removeflaskfromsteam bath and let cool under vacuum.Fill 1.5 m 2 mm od (1.7 mm id) Pyrex glass tube with this pack-ing, using vacuum pump and gentle tapping. Plug ends of columnwith glass wool. Condition column 24 h in 190C oven while purg-ingwithN2.LetcolumncoolwhilestillpurgingwithN2;theninstallin chromatograph.D. Preparation of Test Solution(a) Liquids.Weigh test portion containing ca 750 mgheptachlor into 75 mL glass-stoppered vial and add 500 mg refer-ence grade aldrin. Add 75 mL fresh CS2, stopper, and shake vigor-ously 2 min.(b) Solids.Transferweighedtestportioncontainingca750mgheptachlor to Soxhlet and extract 2 h with 75 mL pentane. Let cool,add 500 mg reference grade aldrin to solution, and swirl.E. CalibrationWeigh 0.2500 g reference grade heptachlor and 0.1670 g refer-ence grade aldrin into 25 mL glass-stoppered flask. Dissolve in25 mL CS2. Chromatograph this solution under conditions givenin A(a) 5 times to obtain accurate response correction factor. (Onnew column, it is sometimes desirable to inject several 5 Laliquots of standard solution to condition column before use.)F. DeterminationLetinstrumentequilibrateasinA(a).Injectca1Ltestsolutionatsensitivitysettingsuchthatheightofheptachlorpeakisca34fullscale.For each analysis, allow 1012 min for heptachlor related compo-nents to elute. Components and approximate retention times in minare: heptachlor 4.5, aldrin 5.9, chlordene 3.1, and -chlordane 9.9.G. CalculationsCalculateareaofheptachlorandaldrinpeaksbymultiplyingpeakheight in mm by width of peak at half height in mm. Alternatively,use integrator. Calculate response correction factor (f, ca 0.82) foreach of the 5 standard injections as follows:f =Area of heptachlor peakmg aldrin purity of aldrinArea of aldrin peakmg heptachlorpurity of heptachlorAverage 5 replicates and use average to calculate percentheptachlor in test portions.Heptachlor, % =Area of h
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