代森锰锌分析方法CIPAC.docVIP

1 Identification Test- Drop colorimetric test 1.1 Reagent and apparatus Dithizone: mass fraction≥99.0% Dithizone neutral solution:1g/kg Dithizone chloroform solution Acid Dithizone solution:2mL Dithizone neutral solution+0.25mL glacial acetic acid, diluted with chloroform to 10ml. NaOH solution:40g/L; Filter paper:whatman No.1; Dropper: Melting point determination capillary. 1.2 Determination 1.2.1 “Spot” production Experiment 1 “Spot”: Weight 0.5g sample, add distilled water 2~3mL, Stir to full dispersion. Prepared sample droped to the filter paper with the dropper, the codes are respectively as 1-1,1-2. “Spot” requirement: Center point powder about 5mm diameter, outside the point of circular ring diameter about 20mm. open-air drying. Experiment 2 “Spot” Weight 0.5g sample, add chloroform 2~3mL, Stir to full dispersion. Prepared sample droped to the filter paper with the dropper, the codes are respectively as 2-1,2-2. “Spot” requirement: Center point powder about 5mm diameter, outside the point of circular ring diameter about 20mm. open-air drying. 1.2.2 Identification Experiment 1:Use Dropper absorbed Acid Dithizone solution, then drop to the spot 1-1, the central powder spot should be yellow, outer ring should be pink(repeat one more time, drop to 1-2). Experiment 2: Use Dropper absorbed Dithizone neutral solution, then drop to the spot 2-1, the central powder spot should be yellow at the begning, then rapidly turn into strong brilliant violet (repeat one more time, drop to 2-2). If the test results meet the test 1 and test 2 at the same time, that the sample believe to be Mancozeb. 2 Determination of the mass fraction of mancozeb 2.1 Outline of Methods Sample decomposed with the boiling HI-glacial acetic acid solution, generated Ethylenediamine salt, carbon disulfide and hydrogen sulfide gas which can be interfere the analysis. First , H2S was absorbed with CH3COOPb solution, then carbon disulfide was absorbed with KOH-CH3OH solution and generated Potassium met