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卡尔费什试剂(Karl Fish reagent)
卡尔费什试剂(Karl Fish reagent)
Karl Fehu principle and technology of water content measurement
The Carle Fischer method, abbreviated as the Hugh Hugh method, was proposed in 1935 by Carle Fischer (KarlFj Scher) to measure the capacity of water. The Fischer method is the most specific and accurate method for the determination of water in substances. Is the classic method but after years of improvement, to improve the accuracy and expand the measurement range, has been listed as many substances in the standard method for determination of moisture.
Fischer French iodometric method, its basic principle is to use iodine sulfur dioxide, need quantitative water in reaction:
120 S02 ten 2H2O=2HI ten H2SO4 (1)
The above reaction is reversible. In order for the reaction to move in a positive direction and to proceed quantitatively, the alkaline substance must be added. It has been proved that pyridine is the most suitable reagent, and pyridine can also combine with iodine and sulfur dioxide to reduce the vapor pressure of the two. Therefore, reagents must be added to methanol or another solvent containing a reactive OH group to convert sulfur anhydride pyridine into stable methyl hydrogen sulfate pyridine.
The theoretical molar ratio of reagent is iodine: sulfur dioxide: pyridine, methanol = 1:1:3:1.
Preparation and calibration of measuring reagent
Usually, when the reagent is prepared, only the iodine should be strictly in accordance with the chemical measurement. The other group is excessive. The molar ratio is usually iodine: sulfur dioxide: pyridine: methanol = 1:3:10:50. Preparation fees, reagents used by each substance must strictly control its water content, generally not more than 0.1%, if the microanalysis should not be more than a few ppm.
The preparation steps take anhydrous pyridine 133mL and iodine 42.33g, and then pour into a bottle with brown reagents, shake to the iodine, and then dissolve into the anhydrous methanol 333ml. It is difficult to accurately weigh the w
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