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Kjeldahl method : ウィキペディア英語版
Kjeldahl method
The Kjeldahl method or Kjeldahl digestion ((:ˈkʰɛld̥æːˀl)) in analytical chemistry is a method for the quantitative determination of nitrogen in chemical substances developed by Johan Kjeldahl in 1883.〔Kjeldahl, J. (1883) ("Neue Methode zur Bestimmung des Stickstoffs in organischen Körpern" ) (New method for the determination of nitrogen in organic substances), ''Zeitschrift für analytische Chemie'', 22 (1) : 366-383.〕〔Julius B. Cohen ''Practical Organic Chemistry'' 1910 (Link to online text )〕
== Method ==
The method consists of heating a substance with sulphuric acid, which decomposes the organic substance by oxidation to liberate the reduced nitrogen as ammonium sulphate. In this step potassium sulphate is added to increase the boiling point of the medium (from 337 °C to 373 °C) . Chemical decomposition of the sample is complete when the initially very dark-coloured medium has become clear and colourless.
The solution is then distilled with a small quantity of sodium hydroxide, which converts the ammonium salt to ammonia. The amount of ammonia present, and thus the amount of nitrogen present in the sample, is determined by back titration. The end of the condenser is dipped into a solution of boric acid. The ammonia reacts with the acid and the remainder of the acid is then titrated with a sodium carbonate solution by way of a methyl orange pH indicator.
: Degradation: Sample + H2SO4 → (NH4)2SO4(aq) + CO2(g) + SO2(g) + H2O(g)
: Liberation of ammonia: (NH4)2SO4(aq) + 2NaOH → Na2SO4(aq) + 2H2O(l) + 2NH3(g)
: Capture of ammonia: B(OH)3 + H2O + NH3 → NH4+ + B(OH)4
: Back-titration: B(OH)3 + H2O + Na2CO3 → NaHCO3(aq) + NaB(OH)4(aq) + CO2(g) + H2O
In practice, this analysis is largely automated; specific catalysts accelerate the decomposition. Originally, the catalyst of choice was mercuric oxide. However, while it was very effective, health concerns resulted in it being replaced by cupric sulfate. Cupric sulfate was not as efficient as mercuric oxide, and yielded lower protein results. It was soon supplemented with titanium dioxide, which is currently the approved catalyst in all of the methods of analysis for protein in the Official Methods and Recommended Practices of AOAC International.〔AOAC International〕

抄文引用元・出典: フリー百科事典『 ウィキペディア(Wikipedia)
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