Kjeldahl

Kjeldahl method An analytical method for the determination of nitrogen particularly in organic materials. The N is converted to NH with cone. H2SO4 and catalysts. After neutralization the NH j is distilled ofT and estimated by titration after absorption. 

Ammonia may be estimated by dissolving the gas in a known volume of standard acid and then back-titrating the excess acid. In a method widely used for the determination of basic nitrogen in organic substances (the Kjeldahl method), the nitrogenous material is converted into ammonium sulphate by heating with concentrated sulphuric acid. The ammonia is then driven off by the action of alkali and absorbed in standard acid. 

A very suitable apparatus for semi-micro steam-distillation, particularly for suspensions that are likely to bump badly, is showm in Fig. 44. This consists of a 50 ml. Kjeldahl flask, clamped at an angle of 45°, and fitted with a long glass tube for the inlet of steam. The Outlet-tube is bent twice, first at 135° and then at 45° as shown, and fitted into a small water-condenser. 

The two chief methods for estimating nitrogen in organic compounds are (i) the Dumas method, which can be applied to all organic compounds (ii) the Kjeldahl method, which is of more restricted application, but which is frequently used in biochemical and physiological work. Its limitations are indicated in the description of the method (p. 492). 

Two convenient forms of bath are shown ui Fig. 11,10, 2, a and 6. The former consists of a long-necked, round-bottomed flask (a longnecked Kjeldahl flask of 100 ml. capacity is quite satisfactory) supported by means of a clamp near the upper part of the neck. The thermometer is fltted through a cork, a section of the cork being cut away (see inset) so that the thermometer scale is visible and also to allow free expansion of the air in the apparatus. The bulb is about three-quarters filled with... 

Kjeldahl analysis an acid-base titrimetric method for determining the amount of nitrogen in organic compounds, (p. 302)... 

Oxygen and nitrogen also are deterrnined by conductivity or chromatographic techniques following a hot vacuum extraction or inert-gas fusion of hafnium with a noble metal (25,26). Nitrogen also may be deterrnined by the Kjeldahl technique (19). Phosphoms is determined by phosphine evolution and flame-emission detection. Chloride is determined indirecdy by atomic absorption or x-ray spectroscopy, or at higher levels by a selective-ion electrode. Fluoride can be determined similarly (27,28). Uranium and U-235 have been determined by inductively coupled plasma mass spectroscopy (29). 

Protein Content. The protein content of milk can be determined using a variety of methods including gasometric, Kjeldahl, titration, colorimetric, and optical procedures (see Proteins). Because most of the techniques are too cumbersome for routine use in a dairy plant, payment for milk has seldom been made on the basis of its protein content. Dye-binding tests have been appHed to milk for determination of its protein content these are relatively simple to perform and can be carried out in dairy plant laboratories. More emphasis will be given to assessing the nutritional value of milk, and the dependence on fat content as a basis for payment will most likely change. 

Devarda s Method. Nitrogen in nitrates or nitric acid also may be deterrnined by the Kjeldahl method or by Devarda s method. The latter is both convenient and accurate when no organic nitrogen is present. The nitrate is reduced by Devarda s alloy to ammonia in an alkaline solution. The ammonia is distilled and titrated with standard acid. 

Commercially produced barium is analyzed for metallic impurities by means of emission spectroscopy. Carbon content can be deterrnined by combustion, and nitrogen by the Kjeldahl method. Total barium can best be deterrnined gravimetricaHy by precipitation as the sulfate. 

Oxidative degradation of [B qH q] and [B22H22] C to boric acid is extremely difficult and requires Kjeldahl digestion or neutral permanganate. The heat of reaction obtained from the permanganate degradation leads to a calculated heat of formation for [B qH q] (aq) of 92.5 21.1 kJ/mol (22.1 5.0 kcal/mol) (99). The oxidative coupling of both [B qH q] and has been studied ia some detail (100). 

Commercially produced calcium metal is analyzed for metallic impurities by emission spectroscopy. Carbon content is determined by combustion, whereas nitrogen is measured by Kjeldahl determination. 

SCWO Supercritical Water Oxidation TKN Total Kjeldahl Nitrogen TOC Total Organic Carbon TSS Total Suspended Solids WAO Wet Air Oxidation... 

For the estimation of ephedrine in its salts or simple solutions, titration methods and a Kjeldahl estimation have been described by various authors. The formation of iodoform from ephedrine has been proposed as a method of estimation by Sanchez, and biological methods have been used by several authors. ... 

Reactions under pressure are usually carried out in an autoclave. However, several simple vessels can be used for reactions at moderate pressure. A heavy walled Pyrex test tube or Kjeldahl flask drawn out and sealed with an oxygen torch makes a suitable container for many Diels-Alder reactions. The tube can be heated in an oil or water bath, but care must be exercised to protect against explosions. At the conclusion of the reaction, the tube is cooled to room temperature, the neck is scratched with a file or carborundum chip, and a hot Pyrex rod is touched to the scratch. A large crack in the neck should result, and the sealed top can be easily knocked off. 

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