Sulphur tests

API specification Piston deposit test Piston type Fuel sulphur Test... 

Fibres a-napthol hypobromite test for arginine Ninhydrin test for P-alanine Adamciewicz test for tryptophane Vanilla test for tryptophane Morse test for hydroxy-proline Solubility in 18% NaOH (1 hr hot) Sulphur test for cystine... 

ANDREW C.S. 1975. Evaluation of plant and soil sulphur tests in Australia, pp. 196-200. In Sulphur in Australasian Agriculture. 

Sulphur Test (Hay).—Sprinkle some finely powdered sulphur on the surface of 10 ml. of dilute bile in a test tube. The particles gradually penetrate the surface and sink through the liquid owing to the reduction in surface tension due to the bile salts. 

Trichloroethanoic acid, CCI3COOH. A crystalline solid which rapidly absorbs water vapour m.p. 58°C, b.p. 196-5" C. Manufactured by the action of chlorine on ethanoic acid at 160°C in the presence of red phosphorus, sulphur or iodine. It is decomposed into chloroform and carbon dioxide by boiling water. It is a much stronger acid than either the mono- or the dichloro-acids and has been used to extract alkaloids and ascorbic acid from plant and animal tissues. It is a precipitant for proteins and may be used to test for the presence of albumin in urine. The sodium salt is used as a selective weedkiller. 

Molisch s test A general test for carbohydrates. The carbohydrate is dissolved in water, alcoholic 1-naphthol added, and concentrated sulphuric acid poured down the side of the tube. A deep violet ring is formed at the junction of the liquids. A modification, the rapid furfural test , is used to distinguish between glucose and fructose. A mixture of the sugar, 1-naphthol, and concentrated hydrochloric acid is boiled. With fructose and saccharides containing fructose a violet colour is produced immediately the solution boils. With glucose the appearance of the colour is slower. 

Boron trioxide is not particularly soluble in water but it slowly dissolves to form both dioxo(HB02)(meta) and trioxo(H3B03) (ortho) boric acids. It is a dimorphous oxide and exists as either a glassy or a crystalline solid. Boron trioxide is an acidic oxide and combines with metal oxides and hydroxides to form borates, some of which have characteristic colours—a fact utilised in analysis as the "borax bead test , cf alumina p. 150. Boric acid. H3BO3. properly called trioxoboric acid, may be prepared by adding excess hydrochloric or sulphuric acid to a hot saturated solution of borax, sodium heptaoxotetraborate, Na2B407, when the only moderately soluble boric acid separates as white flaky crystals on cooling. Boric acid is a very weak monobasic acid it is, in fact, a Lewis acid since its acidity is due to an initial acceptance of a lone pair of electrons from water rather than direct proton donation as in the case of Lowry-Bronsted acids, i.e. 

By the brown ring test with iron(II) sulphate and cold concentrated sulphuric acid. 

Arsenic present only in traces (in any form) can be detected by reducing it to arsine and then applying tests for the latter. In Marsh s test, dilute sulphuric acid is added dropwise through a thistle funnel to some arsenic-free zinc in a flask hydrogen is evolved and led out of the flask by a horizontal delivery tube. The arsenic-containing compound is then added to the zinc-acid solution, and the delivery tube heated in the middle. If arsenic is present, it is reduced to arsine by the zinc-acid reaction, for example ... 

This reaction is a useful test for a sulphite or for moist sulphur dioxide, which turns dichromate paper (filter paper soaked in potassium dichromate) from yellow to green. 

Oxidation of a sulphur compound with concentrated nitric acid yields sulphuric acid or a sulphate, which can be tested for with barium chloride. This can be used to estimate the sulphur. 

Thus, filler paper which has been dipped into a solution of potassium dichromate turns green in the presence of sulphur dioxide. This reaction provides the usual test for sulphur dioxide. 

The purple colour of this ion alone is a sufficient test for its presence addition of sulphuric acid and hydrogen peroxide discharges ihe colour. 

When concentrated sulphuric acid is added to a nitrate in the presence of aqueous iron(II) sulphate, the nitrogen oxide liberated forms a brown complex [Fe(H20)5N0] which appears as a brown ring at the acid-aqueous interface (test for a nitrate, p 243). 

The residual liquid in the flask is a dilute alkaline solution of sodium acetate. To liberate the acetic acid, add dilute sulphuric acid until the solution is definitely acid to litmus, and then distil off about 20 ml. Perform on this aqueous distillate the tests for acetic acid given on p. 347-... 

Dissolve 5 g. (5 ml.) of aniline in 50 ml. of warm dilute sulphuric acid in a conical flask and add 50 ml. of water. Place a thermometer in the solution, immerse the flask in a mixture of ice and water, and cool until the temperature of the stirred solution falls to 5°. Dissolve 4-5 g. of powdered sodium nitrite in 20 ml. of water, and add this solution in small quantities (about 2-3 ml. at a time) to the cold aniline sulphate solution. Keep tne latter well shaken and maintain the temperature at about 5° (see p. 183). When all the sodium nitrite solution has been added, transfer about 5 ml. of the cold solution to a test-tube for each of the following reactions. The remainder of the diazonium hydrogen sulphate solution must be kept in ice-water until required, and then when all the reactions have been carried out, the solution should be poured down the sink. 

Now grind up the mixture of solution and glass in the mortar to ensure extraction of the sodium salts, and then filter. Divide the filtrate into three portions, reserving two portions for testing for halogens and sulphur. 

To determine which halogen is present, take 1-2 ml. of the filtrate from the sodium fusion, and add dilute sulphuric acid until just acid to litmus. Add about 1 ml. of benzene and then about 1 ml. of chlorine water and shake. A yellowish-brown colour in the benzene indicates bromine, and a violet colour iodine. If neither colour appears, the halogen is chlorine. The result may be confirmed by testing the solubility of the silver halide (free from cyanide) in dilute ammonia solution silver chloride is readily soluble, whereas the bromide dissolves with difficulty, and the iodide not at all. 

Sulphur. THE LASSAIGNE SODIUM TEST. The sodium fusion will have converted any sulphur present in the original compounds to sodium sulphide. Dissolve a few crystals of sodium nitroprusside, Na8[Fe(CN)5NO],zH20, in water, and add the solution to the third portion of the filtrate obtained from the sodium fusion. A brilliant purple coloration (resembling permanganate) indicates sulphur the coloration slowly fades on standing. Note, (i) Sodium nitroprusside is unstable in aqueous solution and therefore the solution should be freshly prepared on each occasion, (ii) This is a very delicate test for sulphides, and it is essential therefore that all apparatus, particularly test-tubes, should be quite clean. 

Zinc dust of good quality usually contains only negligible quantities of halogen and sulphur, and is nitrogen-free. A blank for these elements should, however, be made with every fresh batch of reagent prepared if perceptible traces of halogen or sulphur are present, a blank or control test must be performed side by side with that on the organic compound, and the results compared. 

Sulphuric add test. To 0-5 g. of oxalic acid or of an oxalate, add I ml. of cone. H2SO4 and warm CO and COg are evolved (cf. formic acid). The CO burns with a blue flame. Detect the COg by passing the mixed gases evolved into lime-water. It is essential to test for the COj in a separate reaction, or (if the same test-tube is used) before testing for CO. 

Sulphuric add test. Warm 0 5 g. of tartaric acid or a tartrate with i ml. of cone. H2SO4. Heavy charring takes place, CO and SOj being evolved. 

Sulphuric add test. Heat 0 5 g. of citric acid or a citrate with 1 ml. of H2SO4 CO and COg are evolved and the mixture turns yellow, but does not char. Acetone dicarboxylic acid, OC(CH2COOH)g, is also formed, and is tested for after heating the mixture for 1 minute cool, add a few ml. of water and make alkaline with NaOH solution. Add a few ml. of a freshly prepared solution of sodium nitroprusside and note the intense red coloration (see Test 4 a) for ketones, p. 346). 

Sulphuric acid test. Heat 0-5 g, of oxamide with cone. HjSO. CO and COj are evolved. 

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