Sodium detection

Fluorescein sodium Minims Fluorescein Sodium Detection of lesions or foreign bodies in the eye... 

SC-CSRS 300 significantly improves the response factors of ammonium and amines when using conductivity detection, because the analytes are actually detected as totally dissociated methanesulfonic acid, which has a higher equivalent conductance (399 S cm /mol). In contrast, sodium detected as Na OH has an equivalence conductance of only 249 S cm /mol and ammonium detected as OH has an equivalence conductance of only 274 S cm /mol. In Figure 4.50, separations of standard inorganic cations, ammonium, and amines using a conventional CSRS 300 are compared with the same separations using a SC-CSRS 300. 

Fehling s solution A solution of copper sulphate, sodium potassium tartrate and NaOH used for estimating and detecting reducing sugars. 

C12H9N3O4. A brownish-red powder, soluble in sodium hydroxide. Used for the detection and estimation of magnesium, with which it forms a blue lake in alkaline solutions. 

Sulfur (detection of H2S and mercaptans) ( Doctor Test ) NF M 07-029 ASTM D 325 Sodium plumbite test (coloration of interface)... 

Detection of Potassium in the presence of Sodium. Add a cold saturated aqueous solution of sodium picrate to a solution of potassium chloride. A rapid precipitation of the less soluble potassium picrate occurs, even from a i°o solution of potassium chloride. 

Place about i g. of the base in a test-tube, and cover with concentrated (about 20%) sodium hydroxide solution. Bring the mixture gently to the boil, keeping the test-tube lightly closed with the finger meanwhile to prevent undue escape of vapour.. A.s the solution boils a strong fishy odour of dimethylamine is detected, and white fumes form when the test-tube is held near an open bottle of concentrated... 

For Middleton s sodium carbonate-zinc method for the detection of elements, see p. 326. 

Lassaigne s test is obviously a test also for carbon in the presence of nitrogen. It can be used therefore to detect nitrogen in carbon-free inorganic compounds, e.g., complex nitrites, amino-sulphonic acid derivatives, etc., but such compounds must before fusion with sodium be mixed with some non-volatile nitrogen-free organic compound such as starch... 

The Sodium Carbonate-Zinc Method for Detecting Nitrogen, Halogens and Sulphur in Organic Compounds. 

Absolute diethyl ether. The chief impurities in commercial ether (sp. gr. 0- 720) are water, ethyl alcohol, and, in samples which have been exposed to the air and light for some time, ethyl peroxide. The presence of peroxides may be detected either by the liberation of iodine (brown colouration or blue colouration with starch solution) when a small sample is shaken with an equal volume of 2 per cent, potassium iodide solution and a few drops of dilute hydrochloric acid, or by carrying out the perchromio acid test of inorganic analysis with potassium dichromate solution acidified with dilute sulphuric acid. The peroxides may be removed by shaking with a concentrated solution of a ferrous salt, say, 6-10 g. of ferrous salt (s 10-20 ml. of the prepared concentrated solution) to 1 litre of ether. The concentrated solution of ferrous salt is prepared either from 60 g. of crystallised ferrous sulphate, 6 ml. of concentrated sulphuric acid and 110 ml. of water or from 100 g. of crystallised ferrous chloride, 42 ml. of concentrated hydiochloric acid and 85 ml. of water. Peroxides may also be removed by shaking with an aqueous solution of sodium sulphite (for the removal with stannous chloride, see Section VI,12). 

CAUTION. Ethers that have been stored for long periods, particularly in partly-filled bottles, frequently contain small quantities of highly explosive peroxides. The presence of peroxides may be detected either by the per-chromic acid test of qualitative inorganic analysis (addition of an acidified solution of potassium dichromate) or by the liberation of iodine from acidified potassium iodide solution (compare Section 11,47,7). The peroxides are nonvolatile and may accumulate in the flask during the distillation of the ether the residue is explosive and may detonate, when distilled, with sufficient violence to shatter the apparatus and cause serious personal injury. If peroxides are found, they must first be removed by treatment with acidified ferrous sulphate solution (Section 11,47,7) or with sodium sulphite solution or with stannous chloride solution (Section VI, 12). The common extraction solvents diethyl ether and di-tso-propyl ether are particularly prone to the formation of peroxides. 

Hydrolysis (or saponification) of n-butyl acetate. Boil 4-5 g. of n-butyl acetate (Section 111,95) with 50 ml. of 10 per cent, sodium hydroxide solution under reflux until the odour of the ester can no longer be detected (about 1 hour). Set the condenser for downward distiUation and coUect the first 10 ml. of distillate. Saturate it with potassium carbonate, aUow to stand for 5 minutes, and withdraw all the Uquid into a small pipette or dropper pipette. AUow the lower layer of carbonate solution to run slowly into a test-tube, and place the upper layer into a small test-tube or weighing bottle. Dry the alcohol with about one quarter of its buUr of anhydrous potassium carbonate. Remove the alcohol with a dropper pipette and divide it into two parts use one portion for the determination of the b.p. by the Siwoloboff method (Section 11,12) and convert the other portion into the 3 5-dinitrobenzoate (Section III, 27) and determine the m.p. 

Place 5-2 g. (5 ml.) of anihne and 45 ml. of 10 per cent, aqueous sodium hydroxide solution in a wide-necked bottle (or, bF not available, a conical flask), and then add 8 -5 g. (7 ml.) of benzoyl chloride, stopper, and shake vigorously for 10-15 minutes. Heat is evolved in the reaction. The crude benzoyl derivative separates as a white powder. When the reaction is complete (t.e., when the odour of benzoyl chloride can no longer be detected smell cautiously), make sure that the reaction mixture is... 

Place 45 g. (43 ml.) of benzal chloride (Section IV,22), 250 ml. of water and 75 g. of precipitated calcium carbonate (1) in a 500 ml. round-bottomed flask fltted with a reflux condenser, and heat the mixture for 4 hours in an oil bath maintained at 130°. It is advantageous to pass a current of carbon dioxide through the apparatus. Filter off the calcium salts, and distil the filtrate in steam (Fig. II, 40, 1) until no more oil passes over (2). Separate the benzaldehyde from the steam distillate by two extractions with small volumes of ether, distil off most of the ether on a water bath, and transfer the residual benzaldehyde to a wide-mouthed bottle or flask. Add excess of a concentrated solution of sodium bisulphite in portions with stirring or shaking stopper the vessel and shake vigorously until the odour of benzaldehyde can no longer be detected. Filter the paste of the benzaldehyde bisulphite compound at the pump... 

In order to detect these elements in organic compounds, it is necessary to convert them into ionlsable inorganie substanees so that the ionic tests of inoiganio qualitative analysis may be applied. This conversion may be accomplished by several methods, but the best procedure is to fuse the organic compound with metallio sodium (Lassalgne s test). In this way sodium cyanide, sodium sulphide and sodium halides are formed, which are readily identified. Thus ... 

Sulphur, as sulphide ion, is detected by precipitation as black lead sulphide with lead acetate solution and acetic acid or with sodium plumbite solution (an alkaLine solution of lead acetate). Halogens are detected as the characteristic silver halides by the addition of silver nitrate solution and dilute nitric acid the interfering influence of sulphide and cyanide ions in the latter tests are discussed under the individual elements. 

THE SODIUM CARBONATE - ZINC METHOD FOR THE DETECTION OF NITROGEN, SULPHUR AND HALOGENS IN ORGANIC COMPOUNDS... 

When an organic compound is heated with a mixture of zinc powder and sodium carbonate, the nitrogen and halogens are converted into sodium cyanide and sodium hahdes respectively, and the sulphur into zinc sulphide (insoluble in water). The sodium cyanide and sodium hahdes are extracted with water and detected as in Lassaigne s method, whilst the zinc sulphide in the residue is decomposed with dilute acid and the hydrogen sulphide is identified with sodium plumbite or lead acetate paper. The test for nitrogen is thus not affected by the presence of sulphur this constitutes an advantage of the method. 

Sulphur. Moisten the centre of a filter paper with sodium plumbite solution. Add about 10 ml. of dilute hydrochloric acid to the residue in the dish and immediately cover it with the prepared filter paper. If zinc sulphide is present in the residue, a dark brown stain, visible on the upper surface of the paper, will be obtained frequently the presence of hydrogen sulphide can also be detected by its odour. 

The distillate may contain volatile neutral compounds as well as volatile acids and phenols. Add a slight excess of 10-20 per cent, sodium hydroxide solution to this distillate and distil until the liquid passes over clear or has the density of pure water. The presence of a volatile, water-soluble neutral compound is detected by a periodic determination of the density (see Section XI,2) if the density is definitely less than unity, the presence of a neutral compound may be assumed. Keep this solution Si) for Step 4. 

Sodium nitroprusside (for sulfur detection) dissolve about 1 g of sodium nitroprusside in 10 mL of water as the solution deteriorates on standing, only freshly prepared solutions should be used. This compound is also called sodium nitroferricyanide and has the formula Na2pe(NO)(CN)5 2H2O. 

Description of Method. The water-soluble vitamins Bi (thiamine hydrochloride), B2 (riboflavin), B3 (niacinamide), and Be (pyridoxine hydrochloride) may be determined by CZE using a pH 9 sodium tetraborate/sodlum dIhydrogen phosphate buffer or by MEKC using the same buffer with the addition of sodium dodecyl-sulfate. Detection Is by UV absorption at 200 nm. An Internal standard of o-ethoxybenzamide Is used to standardize the method. 

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