Carbon tetrachloride extraction nitrate

The reaction can be followed by adding an aliquot to eth-anolic silver nitrate solution (Note 9). The reaction is complete when no precipitate of the silver derivative is obtained. Also the disappearance of the infrared absorption band at 3300 cm. (3.03 fx) (ethynyl z)CH) can be followed with carbon tetrachloride extracts of aliquots. 

Chloride Carbon -tetrachloride Chloride reacted with phenyl mercuric nitrate to produce phenyl mercury chloride, then carbon tetrachloride extraction, then GLC 0.4mg L- [799]... 

Table II. O.IM Trilaurylmethylammonium Nitrate—Carbon Tetrachloride Extraction of Cerium and Berkelium from Nitric Acid Solutions in the Presence of Sodium Bismuthate...

Buchberger et al. [104] carried out a selective determination of iodide in brine. The performance of a potentiometric method using an ion-selective electrode and of liquid chromatography coupled with ultraviolet detection at 230 nm were compared as methods for the determination of iodide in the presence of other iodide species. Satisfactory results were obtained from the potentiometric method provided the solution was first diluted tenfold with 5 M sodium nitrate, and external standards were used. Better reproducibility was, however, achieved with HPLC, provided precautions were taken to prevent reduction of iodine to iodide in the mobile phase, for which extraction of iodine with carbon tetrachloride prior to analysis was recommended. This was the pre-... 

In a similar procedure [32] the sediment is wet oxidised with dilute sulphuric acid and nitric acids in an apparatus in which the vapour from the digestion is condensed into a reservoir from which it can be collected or returned to the digestion flask as required. The combined oxidised residue and condensate are diluted until the acid concentration is IN and nitrate is removed by addition of hydroxylammonium chloride with boiling. Fat is removed from the cooled solution with carbon tetrachlodithizone in carbon tetrachloride. The extract is shaken with 0.1M hydrochloric acid and sodium nitrite solution and, after treatment of the separated aqueous layer with hydroxylammonium chloride a solution of urea and then EDTA solution are added to prevent subsequent extraction of copper. The liquid is then extracted with a 0.01% solution of dithizone in carbon tetrachloride and mercury estimated in the extract spectrophotometrically at 485nm. 

Extraction of the elemental form of bromine is used to separate short-lived bromine activities from fission products. Potassium chlorate in 8 N nitric acid solution (255)s potassium permanganate in nitric acid solution (106,248), and a bromlde-bromate-hypofchlorite mixture in acidic solution (247) have been used as the oxidizing agent. The bromine is extracted into carbon tetrachloride and can be back-extracted into the aqueous solution by reducing agents, such as potassium nitrate (255)> hydrazine hydrochloride (106,248), or sodium hydrosulphite (106). 

Test for iodide in the neutralized soda extract or in a solution of the sodium salts by the addition of a few drops of chlorine water (or acidified sodium hypochlorite solution) and 2-3 ml chloroform or carbon tetrachloride the latter is coloured violet. Add excess silver sulphate solution to another portion of the neutral solution and filter off the silver iodide remove the excess silver sulphate with sodium carbonate solution. Pass sulphur dioxide into the filtrate to reduce iodate to iodide, boil off the excess sulphur dioxide, and add silver nitrate solution and dilute nitric acid. A yellow precipitate of silver iodide confirms the presence of iodate in the original substance. 

Wash the precipitate (A) with 2m ammonia solution, and remove half of it to a small beaker with the aid of a clean spatula. Treat the residue on the filter with a little silver nitrate solution containing a few drops of dilute acetic acid a brownish-red residue (due to Ag3As04) indicates arsenate present. If the residue is yellow (largely Ag3P04), pour 6m hydrochloric acid through the filter a number of times, and add a little potassium iodide solution and 1-2 ml chloroform or carbon tetrachloride to the extract and shake if the organic layer acquires a purple colour, an arsenate is present. 

The presence of iodate in the soda extract can be readily detected as follows. Treat 2 ml of the solution with silver nitrate solution until precipitation ceases, heat to boiling for 2-3 minutes and filter. Render the filtrate strongly acid with hydrochloric acid, add 2 ml of 0-5m iron(II) sulphate solution (or 0 5m sodium sulphite solution) and shake it with 2 ml carbon tetrachloride. A purple colouration of the organic layer indicates iodate. 

Acidify 3 ml of the soda extract with concentrated perchloric acid and add 1 ml in excess (note 2 below) add silver nitrate solution, slowly and with stirring, until precipitation is complete. Filter and collect the filtrate in a ground-glass stoppered conical flask or test-tube. Add m sodium chloride solution, 05 ml at a time, to the filtrate until no more precipitate forms. Stopper the flask or test-tube and shake the mixture vigorously after each addition. Filter off the silver chloride (note 3 below), transfer the filtrate to the stoppered vessel, add an equal volume of concentrated hydrochloric acid (if a precipitate of sodium chloride forms, filter), cool, then add 1-2 g solid iron(II) ammonium sulphate and 2 ml carbon tetrachloride. Shake the mixture intermittently for 5 minutes. A purple colour in the carbon tetrachloride indicates periodate present. 

Nitric Acid. By the action of concentrated nitric acid on /3/3 dichlorovinyl chloroarsine a crystalline product is obtained which melts at 97° to 99° C. this is the nitrate of )8)8 dichlorovinyl arsenic acid (ClCH=CH)2As00H.HN03. This compound apparently does not ionise in solution, but when dissolved in aqueous alcohol and treated with sodium hydroxide solution until the nitric acid is neutralised, decomposition takes place. On extracting with chloroform and evaporating the extract, a crystalline mass remains which consists of dichlorovinyl arsenic acid (Mann and Pope), (CHCl=CH)2AsOOH. This is purified by recrystallisation from water or carbon tetrachloride, when it melts at 120° to 122° C. Like cacodylic acid, it is amphoteric, forming salts with acids as well as with bases. 

A gas chromatographic procedure is cited in the BP for the assay econazole nitrate in a cream base". Econazole nitrate is extracted into methanol - 0.6m sulphuric acid, whilst other lipid soluble excipients are extracted into carbon tetrachloride. The aqueous extracts are made alkaline with 2 M ammonia and extracted into Chloroform. An internal standard, 1,2,3,4-tetraphenylcyclopenta-l,3-diene is added to the chloroform extracts and then evaporated to a low volume. Extracts were chromatographed on a 1.5 m x 2.0 mm OV-17 (or equivalent column) at 270°C using nitrogen as carrier gas and flame ionization detection. 

A solution of triphenylbismuthine (22 g) in dry carbon tetrachloride (50 ml) was cooled to - 15°C and treated with a similarly cooled solution of henzoyl nitrate prepared in situ from benzoyl chloride (37 g) and silver nitrate (50 g). The mixture was well shaken, left to stand for 16 h and filtered. The residue was extracted with chloroform repeatedly and the combined filtrate and extracts were diluted with light petroleum to precipitate the dinitrate as a solid (27.5 g). This, on further extraction with cold ether, left insoluble triphenylbismuth dinitrate (12.5 g) [24JCS( 125)854],... 

From other experiments in which the effects of mass transfer have been analyzed, it appears that the following systems are mass transfer limited uranyl nitrate extraction by TBP, copper extraction by sodium-loaded DEHPA.19 and extraction of zinc and copperfll) chlorides by TIOA.20 Zinc extraction by dithizone in carbon tetrachloride is mass transfer limited at high zinc concentrations but kineticaily controlled at low zinc levels.21 Ferric ion extractions are repoted to be slow because of its sluggish llgand-excbenge kinetics.22 Extraction of ferric chloride by TIOA, for example, is controlled by a slow heterogeneous reaction.21... 

Separation of Am(III), Cf(III), and Cm(III) in various ELM systems was investigated by Novikov et al (54-56). Optimized conditions for recovery of these permeates involved an outer aqueous solution of diethylenetriaminepentaacetic acid (DTPA), citric acid, sodium nitrate, and nitric acid at pH 3.0, a membrane phase of DEHPA and SPAN 80 in carbon tetrachloride, and an inner aqueous solution of K10P2W17O8J, sodium azide, and hydrazoic acid at pH 3.0. When citric acid was added to the outer solution to enhance the extraction rate of the membrane and the actinide recovery, selectivity declined. A... 

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