Dryness determination

Add 1 ml. of the alcohol-free ether to 0-1-0-15 g. of finely-powdered anhydrous zinc chloride and 0 5 g. of pure 3 5-dinitrobenzoyl chloride (Section 111,27,1) contained in a test-tube attach a small water condenser and reflux gently for 1 hour. Treat the reaction product with 10 ml. of 1-5N sodium carbonate solution, heat and stir the mixture for 1 minute upon a boiling water bath, allow to cool, and filter at the pump. Wash the precipitate with 5 ml. of 1 5N sodium carbonate solution and twice with 6 ml. of ether. Dry on a porous tile or upon a pad of filter paper. Transfer the crude ester to a test-tube and boil it with 10 ml. of chloroform or carbon tetrachloride filter the hot solution, if necessary. If the ester does not separate on cooling, evaporate to dryness on a water bath, and recrystallise the residue from 2-3 ml. of either of the above solvents. Determine the melting point of the resulting 3 5 dinitro benzoate (Section 111,27). 

Oxidation of galactose (or a galactose-containing sugar) to mucic acid. Dissolve 1 g. of galactose or lactose in a mixture of 10 ml. of water and 5 ml. of concentrated nitric acid contained in a small evaporating dish, and evaporate the solution to dryness on a water bath. Stir the cold residue with 10 ml. of cold water, filter off the mucic acid, wash it with cold water, dry and determine the m.p. (212-213° with decomposition). 

The general manufacturing scheme for phosphate salts is shown in Figure 11. Condensed phosphates are prepared from the appropriate orthophosphate or mixture of orthophosphates, so the preparation of orthophosphates must be considered first for the manufacture of any phosphate salt. Phosphoric acid is neutralized to form a solution or slurry with a carefully adjusted acid/base ratio according to the desired orthophosphate product. The orthophosphate may be recovered either by crystallization from solution, or the entire solution or slurry may be evaporated to dryness. The dewatering (qv) method is determined by the solubihty properties of the product and by its desired physical properties such as crystal size and shape, bulk density, and surface area. Acid orthophosphate salts may be converted to condensed phosphates by thermal dehydration (calcination). 

In this determination about 2 grams are saponified in the usual manner, and the saponification residue rendered slightly alkaline, and evaporated to dryness on a water-bath. The residue is dissolved in 5 c.c. of water and acidified with 2 c.c. of dilute sulphuric acid. This liquid is now distilled by passing a current of steam through it, and when no... 

The pH of the reaction mixture is taken both before and after the addition of the last portion of the quinidine-methanol solution. The mixture is gently warmed (30° to 50°C), and the pH determined at 20 minute intervals. At the end of 4 hours, or when the reaction has gone to completion as evidenced by the pH of the mixture (between pH 6.5 and 7.5), the stirring is then stopped and the mixture cooled to 0°C and filtered. The solvent is evaporated to dryness under reduced pressure, utilizing as little heat as is feasible. The dried residue Is powdered and suspended in 10 volumes of methanol and filtered. The insoluble powder is dried, and is quinidine polygalacturonate, melting at 180°C with decomposition. 

Theory. Conventional anion and cation exchange resins appear to be of limited use for concentrating trace metals from saline solutions such as sea water. The introduction of chelating resins, particularly those based on iminodiacetic acid, makes it possible to concentrate trace metals from brine solutions and separate them from the major components of the solution. Thus the elements cadmium, copper, cobalt, nickel and zinc are selectively retained by the resin Chelex-100 and can be recovered subsequently for determination by atomic absorption spectrophotometry.45 To enhance the sensitivity of the AAS procedure the eluate is evaporated to dryness and the residue dissolved in 90 per cent aqueous acetone. The use of the chelating resin offers the advantage over concentration by solvent extraction that, in principle, there is no limit to the volume of sample which can be used. 

Procedure. Allow the whole of the sample solution (1 L) to flow through the resin column at a rate not exceeding 5 mL min . Wash the column with 250 mL of de-ionised water and reject the washings. Elute the copper(II) ions with 30 mL of 2M nitric acid, place the eluate in a small conical flask (lOOmL, preferably silica) and evaporate carefully to dryness on a hotplate (use a low temperature setting). Dissolve the residue in 1 mL of 0.1 M nitric acid introduced by pipette and then add 9 mL of acetone. Determine copper in the resulting solution using an atomic absorption spectrophotometer which has been calibrated using the standard copper(II) solutions. 

Procedure. Dissolve a weighed portion of the substance in which the amount of iron is to be determined in a suitable acid, and evaporate nearly to dryness to expel excess of acid. Dilute slightly with water, oxidise the iron to the iron(III) state with dilute potassium permanganate solution or with a little bromine water, and make up the liquid to 500 mL or other suitable volume. Take 40 mL of this solution and place in a 50 mL graduated flask, add 5 mL of the thiocyanate solution and 3 mL of AM nitric acid. Add de-ionised water to dilute to the mark. Prepare a blank using the same quantities of reagents. Measure the absorbance of the sample solution in a spectrophotometer at 480 nm (blue-green filter). Determine the concentration of this solution by comparison with values on a reference curve obtained in the same way from different concentrations of the standard iron solution. 

In addition to meeting the foregoing requirements, a good internal standard will be easy to add uniformly and precisely, and (preferably) no appreciable amount of the element St (free or combined) will be present in the sample before the addition. Cope29 provides an excellent illustration of these points. He found that yttrium nitrate dissolved in ethyl alcohol could be added to a powdered uranium mineral in a mortar, whereupon grinding immediately to dryness dispersed the internal standard (yttrium) so uniformly that uranium could be satisfactorily determined in certain minerals. But the mineral euxenite is an exception, for it contains both yttrium and uranium, and this complicates the uranium determination with yttrium as internal standard. 

Soxhlet extraction followed by liquid chromatography/photodiode-array detection (LC/PAD) is used for the trace determination of propanil and its major metabolite, 3,4-dichloroaniline, in soil. A 10-g soil sample is extracted with methanol in a Soxhlet system for 8 h. After the extracts have been concentrated to dryness, the residue is dissolved in 500 pL of n-hexane. °... 

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