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• W212071011 abstract "Tetrachlorophthalic acid has been used as a precipitant for the determinations of thorium and zirconium. These two metals precipitate at rather high acidities. Recently, the solubility products of thorium, lanthanum, praseodymium, and neodymium tetrachlorophthalates have been reportedt. It is interesting to note that Crookes already prepared scandium tetrachlorophthalate in 1910. These facts lead us to study the said acid as a reagent for scandium and its separation from thorium.It is found that scandium precipitates quantitatively with tetrachlorophthalic acid in the pH range of 2.4—4.4 (cf. Table 1), whilst thorium in pH 1.0—1.1. Hence, there exists the possibility of separating these two elements simply by adjusting the acidity of the solution, which has been substantiated experimentally in this communication.For the quantitative precipitation of scandium, 2.5—3 moles of the reagent are needed for each gram-atom of scandium, and a large excess of the precipitant (up to 7.8 moles precipitant per gram-atom of scandium have been tested) does no harm (cf. Table 2*).The method is suitable for 1—102 mg of scandium oxide or 0.6—67 mg of scandium(cf. Table 3*).Scandium and thorium tetrachlorophthalates have been prepared under analytical conditions, and subjected to thermolysis. Under 200℃, the salts are heated in a drying oven, and over 200℃, in an electric muffle furnace. The drying oven is hcatcd up with a rate of 2℃ per minute, and the muffle with a rate of 5℃ per minute. After reaching the desired temperature, the crucible is taken out, cooled and weighed. The crucible is partially covered during heating. The results are plotted in Figure 1~* (Curve A stands for scandium tetrachlorophthalate and B, for thorium tetrachlorophthalate). These curves are similar in shape, each with two plateaus, which denote respectively the formation of basic tetrachlorophthalates and oxides. For the scandium tetrachlorophthalate, the plateaus are found at the temperature intervals (a) 80—150℃ and (b) 670—960℃, and for thorium tetrachlorophthalate, (a) 80—150℃ and (b) 720—960℃. The composition of scandium basic tetrachlorophthalate has been found experimentally to be C_6Cl_4(COO)_2Sc (OH) H_2O.From the constancy ha weight of both scandium and thorium tetrachlorophthalatcs inthe temperature interval 80—150℃, it may be concluded that both precipitates can be dried and weighed as such, instead of ignition to the corresponding oxides.The effects of some alkalis and ammonium salts upon the scandium precipitation have been tested experimentally. The results are listed in Table 4~*. Large amounts (up to 4 gms) of ammonium nitrate, chloride, and acetate exert no influence. Large amounts of sulphate ions, owing to their complexing with scandium (Ⅲ), interfere as in the cases of m-nitrobenzoic and quinaldinic acids. Though acetate ions complexes with scandium (Ⅲ) too, yet the precipitation of scandium tetrachlorophthalatc takes place in rather acid medium, which lowers the concentration of acetate ions. Sodium and potassium ions cause slightly positive errors, owing very probably to the co-precipitation of the nonvolatile alkalis.Within pH 2.5—3.4, the amount of light lanthanides prccipitated with tctraphthalic acid is small (about 0.3—2 mg of oxides). Erbium (Ⅲ) and yttrium (Ⅲ) precipitate quantitatively at pH 8.1—9.5 and pH 10 respectively. Ceric ions precipitate, though not quantitatively, at pH 0.5, and its interference in scandium and thorium determinations may be avoided by reducing them to the cerous state with a reductant, such as hydroxylamine. The separation of scandium from light lanthanides (up to Sc:Ln=1:96,) and yttrium (up to Sc:Y=1:10.4) by double precipitation with tetrachlorophthalic acid is successful (cf. Table 5~*).Based upon the findings reported above, a procedure has been devised for the separation of thorium and scandium and their determinations. The results of some synthetic mixtures analysed with the procthcthcedure are listed in Table 6~*. The weight ratios of scandium oxide to thorium oxide varied from 1:2.5 to 1:9.8 have been tested and the absolute errors lie within +0.1 to +0.3 mg of scandium oxide and 0.0 to +0.7 mg of thorium oxide. The essential steps of the procedure are as follows. Precipitate thorium twice as tetrachlorophthalate at pH 1.0—1.1 and treat the precipitate according to Gordon et al. The filtrates and washings are brought to pH 3.0 and treated with the precipitant again. Digest for two hours on a water bath with occasional stirring. Cool, filter with a retentive paper. Wash and treat the scandium precipitate further as the thorium precipitate." @default.
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• W212071011 date "1962-12-01" @default.
• W212071011 modified "2023-09-25" @default.
• W212071011 title "ON THE SEPARATION AND DETERMINATION OF SCANDIUM AND THORIUM; 3. WITH TETRACHLOROPHTHALIC ACID AS REAGENT" @default.
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