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United States Patent Office Eatented (Oct 3,002,811 United States Patent Office Eatented (Oct. 3, 1961 certarrests An 3,092.82. the saturation point is reached. At this point addi ETS; GF SURFBNé ALKAL tional hydriodic acid is added, the quantity of which AETAS, SOSES may vary from 5% to 25% of the volume of the satu Erwin. E. Johnson, Parta, Chie, assignor to The Harshaw rated alkali metal iodide solution according to the purity gical (Cengary, Ceveland, Oaio, a corporation of of the final product desired. The solution is then left B to cool to about 30° C., whereupon a crop of alkali No Drawing. Fied May 28, 1959, Ser. No. 826,368 metal iodide crystals is separated. 9 Cainas. (C. 23-89) The following are specific examples of the various purification processes for alkali metal iodides. This invention relates to a new method for the puri O fication of alkali metal iodides such as lithium iodide, Variation I cesium iodide and rubidium iodide. (A) Starting materials: The invention has particular significance where the Sodium iodide containing 16 p.p.m. potassium alkali metal iodide is used in the preparation of scintila Hydriodic acid 43% tion crystals. Sodium iodide has been found to pro 5 duce suitable optical crystals which are especially use 60 g. Nai were dissolved in 45 ml. HI (43%) hot. ful when employed as scintillation crystals. However, Solution was cooled to about 30° C. whereupon a crop as sci?tillation crystals are used as sensing devices for of crystals, largely Na2H2O, separated. These were. radiation energy, every effort must be made to reduce drained of acid mother liquor and samples of crystals the amount of radioactive material contained in the 20 (product) dried. Sample of acid mother liquor was scintillation crystal itself. Sodium iodide and related evaporated to dryness. Potassium analysis: alkali metal iodides contain potassium impurities which, P. p.m. in turn, contain quantities of a natural radioactive isotope NaI product--------------------------------- 7.0 Ké0 which emits both beta and gamma radiation. The Nai from acid mother liquor----------------- 60.0 presence of potassium is cbjectionable to such an extent (B) Starting materials: that the contamination of sodium iodide with only a few Na containing 30 p.p.m. potassium parts per million of potassium will render a scintiilation crystal produced from such materials unserviceable for HI (43%) certain applications, 800 g. Nai were dissolved in 600 ml. hot Hi plus 5 It is, therefore, alth object of this invention to purify 30 ini. H.C. Charge was cooled to about 30. C. where alkali metal iodides. It is another object of this inven upon a crop of crystals, largely Nai.2H2O separated. tion to purify alkali metal iodides by the removal of These were filtered from the acid mother liquor, Sam potassium contaminants. ple of crystals was dried and analyzed. Potassium con it is still another object of this invention to prepare tent of dry product (NaI)-0.4 p.p.m. " sodium iodide scintillation crystals substantially free from 35 radioactive potassium impurities. (C) Starting materials: The alkali metal iodide starting materials refined by Nai containing 6.2 p.p.m. potassium the process of this invention are C.P. grades of alkali H 42% metal iodides, which usually contain contaminating po tassium-impurities of the order of about 10 parts per 800 g. Na were dissolved in 600 ml. hot HI (42%) inillion to 15 parts per million, although by present plus 10 ml. H.O. Solution was cooled to about 30 industrial standards this value may be less than 10 parts C. whereupon a crop of crystals, largely Na.2H2O, per million or as high as 100 parts per million. U.S.. separated. These were filtered from the acid mother grades of alkali metal iodides may also be used if the liquor. Sample of crystals (product) was dried and potassium is in the desired range. The alkali metal 45 analyzed. Sample of acid mother liquor was evaporated iodide starting material is purified by first dissolving in to dryness and analyzed. Potassium analysis: a liquor consisting of water and hydriodic acid and then Pp.m. crystallizing from said liquor, whereby purified alkali Nal product.--------------------------------- 1.5 metal iodide crystals are formed, while substantial pro NaI fron acid mother liquor----------------- 41.0 portions of said potassium contaminants remain in the 5 resulting mother liquor. (D) Starting materials: The basic procedure has been divided into three major Cesium iodide containing 485 p.p.m. potassium variations depending upon the expenditure of hydriodic C.P. Hydriodic acid 48% acid and the degree of purity desired in the final prod uct. In the first variation of the basic procedure the 55 500 grants of CsI were dissolved in a minimum amount alkali metal iodide is merely dissolved in hot aqueous of water. 50 ml. of 48% H) was then added. The hydriodic acid of a preferred concentration of about solution was evaporated by boiling until an appreciable 43%, although other commercially available grades of mass of Csi crystals were produced. The charge was aqueous concentrations from about 40% to 55% may cooled to about 30° C. and then filtered. The yield of be employed. The alkali metal iodide solution is then 6 dry Csi crystals was 376 g. A sample of the acid cooled to about 30 C., whereupon a crop of alkali. mother liquor was evaporated to dryness and analyzed, metal iodide crystals will separate out. the second Potassium analysis: variation of the basic procedure an aqueous solution P. p.m. of alkali metal iodide is boiled until a saturated solu Starting Cs stock--- urs m n n wou - win we was a w------------ 485 tion is produced. Hydriodic acid is then added until 65 Crystal product------------------------------ 93 a pH of about 1.0 is reached. The solution is then cooled to about 30° C., whereupon a crop of alkali metal Cs from acid mother liquor----------------- - 2090 iodide crystals will separate out. The third variation NoTE: In above experiments “hot” solutions of HI of the basic procedure embodies the formation of a for dissolving Na were in the range of 85 C. to 95 solution of alkali metal iodide in water and the lower 70 C. Filtrations were made on fritted glass funnels. HI ing of the pH to about 1.0 by the addition of hydriodic used - was of C.P. quality but varied in strength as in acid. The solution is then evaporated by boiling until dicated in the preceding and following experiments. 3,002,81.i. 3. 4. Variation II NaI.2H2O, separated. These were drained (not filtered) Starting materials: from acid mother liquor. Sample of drained crystals NaI containing 64 p.p.m. potassium was taken, dried and analyzed for potassium. P. p.m. potassium. H 48% 5 800 g. NaI were dissolved in water and filtered. HE Analysis dry product (Nal)--------------------- 4.0 was added until solution pH was lowered to 1.0. Solu (E) Starting materials: tion was evaporated by boiling until saturated, then Nal containing 9.7 p.p.m. potassium cooled to about 30° C. whereupon a crop of crystals, His 47% largely Na.2H2O, separated. These were filtered from O i.0 kg. Na was dissolved in distilled water and filtered. mother liquor and a sample was taken, dified and then Hii was added until pH of solution reached 1.0-0.1. analyzed for potassium. Analysis dry product: 29.8 Solution was evaporated by boiling until saturated. H p.p.m. potassium. (47%) was immediately added, with mixing, in an Variation III amount equal in volume to 10% of the volume of the (A) Starting materials: 15 saturated Na solution. Product was left to cool to Nai containing 64 p.p.m. potassium about 30° C., whereupon a crop of crystals, largely H 48% Na.2H2O, separated. These were filtered from acid mother liquor. Sample of filtered crystals were taken, 800 g, NaI were dissolved in water and filtered. H dried and analyzed for potassium. was added until solution pH was lowered to 1.0-0.1. 20 Solution was evaporated by boiling until saturated. At P. p.m. potassium this point volume of saturated solution was determined Analysis dry product (Nai).--------------------- 0.6 and to this solution there was added HI (48%)-45 ml., (F) 500 g. Li was dissolved in water and potassium equal in volume to 10% of the saturated solution volume. iodide was added thereto. A sample of the solution was Hot solution was well mixed and left to cool to about 30 25 analyzed for potassium. pH of the Li charge was ad C. whereupon a crop of crystals, largely Nai.2H2O, sep justed to 1.0 using Hi 48% C.P. The acid solution was arated. These were filtered from mother liquor. Sample evaporated by boiling to the point where a yield of of crystals was taken, dried and analyzed for potassium. about 70% of the starting batch could be obtained when Analysis dry product (Na)-6.0 p.p.m. potassium. charge was cooled to 30° C. While still hot there was (B) Starting materials: 30 added to the charge Hi 48%. C.P. equal in volume to NaI containing 64 p.p.m. potassium 10% of the volume of the evaporated Li solution. The HI 48% charge was set aside to cool and crystallize, whereupon 800 g. NaI containing 64 p.p.m. potassium were dis a crop of crystals (Lii.3HO) separated. Crystals were solved in water and filtered. H was added until solu separated by filtration from the acid mother liquor. A tion pH was lowered to 1.0-0.1.
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