Iodates preparation

A solution of sodium iodate, prepared from lOg of iodine according to (I), is diluted to 120ml with water and 4g of sodium hydroxide are added. Twenty-two grams of potassium persulfate are used as m (II) and then a second portion of 17g sodium hydroxide is added. The mixture is boiled for 15 minutes longer, then cooled to 40° C, and the liquid is decanted. The solid is broix it on to the filter with about 25ml of ice water, pressed dry, and then heated at 110°C for one or two hours. 

Ha.la.tes, Silver chlorate, AgClO, silver bromate, AgBrO, and silver iodate, AglO, have been prepared. The halates may decompose explosively if heated. 

Tellurium perchlorate, iodate, and methylthiosulfate, as weU as Te(IV) salts of aUphatic and aromatic acids, have been prepared. 

Bromates and iodates are prepared on a much smaller scale, usually by chemical oxidation. For example, Br is oxidized to Br03 by aqueous hypochlorite (conveniently effected by passing... 

The product is the dihydrogen orthoperiodate N33H2I06, which is a convenient starting point for many further preparations (see Scheme on next page). Paraperiodates of the alkaline earth metals can be made by the thermal disproportionation of the corresponding iodates, e g. ... 

In the second method a solution of the approximate strength required is prepared, and this is standardised against some standard alkaline substance, such as sodium tetraborate or anhydrous sodium carbonate standard potassium iodate or pure silver may also be used (see Section 10.84). If a solution of an exact strength is required, a solution of an approximate strength somewhat greater than that desired is first prepared this is suitably diluted with water after standardisation (for a typical calculation, see Appendix 17). 

Preparation ofpure potassium hydrogeniodate. Dissolve 27 g of potassium iodate in 125 mL of boiling water, and add a solution of 22 g of iodic acid in 45 mL of warm water acidified with six drops of concentrated hydrochloric acid. Potassium hydrogeniodate separates on cooling. Filter on a sintered-glass funnel, and wash with cold water. Recrystallise three times from hot water use 3 parts of water for 1 part of the salt and stir continuously during each cooling. Dry the crystals at 100 °C for several hours. The purity exceeds 99.95 per cent. 

The standard solution is prepared by dissolving a weighed amount of pure potassium iodate in a solution containing a slight excess of pure potassium iodide, and diluting to a definite volume. This solution has two important uses. The first is as a source of a known quantity of iodine in titrations [compare Section 10.115(A)] it must be added to a solution containing strong acid it cannot be employed in a medium which is neutral or possesses a low acidity. 

For the preparation of standard iodine solutions, resublimed iodine and iodate-free potassium iodide should be employed. The solution may be standardised against pure arsenic(III) oxide or with a sodium thiosulphate solution which has been recently standardised against potassium iodate. 

Procedure Preparation of 0.05A/ iodine. Dissolve 20 g of iodate-free potassium iodide in 30-40 mL. of water in a glass-stoppered 1 L graduated flask. Weigh out about 12.7 g of resublimed iodine on a watchglass on a rough balance (never on an analytical balance on account of the iodine vapour), and transfer it by means of a small dry funnel into the concentrated potassium iodide solution. Insert the glass stopper into the flask, and shake in the cold until all the iodine has dissolved. Allow the solution to acquire room temperature, and make up to the mark with distilled water. 

The standardisation of thiosulphate solutions may be effected with potassium iodate, potassium dichromate, copper and iodine as primary standards, or with potassium permanganate or cerium)IV) sulphate as secondary standards. Owing to the volatility of iodine and the difficulty of preparation of perfectly pure iodine, this method is not a suitable one for beginners. If, however, a standard solution of iodine (see Sections 10.112 and 10.113) is available, this maybe used for the standardisation of thiosulphate solutions. 

Note. This is prepared by dissolving 5 g of potassium iodate in 167 mL of concentrated nitric acid, and diluting to 500 mL. 

Procedure. Acidify the iodate solution (lOOmL containing ca 0.3 g of I03) (see Note) with sulphuric acid, and pass in sulphur dioxide (or add a freshly prepared saturated solution of sulphurous acid) until the solution, which at first becomes yellow, on account of the separation of iodine, is again colourless. Boil off the excess of sulphur dioxide, and precipitate the iodide with dilute silver nitrate solution as described in Section 11.64. Weigh as Agl. 

Cerium, D. of as oxide via iodate, (g) 453 Cerium(IV) ammonium nitrate see Ammonium cerium(IV) nitrate Cerium(IV) ammonium sulphate see Ammonium cerium(IV) sulphate Cerium(IV) hydroxide 380 preparation of, 380... 

Vicinal iodo carboxylates may also be prepared from the reaction of olefins either with iodine and potassium iodate in acetic acid/ or with N-iodosuccinimide and a carboxylic acid in chloroform. " A number of new procedures for effecting the hydroxylation or acyloxylation of olefins in a manner similar to the Prevost or Woodward-Prevost reactions include the following iodo acetoxylation with iodine and potassium chlorate in acetic acid followed by acetolysis with potassium acetate reaction with iV-bromoacetamide and silver acetate in acetic acid reaction with thallium(III) acetate in acetic acid and reaction with iodine tris(trifluoroacetate) in pentane. ... 

During the preparation of the quaternary oxidant tetraethylammonium iodate from the aqueous reagents, the residue after vacuum evaporation of most of the water exploded, breaking the flask. This was attributed to possible presence of excess periodic acid in the reaction mixture [1]. Further details and precautions to avoid heating the salt, normally stable in storage, are given [2],... 

MRH Barium chlorate 5.06/83, calcium chlorate 5.61/77, potassium chlorate 6.07/76, sodium bromate 4.98/80, sodium chlorate 7.32/75, zinc chlorate 6.11/76 Dry finely divided mixtures of red (or white) phosphorus with chlorates, bromates or iodates of barium, calcium, magnesium, potassium, sodium or zinc will readily explode on initiation by friction, impact or heat. Fires have been caused by accidental contact in the pocket between the red phosphorus in the friction strip on safety-match boxes and potassium chlorate tablets. Addition of a little water to a mixture of white or red phosphorus and potassium iodate causes a violent or explosive reaction. Addition of a little of a solution of phosphorus in carbon disulfide to potassium chlorate causes an explosion when the solvent evaporates. The extreme danger of mixtures of red phosphorus (or sulfur) with chlorates was recognised in the UK some 50 years ago when unlicenced preparation of such mixtures was prohibited by Orders in Council. 

Fluorescein (147) is prepared by the same route as Pigment Red 90 (see p. 575). The compound is iodized with iodine and potassium iodate in an acidic medium. The iodic acid reoxidizes the resulting hydrogen iodide back to iodine ... 

Theory First of all the potassium iodate is dried to a constant weight at 110°C to make it completely free from moisture and then brought to room temperature in a desiccator. It is pertinent to mention here that KI03 is a very stable salt and may be obtained in a very pure form. Therefore, it is possible to prepare the standard solutions of KI03 by dissolving the calculated weight of the salt in water and diluting the same to an approximate volume. 

Unexpected uniformities observed in the impact-sensitivities of a group of 22 amminecobalt oxosalts are related to kinetic factors during the initiation process [6], A series of ammine derivatives of cadmium, cobalt, copper, mercury, nickel, platinum and zinc with (mainly) iodate anions was prepared and evaluated as explosives [7], Earlier, ammine and hydrazine derivatives of cadmium, cobalt, copper and nickel with chlorate or perchlorate anions had been evaluated as detonators. Dihydrazinecopper(II) chlorate had exploded when dried at ambient temperature [8],... 

Several explosive salts including the acetylide, azide, borate, bromate, chlorate, chromate, iodate (and ammonium iodate double salt), nitrite, perchlorate (and ammonium perchlorate double salt), periodate, permanganate, picrate and trinitrobenzoate were prepared. The 3 latter salts and the acetylide, azide and bromate are impact-sensitive detonators [1], It appears probable that many of the explosively unstable compounds [2], formed in various ways from interaction of mercury or its compounds with ammonia or its salts, may have the common polymeric structure now recognised for Millon s base [3], This is a silica-like network of N+ and Hg in 4- and 2-coordination, respectively, with OH and water in the interstitial spaces. Individually indexed compounds are Poly(dimercuryimmonium acetylide)... 

Iodic acid may be prepared by the reaction of sulfuric acid with barium iodate. The solution is fdtered to remove barium sulfate and then crystaUized to obtain iodic acid ... 

Another method of preparation that does not involve the formation of iodate is by treating iron turnings with iodine solution. The product, ferroso-ferric iodide, Fesls I6H2O, is boiled with 15 wt% potassium carbonate solution ... 

---