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United States Patent Office Patiented Sept 2,904,470 United States Patent Office Patiented Sept. 15, 1959 1 2 tion with bacteria or other organic matter, thus pro longing the activity of the solution. It is known that when elemental iodine is dissolved in 2,904,470 water a minute quantity of hypoiodous acid is formed. DIATOMICIODINE-HYPOIODOUS ACID GEN 5 However, this quantity of hypoiodous acid is too small to :ERATING COMPOSITIONS provide any useful therapeutic effect. It should be noted Abraham Berliner and Benjamin Carroll, New York, N.Y. that the solutions of the present invention contain hy poiodous acid at a concentration greater than that pro "No Drawing. Application December 1, 1955 duced when iodine is dissolved in water. Also the solu Serial No. 550,463 0 tions are preferably essentially free from iodide and tri iodide ions. 7 Claims, (Cl. 167-70) We have further found that aqueous solutions of diatomic iodine and hypoiodous acid are relatively un stable and that if effective germicidal action is to be This invention relates to germicides and more par 5 achieved the solutions must be prepared under carefully -ticularly to a novel iodine containing composition that controlled conditions as described herein. Because of the is adapted to be dissolved in water to produce an aqueous comparative instability of the solutions, it is desirable solution of diatomic iodine and hypoiodous acid, which that they be prepared shortly before they are used and solution is also new and possesses improved germicidal accordingly the present invention contemplates the use properties. Germicidal iodine-containing solutions made 20 of a solid composition which is readily soluble in water according to the present invention may be used for either and contains all the ingredients necessary to produce the therapeutic purposes or as sterilizing agents for a variety desired germicidal solution. One type of solid composi of non-therapeutic applications. The present application tion that has been found useful in preparing the present is a continuation-in-part of our pending applications Solutions comprises a water soluble metal iodide and a Serial No. 432,328, filed May 25, 1954, and Serial No. 25 chlorine-bearing organic compound which when dissolved 458,987, filed September 28, 1954, both of which are now , , in water yields hypochlorous acid. The reaction of hy :abandoned.- -. - pochlorous acid and metal iodide to form diatomic iodine It has of course been known formany years that iodine and hypoiodous acid may be represented by the follow and certain of its compounds possess useful germicidal ing equations: properties. Numerous iodine-containing compositions 30 have been previously proposed including aqueous and al coholic solutions of elemental iodine and solutions of elemental iodine in aqueous metal iodides, but all of these prior compositions have been subject to certain defects. We have further found that even if the solution is Thus iodine-in-aqueous solution.has not been extensively 35 freshly prepared from a solid composition as indicated 'used because it is difficult-to-dissolve, has only a limited above, it may still be too unstable to be practical unless solubility in water, and yields solutions which are not certain other factors are also controlled. For example, sufficiently stable to be...stored over extended periods of it has been found important to maintain the ratio of time. In general, such solutions are effective only when chlorine-bearing compound to metal iodide within par they are used shortly after they are prepared. To over 40 ticular limits if a reasonably stable solution is to be come these defects, solutions of iodine in aqueous metal achieved, and it has also been found that pH has an im iodides have been used. While the quantity of iodine portant bearing on the stability of the solution. The in solution can be greatly increased in this way, the iodine schlorine-bearing compound and metal iodide are desir in such solutions is in the form of tri-iodides which are ably used in such proportions that the molar ratio of not only. Substantially inferior to elemental iodine in their active chlorine in the chlorine-bearing compound to the 45 metal iodide is from 0.51 to 0.75. The pH of the solu germicidal properties but also are to some extent toxic tion should be maintained between 3 and 8, the optimum toward animal tissue. pH for most solutions being about 6. The desired con It is accordingly an object of the present invention to trol of pH can be conveniently obtained by incorporating provide a novel aqueous iodine-containing solution which in the solid composition a buffer which when dissolved ifor a given iodine concentration possesses improved e.g. in Water maintains the pH within the desired Tange. fast-acting, germicidal properties. It is another object 50 To produce the desired germicidal solution the solid sof-the-invention to provide an aqueous solution contain composition is dissolved in a sufficient quantity of water ring elemental iodine and an agent capable of re-oxidizing to give a solution containing from 5 to 600 parts per mil to elemental form iodine that has been converted to lion of diatomic iodine and from 3 to 100 parts per - iodine compounds by. reaction with organic matter...and million of HIO in excess of that normally present when bacteria. It is still another object of the invention to 55 diatomic iodine hydrolyzes in water. provide a solid composition which dissolves readily in proportions of chlorine-bearing compoundWhen andthe propermetal water to form such an aqueous solution and which can, iodide are used and the pH is maintained within the if desired, be formulated as a tablet. Other. objects of proper range, a solution essentially free from iodide and the invention will be in part obvious and in part pointed 60 tri-iodide ions is obtained. Such solutions retain a high out hereafter. - degree of germicidal activity, i.e. a degree of activity The present invention is based on our discovery that significantly greater than that given by elemental iodine aqueous solutions containing elemental iodine and hy alone, for a period of 5-minutes to an hour. The ratio poiodous acid prepared as described herein have improved of diatomic iodine to hypoiodous acid can be varied by germicidal activity. We have found that diatomic iodine varying the ratio of chlorine-bearing compound to metal 65 iodide in the solid composition, the higher ratios produc and hypoiodous acid in such solutions exhibit a synergistic ing higher HIO concentrations. The optimum ratio of effect, that is, the germicidal effectiveness of the solu 12 to HIO appears to be in the neighborhood of 5:1. stions is greater than would be expected from a mere mix Another factor that affects the stability of the solutions ture of these two substances. Moreover, the hypoiodous is the total concentration of germicidal ingredients. In acid acts to re-Oxidize and thereby re-generate that por 70 general dilute solutions are more stable than concen tion of the elemental iodine which is reduced by reac trated solutions, and their germicidal activity decreases 2,904,470 4. 3. A. more slowly. On the other hand the initial germicidal potassium biphthalate and more generally any known activity of dilute solutions is less than that of concen buffer which will maintain the pH of the solution be trated solutions. Thus for therapeutic applications it is tween 3 and 8 and will not interfere with the desired usually preferable to employ moderately concentrated reaction between the principal ingredients. solutions having a high-activity period of say 5 to 20 In addition to the chlorine-bearing compound, buffer minutes, whereas for sanitizing or general sterilizing pur and metal iodide, the present solid composition, partic poses it is ordinarily preferable to use a more dilute ularly if it is to be pressed into tablet form, may contain solution which retains its activity for 30 to 60 minutes. various other ingredients. For example, in order to as Solutions prepared in the manner indicated may be sist the tablet in dissolving in water it is frequently desir used for various therapeutic applications for which iodine 10 able to have the tablet effervesce, and to achieve such ef solutions have previously been used such as, for example, fervescence a quantity of sodium bicarbonate or other general topical applications in cases of infection and for suitable carbonate may be incorporated in the composi the prevention of infection. Also the solutions may be tion. In cases where the solution formed from the tablet used with advantage for non-therapeutic applications such is to be used as an oral lavage it may be desirable to in as for general sanitizing purposes. 5 clude a sweetener in the tablet. This sweetener should Usually all iodine solutions, even those supposedly be selected with some care to avoid incorporating an or containing purely elemental iodine, have small quantities ganic compound that is readily oxidized by the iodine or of tri-iodide and hypoiodous acid. This is due to some hypoiodous acid. We have found that sucrose or fructose extent to the hydrolysis of I2 in water according to are suitable for this purpose. The composition may also 20 include binders and inert fillers well known in the tablet equations: making art, provided that such components are non-re I.--HO=1---H+ -i-HIO active or substantially non-reactive with the principle in 2--I = gredients of the composition. The amount of tri-iodide resulting from the reaction In order to point out more fully the nature of the pres indicated by the above equations is negligible compared ent invention, the following specific examples are given of to the tri-iodide caused by the oxidation of slight quan 25 solid compositions capable of being dissolved in water tities of organic matter usually found in water and in to produce the solutions of the present invention.
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