Purification of chromium (VI) for use in the PBI determination.
نویسندگان
چکیده
In connection with the determination of serum protein-bound iodine (PBI), it is occasionally advantageous to have available reagents with a very low iodine blank. Of the reagents required in a PBI procedure employing dialysis, wet combustion with 112S04 and Cr (VI), volatilization of iodine after liberation with 113P03, and estimation of iodine by means of the Ce (IV)-As (III) reaction, the Cr (VI) contributes most of the iodine blank. Although Cr03 and Na2Cr2O7 can be obtained having as little as 5 X 10-s Gm. I per Gm. Cr, the value is often much higher. Of various procedures undertaken for preparing Cr (VI) which is essentially free of iodine, conversion to chromyl chloride has proved most satisfactory. Using the method recommended by Fernelius (1), a batch of heavily contaminated Cr03 containing 88 x 10 Gm. I per Gm. Cr, for example, was converted to crude CrO2Cl2 containing 1 X 10 gm. I per Gm. Cr, with a yield of 66 per cent. Studies utilizing 1131 (as Nal) added to the initial Cr03 solution confirmed the efficiency of the separation by indicating better than fiftyfold purification. The crude chromyl chloride can be diluted with water and used with concentrated sulfuric acid for wet combustion of serum in the PBI determination. The digestion, however, had best be carried out in a wellventilated hood because of the noxious fumes evolved.
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ورودعنوان ژورنال:
- Clinical chemistry
دوره 1 2 شماره
صفحات -
تاریخ انتشار 1955