| Separation methods of trace zirconium in uranium and determination of zirconium in nuclearmaterial are reviewed.Because the concentration of zirconium in uranium has large ranges,from 1.50xlO'6-3.8g/gU,Not only how to decrease the remainder of uranium to eliminate its determinate effect but also how to acquire higher recovery of zirconium is considered,so the method of silica gel,the method of TBP levextrel resin chromatography,the method of TTA chromatography and the method of TTA extraction are compared. Then TTA extraction is chosen to acquire the ideal separation purpose.Compared with ICP-MS and ICP-AES,XRF has characters of high repeatability,stability,low cost,high concentration elements analysis,the ability to determinate solid sample and having comprehensive practicability,but XRF has lower sensitivity,so how to increase the concentration of the sample to acquire better precision is a difficult problem,the optimum of operating condition:the integral time of spectral lines is 60s,the integral time of background lines is 20s,the voltage of XRF is 50KV,the electric current is 50mA. The optimum method of TTA extraction:the extracting agent cocentration is 0.5mol/L,the diluent is xylene,the extracting media is nitric acid,its concentration is 4mol/L,the extracting time is lOmin. The recovery can reach 95% after it extracts once,RSD% is lower than 10%,the detection limit of zirconium is 1.3u.g/mL. And increasing the application of film in XRF is studied. The method of using organic sample to make resource after extracted by TTA can be used to determine zirconium in simulated process solution of spent fuel reprocessing quickly and veraciouly.ICP-MS has some advantages,such as high sensitivity,lack of chemical interferences,low detection limits. It can determine the elements in water. When TTA is used to extract zirconium in uranium,the combination of zirconium and TTA is very strong,the concentrated acid of nitric acid and hydrochloric acid can not destroy their combination. Back extraction by HNO3-HF and back extraction by concentrated HNCh after lower the concentration of organic phase are studied,the method of back extration by HNOrHF can not be used to ICP-MS,because some zirconium is hydrolysis when HF is removed by heat. However,the method of back extraction by concentrated nitric acid after lower the concentration of organic phase can be used to ICP-MS,the recovery is93.2%,RSD% is 5.24%,the decontamination factor of uranium is 3.2xl04,the detection limit of zirconium is 0.04ng/mL. The method of TTA extracting trace zirconium in uranium is firstly used to ICP-MS,the result is satisfied,it can be used to determine zirconium in uranic production quickly and veraciously.CID-ICP-AES has the advantages of high sensitivity,high Signal-to-Noise and high quantum efficiency,which nearly reaches theoretical limit value of theoretical parts of an apparatus;it can memorize thousands of spectra lines at the same time. CID-ICP-AES is the newest model,and there are still few articles to report analytical character of this type,as this result the optimum of operating condition and the effect of analytical parameters for photometric precision,Signal-to-Noise and detection limits are studied:R.F.Power is 11 SOW,nebulizer pressure is 28psi,the measurement time is 3 times and the integral time is 20s. The method of TTA extracting trace zirconium in uranium is firstly used to ICP-AES,the recovery is 93.2%,the detection limit of zirconium is 0.001|ig/mL. The method can be used to determine low concentration of zirconium. |
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