Objective:To study the application of antimony cerium catalytic spectrophotometry using a fully automatic biochemical analyzer (hereinafter referred to as this method) in the determination of water iodine.Methods:Based on the principle of antimony cerium reoxidation reduction reaction catalyzed by iodine, the iodine content in water was determined in the range of 0 - 100 μg/L iodine mass concentration. The detection limit, precision and accuracy (determination of standard substances GBW09113j and GBW09114j for iodine composition analysis in water and the experiment of standard recovery) of this method were verified. This method was compared with the arsenic and cerium catalytic spectrophotometry recommended by the National Reference Laboratory for Iodine Deficiency Disorders.Results:Within the range of 0 - 100 μg/L iodine mass concentration, the qualitative and quantitative detection limits of this method were 0.81 and 2.70 μg/L, respectively (sampling quantity was 35 μl). In the precision experiment, the relative standard deviation of water samples with different iodine mass concentrations ranged from 1.2% to 4.0%. The determination results of the standard substances GBW09113j and GBW09114j for iodine composition analysis in water were both within the given standard value range. The standard recovery rates of water samples with low, medium and high iodine mass concentrations ranged from 101.0% to 106.0%, and the total average standard recovery rate was 103.2%. The results of the method comparison experiment showed that there was no statistically significant difference in the results of water iodine determination between the two methods ( t = - 0.78, P = 0.779). Conclusion:This method has a low detection limit, high precision and good accuracy, making it suitable for the detection of large quantities of samples in the monitoring of iodine deficiency disorders.

Objective:To establish a hydride generation atomic fluorescence method using ammonium persulfate as the digestion reagent for determination of arsenic in urine (hereinafter referred to as this method).Methods:The collected urine samples with ammonium persulfate were heated and digested on the tubular electric heating automatic control constant temperature digester (60 holes), with 5% hydrochloric acid solution as reaction medium and current carrier and 1.5% potassium borohydride solution as reducing agent. Arsenic content was determined with a four-channel atomic fluorescence spectrometer. The arsenic standard solution of 0 - 10 μg/L was prepared to determine the standard curve of this method, and the method was evaluated from the detection limit, linear range, correlation coefficient, precision, standard addition recovery experiment, and urine arsenic quality control sample detection. The standard method "Determination of Arsenic in Urine by Hydride Generation Atomic Fluorescence Spectrometry" (WS/T 474-2015, referred to as the standard method) was used for comparison experiments.Results:When the sampling volume was 1 ml, the detection limit of this method (digest with 1 ml 1.5 mol/L ammonium persulfate) was 0.03 μg/L. In the range of arsenic content from 0 - 10 μg/L, the linear relationship between arsenic content and fluorescence intensity was good, and the correlation coefficients ( r) were all 0.999 9. The relative standard deviations( RSD) of the three replicates of urine samples with different concentrations were 1.00%, 0.89% and 0.49%, respectively. Urine arsenic quality control samples were tested, and the test results were all within the range of public values; the overall average recovery was 102.29%, and the recovery range was 92.10% - 108.15%. Compared with the standard method in the determination results of 20 urine samples, the difference was not statistically significant ( t = - 0.40, P > 0.05). Conclusions:The hydride generation atomic fluorescence spectrometry using ammonium persulfate as digestion reagent for the determination of arsenic in urine has the advantages of low detection limit, good precision, high accuracy, small amount of sampling and digestion reagent, simple operation, and less harmful gas generation in sample pretreatment. It is suitable for rapid determination of arsenic in urine in large quantities.