Microwave digestion method for processing silica samples by orthogonal experimental study design digestion temperature, retention time and solvent effects on digestion digestion effect, optimized microwave digestion silica sample digestion parameters. And inductively coupled plasma atomic emission spectrometry (ICP-AES) Determination of the content of sol Fe, Na, K impurity elements. The results showed that the optimized parameters for the sol digestion: digestion temperature of 160 ℃, retention time of 4 min, the amount of hydrochloric acid and hydrofluoric acid were 2.0 and 1.0 m L. The method Fe, Na, K element detection limits were: 0.002,0.002 and 0.003μg / m L, Fe, Na, K spiked recoveries were between 97% to 103% and the relative standard deviation (RSD ) were less than 2%, with good accuracy and precision. Method is simple, accurate and reliable, fully able to meet analysis.
Selection of nitric acid - hydrofluoric acid - sulfuric acid system to decompose sample, extraction of 50% nitric acid, Inductively Coupled Plasma Mass Spectrometry rocks scattered elements germanium without using hydrochloric acid and perchloric acid in the sample preparation process, avoiding Cl Effect of Ge result, the optimum conditions for dissolution of the sample detection limit (3 s) to:. 0.03 μg · g-1, precision (RSD%, n = 6) as follows: 1.30% - 3.94%. The assay method has high sensitivity, precision and less interference, analysis speed, wide linear range, easy to operate, and other advantages. with this method GBW07103 a national standard, GBW07107, GBW07122 measured showed that the results with the standard value match.
Weighed amount Kovar samples with hydrochloric acid, nitric acid dissolution, the dissolved silica hydrofluoric acid, perchloric acid smoke, in addition to carbon. Ammonium citrate as a masking agent, oxidation with hydrogen peroxide Co2 + to Co3 +. Under conditions of pH = 7 to 8, nickel dimethylglyoxime generation of nickel dimethylglyoxime precipitate. After precipitation aging for one hour, after 140 ± 5 ℃ and dried to constant weight.
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