The invention discloses an efficient and safe
microwave digestion-
atomic fluorescence detection method for total
selenium in soil, and belongs to the technical field of
analytical chemistry and environmental detection.According to the method, the content of total
selenium in
selenium-rich soil is rapidly, accurately and safely measured by optimizing the sample weighing amount, the
microwave digestion procedure and the detection conditions, and the detection accuracy is improved. The method comprises the following specific steps: weighing 0.1 g of an air-dried and sieved selenium-rich soil sample, adding 5mL of concentrated
nitric acid, then carrying out a
microwave digestion process of heating to 175 DEG C for 12 minutes and maintaining for 48 minutes, after digestion, adding 5mL of 6mol / L
hydrochloric acid, carrying out acid removal reduction at 140 DEG C, fixing the volume to 15mL by using 5% diluted
hydrochloric acid, and finally determining by using an
atomic fluorescence spectrophotometer by using 5%
hydrochloric acid as a
carrier current and 1%
potassium borohydride and 0.5%
potassium hydroxide as reducing agents. According to the method, the use of dangerous reagents such as
hydrofluoric acid and
perchloric acid is avoided, the detection period is remarkably shortened, the
linear range is 0-10 mu g / L, and the
correlation coefficient is Rgt; the average
recovery rate is up to 101.13%-101.51%, and the precision is RSDlt (Research Standard Defect); the requirements of
rapid detection of the total selenium content of the selenium-rich soil, agricultural production and
environmental evaluation are met.