Determination Of Germanium In Goal By Atomic Fluorescence Spectrome

Cermanium is an important companion element in coal.The accurate determination of cermanium is a prerequisite for the accurate evaluation of cermanium in coal.This paper collected coal samples from different areas of Shanxi Huairen,Shaanxi Binchang,Anhui Huainan,Shandong Zaozhuang,Shandong Yinzhou,Inner Mongolia Tongliao,etc.,focusing on the sample pretreatment method and the influence mechanism of the working conditions of the atomic fluorescence spectrometer,and established the hydride.-A method for the determination of antimony in coal by atomic fluorescence spectrometry,and the feasibility evaluation and uncertainty analysis of the method were carried out,and the following conclusions were drawn:(1)hydride-atomic fluorescence spectrometry can be used to determine the best instrument operating parameters for coal bismuth:(1)The optimal parameter for the negative voltage of the photomultiplier tube is 270 volts,(2)The integration time is 10 seconds,(3)The optimum parameter for the atomizer temperature is 200 degrees Celsius.,(4)The lamp current parameter of the hollow hollow cathode lamp is 80 mA,(5)The delay time is 0.5 seconds,(6)The optimum parameter for carrier gas flow in the equipment is 300 ml per minute,(7)The carrier fluid is a 20% phosphoric acid solution,(8)2.0% potassium borohydride is a reducing agent(currently available).(2)The optimum pretreatment process parameters for the determination of cermanium in coal by hydride-atomic fluorescence spectrometry are:The coal sample half-opening door is ashed,kept at a temperature of 500? for 2 h,and after heating to620?,continue to ash for more than 2 h.When disposing of the ash sample,take it out when it is decomposed into a wet salt.Phosphoric acid extraction was used in the experiment.When the acidity was 20%,the sensitivity of the test signal was the highest.(3)The test method has good precision and accuracy for the test of bismuth in coal.Verify that the reference material results are within the allowable error range;The recoveries of spiked samples are between 90% and 120%.The relative standard deviations of coal samples and standards in different content ranges are less than 5.0%,and the precision and repeatability are better.The linear range of the method is5~100?g/L.Linearity can reach up to three nine,the detection limit of the method is0.061?g/g;the relative error of test results of different experimental personnel is less than 10%,the consistency of different laboratory measurement results and the inspection of outliers,the method repeatability is obtained.The limit was 0.440 ?g/g,and the reproducibility limit was 0.701 ?g/g.Uncertainty analysis of the method:The uncertainty of the sample weighing,processing,constant volume,working curve fitting and repeatability measurement results were investigated.The uncertainty of the expansion of the cerium content in the coal sample was calculated,and the precision and accuracy of the measurement method were calculated.All are better.(4)The results of the thesis supplement the test method for the content of antimony in the national standard coal.The modern instrument analysis and testing technology reduces the experimental process and introduces the experimental part of the error.The test efficiency is high;the test detection limit can reach ng/g level,and the precision is better.High,the absolute error of the sample is small,which solves the problem of testing the low content of bismuth in coal.This method can accurately measure the reserves of strontium in coal seams,which is of great significance for the investigation,evaluation and development of strontium resources.This paper has 15 pictures,18 tables,and 123 references.