针对艾士卡法、库仑滴定法、高温燃烧中和法和红外光谱法等现有国家标准煤中全硫含量测量方法所需化学试剂多、操作复杂和耗时较长的问题，提出了一种采用能量色散型X射线荧光光谱仪快速、无损和可靠测定煤中全硫含量的方法。该方法是一种相对分析方法，通过将未知样品与已知硫含量的样品谱图对比以进行定量分析。通过实验确定了应用该方法分析煤中硫元素的适宜制样方式、制样条件和测量条件;经过样品数据采集、谱图预处理和基体校正后，建立了相应的校准曲线。结果表明:硼酸镶边垫底压片法的制样效果良好，在12 MPa、保压40 s条件下可获得表面光滑平整、不易破裂的样片;实验所确定的硫元素测量管电压和管电流分别为13 kV和800 μA;采用真空装置可以有效控制轻基体背景散射严重及硫元素特征谱线易被空气吸收的问题;通过减小样品粒径和采用经验系数法校正相结合的办法可以降低基体效应的影响;对谱图进行平滑预处理后，有效地增强了谱图分辨率，提高了测量准确性。能量色散型X射线荧光光谱法可将煤中全硫含量的测量时间压缩至60 s;所建立的校准曲线R2为0.996 3，随机选取10个待测样品，除个别样品的测量结果略有差异外，其余均在库仑法的范围内;特低硫样品的再现性和重复性试验RSD分别为3.21%和1.57%，低中硫样品对应的RSD分别为0.56%和0.47%，中高硫样品的RSD分别为0.26%和0.22%。

Eschka method,Coulometric Titration method,High Temperature Combustion method and Infrared Spectroscopy method have been used to determine the total sulfur content in coal by Chinese national standards,which have several shortcomings,such as more chemical reagents consumption and complicated operating procedure. Based upon Energy Dispersive X-Ray Fluorescence ( EDXRF) spectrometer, a rapid, reliable and non-destructive method has been developed for determining the total sulfur content in coal. As a relative analysis method,EDXRF obtains the total sulfur content in any coal by comparing the spectra with those of known samples. The preparation procedure of samples was explored,and the measuring conditions were selected for determining the sulfur content in coal. A reasonable calibration curve was suggested after sample data collection,spectral pretreatment and matrix correction. Experimental results show that smooth and unbreakable tablets are obtained by employing powder tableting with boric acid as adhesive at 12 MPa for 40 seconds. 13 kV and 800 μA are reasonable voltage and current,respectively. A vacuum device adopted in this study can reduce the scattering caused by light matrix as well as the absorption of sulfur’s characteristic X fluorescence line by air. The matrix effect can be corrected by using the empirical coefficient method together with small particle size. The resolution of selected spectra is enhanced and the accuracy of measured data is improved when smooth method is used for pretreatment procedure. The method suggested in this study could shorten the measuring time to 60 seconds and R2 is 0. 996 3 for the correction curve. EDXRF data from 10 random samples are consistent with Coulomb Method except two of them. The relative standard deviation (RSD) of the reproducibility and repeatability tests are respectively 3. 21% and 1. 57% for ultra-low sulfur coal samples,whilst 0. 56% and 0. 47% for lowmedium sulfur coal ones,0. 26% and 0. 22% for medium-high sulfur samples.