陶粒支撑剂元素分析方法对比研究

Comparative Study on Element Analysis Methods for Ceramic Proppants

陶粒支撑剂元素组成复杂、多样,传统化学滴定法存在步骤繁琐、检测结果易受干扰的问题。为了选择准确、可靠的方法进行陶粒支撑剂元素组成检测和分析,分别采用多元素快速分析仪(MER)、X射线荧光光谱仪(XRF)、电感耦合等离子体质谱仪(ICP-MS)检测了已知元素成分含量的陶粒支撑剂(参考样)的元素组成,包括Al_(2)O_(3)、SiO_(2)、Fe_(2)O_(3)、TiO_(2)、K_(2)O、Na_(2)O、CaO、MgO。通过对检测结果的精密度和准确度的对比和分析,确定不同检测方法的特点和适用性。结果表明:3种方法的标准偏差均小于1,相对标准偏差均小于14.63%,与参考样对比的相对误差均小于10.12%,说明3种方法均能进行陶粒支撑剂元素组成检测。其中,MER检测结果精密度和准确度最差,XRF和ICP-MS相对较好;ICP-MS可用于主晶相和过渡元素检测,包括Al、Si、Fe、Ti,检测结果准确度(小于1.03%)和精密度(小于2.05%)较高;XRF可用于助烧剂K、Na、Ca、Mg元素检测,检测结果准确度(小于1.80%)和精密度(小于4.65%)较高。

Because the element composition of the ceramic proppants is complex and diverse,there exist problems of cumbersome steps and easily interfering detection results in the traditional chemical titration methods.In order to provide the accurate and reliable methods for detecting and analyzing the elemental composition,three methods of multi-element rapid analyzer(MER),X-ray fluorescence spectroscopy(XRF),and inductively coupled plasma mass spectrometry(ICP-MS),are used to detect ceramic proppants reference samples with known elemental composition.The elemental composition are calculated as the detected oxides including Al_(2)O_(3),SiO_(2),Fe_(2)O_(3),TiO_(2),K_(2)O,Na_(2)O,CaO and MgO.The characteristics and applicability of different methods is determined via comparing and analyzing the precision and accuracy of the detection results.The results show that the standard deviation of the three methods is less than 1,the relative standard deviation is less than 14.63%,and the relative error compared with the reference sample is less than 10.12%,indicating that all the methods can detect the elemental composition of the ceramic proppants.The detection results obtained by the XRF and ICP-MS have higher repeatability and accuracy than those of the MER.The ICP-MS can be used for the detection of the main crystal phases and transition elements,such as Al,Si,Fe and Ti,with high accuracy(less than 1.03%) and high precision(less than 2.05%).The XRF can be used for the detection of K,Na,Ca and Mg in the sintering aids,with high accuracy(less than 1.80%) and high precision(less than 4.65%).