微波消解微型化学实验快速测定云南磷矿石中的钙  

Rapid determination of calcium in Yunnan phosphate rock by microwave digestion and microscale chemical experiment

作　　者：欧志兵[1,2] 彭桦 李林[1] 杨稳权 何宾宾[1,2] 姜威[1,2] 李宁 朱桂华[1,2] 聂鹏飞 OU Zhibing;PENG Hua;LI Lin;YANG Wenquan;HE Binbin;JIANG Wei;LI Ning;ZHU Guihua;NIE Pengfei(Yunnan Phosphate Group Co.,Ltd.,Kunming 650600,China;National Engineering and Technology Research Center for Development and Utilisation of Phosphorus Resources,Kunming 650600,China)

机构地区：[1]云南磷化集团有限公司,云南昆明650600 [2]国家磷资源开发利用工程技术研究中心,云南昆明650600

出　　处：《磷肥与复肥》2021年第7期40-42,共3页Phosphate & Compound Fertilizer

基　　金：云南省磷化工节能与新材料重点实验室(2019);国家重点研发计划“中低品位磷矿非常规体系反应动力学特征研究”(2018YFC1900202-2);国家重点研发计划“渣-酸高值化协同化利用技术及工程示范”(2018YFC1900206-4)。

摘　　要：采用微波消解云南磷矿石,消解后通过微型化学实验快速测定磷矿石中的钙,用钙羧酸指示剂代替荧光指示剂,用三乙醇胺掩蔽铁、铝、锰离子的干扰,用糊精抑制镁离子和磷酸根离子的干扰。该方法试剂用量只为常规实验用量的1/3左右,测定结果与GB/T 1871.4-1995规定方法无显著差异,绝对误差在0.05~0.36 mg/kg,相对标准偏差为0.42%,加标回收率在86.7%~107.0%,准确度高,精密性好,方法节能易操作、分析成本低、环境污染小,易于推广。Yunnan phosphate rock is digested by microwave method,and then,calcium in phosphate rock is rapidly determined by microscale chemical experiment.Calcium carboxylic acid indicator is used to replace fluorescent indicator,triethanolamine is used to mask the interference of iron,aluminum and manganese ions,dextrin is used to inhibit the interference of magnesium ion and phosphate ion.The amount of reagent used in this method is only about 1/3 of that used in conventional experiments,and there is no significant difference between the results of this method and GB/T 1871.4-1995 method,the.absolute error is 0.05-0.36 mg/kg,the relative standard deviation is 0.42%,and the recovery rate is 86.7%-107.0%.The method has the advantages of high accuracy,good precision,energy saving,easy operation,low analysis cost,low environmental pollution and easy popularization.

关 键 词：微型化学实验 微波消解 云南磷矿石 钙离子测定 

分 类 号：TQ440.72[化学工程—化学肥料工业]