摘要
以镍、钴为主的多金属矿分析,因基体复杂、缺乏标样等因素,研究报道相对较少。实验建立了以熔融法制样,X射线荧光光谱法(XRF)测定以镍、钴为主的多金属矿中主量组分(SiO_2、Al_2O_3、TFe(以Fe_2O_3形式表示)、CaO、MgO、K_2O、Na_2O、TiO_2、P_2O_5、MnO)及矿化元素(Ni、Co)的方法。重点研究了熔融制样熔剂、熔剂和样品稀释比、氧化剂、预氧化温度和时间、熔融温度和时间、基体效应校正等影响因素,并进行了方法指标测试。研究表明,采用Li2B4O7-LiBO_2-LiF(m∶m∶m=4.5∶1∶0.4)混合熔剂,以LiNO_3为氧化剂,熔剂和样品20∶1的稀释比,在650℃预氧化4min,1 050℃熔融9min,能制得较好的熔片。对样品进行精密度考察,各组分测定结果的相对标准偏差(RSD)为0.49%~6.2%,按照实验方法对镍钴矿石标准物质进行分析,测定值与认定值一致。
There are relatively few reports on the analysis of nickel and cobalt polymetallic ores due to the complexity of matrix and lack of standard sample.Nickel and cobalt polymetallic ore sample was prepared by fusion sample preparation method.The contents of main components(SiO 2,Al 2O 3,TFe(expressed in the form of Fe 2O 3),CaO,MgO,K 2O,Na 2O,TiO 2,P 2O 5 and MnO)and mineralization elements(Ni and Co)were determined by X-ray fluorescence spectrometry(XRF).Several influencing factors were studied,including the flux for fusion sample preparation,the dilution ratio between flux and sample,the oxidizer,the pre-oxidation temperature and time,fusion temperature and time,and the correction of matrix effect.Moreover,the index test of method was conducted.It was found that the sample could be well prepared under the following conditions:the Li 2B 4O 7-LiBO 2-LiF(m∶m∶m=4.5∶1∶0.4)was used as mixed flux;the LiNO 3 was selected as oxidizer;the dilution ratio between flux and sample was 20∶1;the pre-oxidation temperature and time was 650℃and 4 min;the fusion temperature and time was 1 050℃and 9 min,respectively.The precision of sample was investigated.The relative standard deviations(RSD)of determination results of each component were between 0.49%and 6.2%.The standard substance of nickel-cobalt ore was determined according to the experimental method,and the found results were consistent with the certified values.
作者
曾美云
邹棣华
李小丹
杨小丽
ZENG Mei-yun;ZOU Di-hua;LI Xiao-dan;YANG Xiao-li(Wuhan Center of Geological Survey,China Geological Survey,Wuhan 430205,China)
出处
《冶金分析》
CAS
CSCD
北大核心
2018年第4期51-56,共6页
Metallurgical Analysis
基金
中国地质调查局地质调查项目(121201009000150002)
关键词
X射线荧光光谱法
镍
钴
多金属矿
熔融制样
主次组分
X-ray fluorescence spectrometry
nickel
cobalt
polymetallic ore
fusion sample preparation
major and minor component
