ICP—AES法分析辉锑矿

本文针对辉锑矿成分复杂、主元素Sb易水解、部分元素易挥发,酸不溶元素的存在以及元素之间的干扰等问题,拟定了酸溶和碱熔分解试样的分析流程。在酸溶系统中结合TBP萃淋树脂和巯基棉分离富集分组,ICP-AES法测定Fe、Ca、Mg、Cu、Mn、Pb、Zn、Co、Ni、Au、Ag、In、Tl、Cd、Bi、Ga、Mo、Se、Te、As等20个元素。碱熔系统不分离主元素,用校正因素校正元素间光谱干扰并采用内标法ICP-AES测定Al、Ti、V、Ba、Sr、Sn、Sc、Cr、Be、Si和Sb等11个元素。试样验证表明,方法可行。     

Extraction of Lithium from Salt Lake Brine using N523-TBP Mixture System

In this work,problems encountered by tri-butyl phosphate( TBP) in the industrialization of lithium extraction from salt lake brine were discussed in detail. The behavior of N,N-bi-( 2-ethylhexyl) acetamide( N523) during lithium extraction was investigated,and its disadvantages were analyzed in the view of practical application. An N523-TBP mixture extraction system was proposed to alleviate or avoid the defects that N523 and TBP met when they were used separately. The optimal composition of this mixture extraction system was determined to be 20% N523-30% TBP-50% kerosene.The effects of brine acidity,Fe/Li molarity ratio,phase ratio and chloride ion concentration on lithium extraction efficiency were discussed. The operation conditions in single-stage extraction were optimized as brine acidity = 0. 05 mol/L,Fe/Li molarity ratio = 1. 3,and phase ratio = 2. The high concentration of chloride ions in brine was beneficial for the extraction of lithium. The structure of the extracted complex was proposed as( LiFeCl_4·n N523·m TBP)·( 2-n) N523·( 2-m) TBP( m + n = 2) by chemical analysis and slope-fitting methods. The extraction thermodynamic functions were calculated preliminarily,and the results suggested that the extraction process was an exothermic( ΔH 0) and spontaneous( ΔG 0) reaction,and the degree of disorder increased( ΔS 0) during the extraction process. This work will give some guidance to the lithium industry of Qinghai in both the fundamental theory and practical application.     

TBP萃淋树脂微色谱柱分离富集钼的研究及应用

研究了ＴＢＰ萃淋树脂微色谱柱分离富集微量钼的柱性能,确定了分离钼的最佳条件。在减压条件下,运用零空床体积洗脱技术,以３ｍｏｌ／ＬＨＣｌ为上柱介质,０．５ｍｏｌ／ＬＨＣｌ洗脱,可使钼（ＶＩ）与钨（Ⅵ）、铁（Ⅲ）、锡（Ⅳ）等干扰离子快速分离,采用邻氯苯基荧光酮胶束增溶光度法,测定矿石中微量钼,结果满意。     

Extraction of Lithium from Salt Lake Brine using N523-TBP Mixture System

In this work, problems encountered by tri-butyl phosphate (TBP) in the industrialization of lithium extraction from salt lake brine were discussed in detail. The lithium extraction behavior of N, N-bi-(2-ethylhexyl) acetamide (N523) was investigated, and its defect was analyzed in the view of practical application. The N523-TBP mixture extraction system was proposed to alleviate or avoid the defects that N523 and TBP met when they were used severally. The composition of this mixture extraction system was determined as 20%N523-30%TBP-50% kerosene. The effects of brine acidity, Fe/Li molarity ratio, phase ratio and chloride ion concentration on lithium extraction efficiency were discussed respectively. The operation conditions in single stage extraction were optimized as brine acidity=0.05 mol/L, Fe/Li molarity ratio=1.3 and phase ratio=2. The high concentration of chloride ion in brine was benefit for extraction of lithium. The structure of extracted complex was proposed as (LiFeCl4·nN523·mTBP)·(2-n)N523·(2-m)TBP (m+n=2) by chemical analysis and slope fitting methods. The extraction thermodynamic functions were calculated preliminarily, and the results suggested that the extraction process was an exothermic (ΔH<0) and spontaneous (ΔG<0) reaction, and the degree of disorder increased (ΔS>0) during the extraction process. This work will give some guidance to the lithium industry of Qinghai in both fundamental theory and practical application.     

钪（Ⅲ）的反相萃取柱色层新体系研究及应用

本文设计出钪（Ⅲ）的反相萃取柱色层新体系并加以应用。该新体系以聚四氟乙烯－７０１为载体，磷酸三丁酯（ＴＢＰ）为固定相，在１０ｍｏｌ·Ｌ￣（－１）盐酸中定量萃取层析钪（Ⅲ），用１０ｍｏｌ·Ｌ（－１）盐酸淋洗杂质元素，４ｍｏｌ·Ｌ（－１）盐酸解脱钪，经二甲酚橙光度法测定其回收率可达１００％。本法简便快速，选择性高，分离效果好，能用于岩石、矿物等物料中钪的定量分离、富集及测定。     

磷酸三丁酯减压微色谱柱分离锡的研究和应用

研究了磷酸三丁酯（ＴＢＰ）减压微色谱柱分离富集Ｓｎ的条件和性能。选定３ｍｍ×７０ｍｍ的微色谱柱，树脂粒度１２０～１４０目，测得静态吸附容量为２７ｍｇ／ｇ，吸附反应速率常数为３６８×１０－３；减压条件下，在１ｍｏｌ／ＬＨＣｌ介质中Ｓｎ被萃取在ＴＢＰ微色谱柱上，用２ｍＬ２ｍｏｌ／ＬＨ２ＳＯ４洗脱后即可用邻氯苯基荧光酮Ｔｗｅｅｎ２０分光光度法测定Ｓｎ含量。经标准样品验证，分离效果好，适于矿样中微量Ｓｎ测定     

磷酸三丁酯三苯基膦醋酸纤维富集-等离子体发射光谱法测定地质样品中的痕量金银

地质样品经王水分解后,在一定浓度的王水和盐酸介质中,以磷酸三丁酯三苯基膦醋酸纤维富集金银,用20g/L硫脲溶液解脱,采用等离子体发射光谱法测定,金、银的回收率为98%~101%,方法检出限金为0.001μg/g,银为0.001μg/g。     

磷酸三丁酯醋酸纤维富集－火焰原子吸收法测定地质样品中痕量金

在５％～４０％王水介质中，用磷酸三丁酯（ＴＢＰ）－醋酸纤维吸附富集Ａｕ，被吸附的Ａｕ用热硫脲溶液解脱，火焰原子吸收法测定。Ａｕ的回收率大于９８％，方法简便快速，经地质标样分析验证结果可靠。     

N523-TBP混合萃取体系从盐湖卤水中萃取锂的机理研究

研究了N523(N,N-二乙基己基乙酰胺)-TBP(磷酸三丁酯)混合萃取体系从盐湖卤水中萃取锂的共萃取效应、盐析效应及共存离子影响。FeCl_3、CoCl_2、NiCl_2、CuCl_2、ZnCl_2等过渡金属氯化物盐对锂的共萃取效应研究表明,FeCl_3是最佳的共萃剂,Fe/Li摩尔比为1.3时萃取效果最优。卤水中KCl、CaCl_2、NaCl、MgCl_2、Al Cl3的盐析效应研究表明,MgCl_2是萃取锂天然的最佳盐析剂。卤水中Na~+、K~+、Ca~(2+)等共存离子对锂萃取效果的影响研究表明,锂与共存离子的分离因数顺序为βLiMgβLiKβLiNaβLiCa。N523-TBP混合萃取体系特别适合从高镁卤水中萃取锂,但不适于从含钙较高的卤水中萃取锂。     

三种体系萃取分离-液闪测定海水中234Th的比较研究

本文对TOA萃取剂萃取钍适宜的操作条件及萃取溶剂进行了试验,提出了TOA/苯萃取234Th的最佳条件: 在 1cm3含 234Th的 6mol/dm3 HNO3 溶液中,用体积比为 0. 5的TOA/苯溶液 2cm3 萃取,然后用 2cm3 1. 0mol/dm3 H2SO4反萃取,最高萃取率达 94%.对TOA/苯、TBP/煤油和TTA/苯这 3种萃取体系的萃取效率及其影响因素、萃取机理、成本等做了比较,认为 3种体系各有利弊,但均可有效地应用于相关的海洋学研究中.