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1.
X射线荧光光谱法测定矿物中轻重稀土 总被引：5，自引：3，他引：5
without Octupole Reaction System and the ICP-MS with ORSSHI Yan-zhi1, WANG Ying-feng1, HE Run-ju其含量转换为轻、重稀土的总量。方法已用于实际样品测定,结果与化学法相符,10次测定的相对标准偏差分别为:CeO2的RSD为1.43%,Y2O3的RSD为1.11%。 相似文献
2.
碳酸盐岩中碳酸盐矿物稀土元素分析方法进展 总被引：1，自引：0，他引：1
碳酸盐岩中测定碳酸盐矿物的稀土元素主要有酸溶-ICP-MS和LA-ICP-MS方法.酸溶-ICP-MS方法用盐酸、硝酸溶解碳酸盐矿物,但也能溶解部分非碳酸盐矿物,而影响分析结果;用醋酸溶样可避免非碳酸盐矿物的干扰,但可能没有溶样完全,同样影响分析结果.LA-ICP-MS是应用激光对碳酸盐矿物进行原位剥蚀,将蒸发物导入ICP-MS进行分析,对不合粘土等的碳酸盐矿物最有效,由于激光束光斑较大,且碳酸盐岩中普遍含有微小的粘土矿物,可能也存在不确定性.总体而言,酸溶-ICP-MS和LA-ICP-MS获得的稀土元素页岩标准化配分模式及主要参数相似,均可用于沉积环境的示踪. 相似文献
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敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪 总被引：2，自引：2，他引：0
用电感耦合等离子体质谱法(ICP-MS)测定地质样品中的稀土及难熔元素,混合酸敞开酸溶法和碱熔融法是两种主要的溶样方法。但地质样品组分复杂,元素之间存在相互共生的现象,对于特殊元素、特殊样品用传统酸溶法会造成部分元素消解不完全,使测定结果不准确;而碱熔法的操作过程繁琐,且溶液盐度高,易产生基体干扰和堵塞仪器进样系统。本文改进了传统四酸和五酸体系,采用氢氟酸-硝酸-硫酸敞开酸溶体系,用国家一级标准物质制作标准曲线测定15种稀土元素,方法准确度(ΔlgC)为0.001～0.027。同时改进了偏硼酸锂碱熔法,样品用偏硼酸锂碱熔提取,加入氢氧化钠调节溶液至碱性条件,所测元素与偏硼酸锂共沉淀后过滤分离熔剂,再用硝酸复溶测定15种稀土元素及铌钽锆铪。两种溶样方法的测定值与认定值的相对误差为1.09%～9.30%。将混合酸敞开酸溶法测定稀土元素、偏硼酸锂碱熔法测定铌钽锆铪的结果与其他实验室密闭酸溶法相比,两组数据的相对偏差为0.13%～15.32%。本实验表明,混合酸敞开酸溶法适用于测定地质样品中的稀土元素,偏硼酸锂碱熔法不仅适用于测定地质样品中的稀土元素及铌钽锆铪,也适用于测定如古老高压变质岩石及铝含量高的样品中的铌钽锆铪。 相似文献
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Rare earth data for nine well-known geochemical reference samples were obtained using a rapid and efficient cation exchange chromatographic separation procedure. It involves the use of a mixed-acid eluent (HCI and HNO3) on a 15 x 1 cm column of Bio-Rad AG50–X8 (200–400 mesh) to remove matrix and many trace elements from rock solutions. The rare earth elements are removed from the column using 60 ml 7M HNO3. The pre-concentration procedure described is routinely used in this laboratory for the determination of the rare earth elements by mass spectrometry-isotope dilution, and has been satisfactorily used for their determination using inductively-coupled plasma-source atomic emission spectrometry. 相似文献
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Rare earth elements were determined by secondary ion mass spectrometry for 13 silicate rock samples, ranging from ultramafic-mafic to acidic compositions, 2 feldspar and 1 biotite separates. As a whole, the investigated samples are characterized by matrices and rare earth elements spectra covering most geological applications. The present data are compared with reference values. The advantage of using secondary ion mass spectrometry as a fundamental tool for trace element detection in bulk samples in the few ppm-ppb region is demonstrated. 相似文献
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F. W. E. STRELOW A. H. VICTOR C. H. S. W. WEINERT 《Geostandards and Geoanalytical Research》1978,2(1):49-55
Ion exchange chromatography is extremely well suited for the complete or partial separation of trace and ultra-trace elements from rooks and minerals. Selective methods are described for the separation of traces of lithium, beryllium, vanadium, uranium, strontium, barium, sodium, potassium and rare earth elements, and their determination in rook samples. The methods are especially useful for accurate standardization work. Some typical elution curves and results for the concentration of these trace elements in the six South African NIM-rock standards and some international standard rocks are presented. 相似文献
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通过对新疆彩霞山铅锌矿床不同类型岩石和矿石的稀土元素地球化学特征的研究,探讨了岩石和矿石中稀土元素地球化学行为。结果显示,矿床中稀土元素的分布是不均匀的。在稀土元素配分模式上,活化的白云石大理岩与矿石是相近的,具有显著的δEu正异常和弱的δCe负异常,表明成矿与白云石大理岩的关系密切。同时,根据稀土元素特征的变化,提出了矿床的形成可能与岩浆活动有关的研究思路。 相似文献
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提出了一种采用高温高压密闭溶样快速消解荧光粉晶体的前处理新方法。针对目前常用的稀土氧化物和稀土磷酸盐类、碱土金属铝酸盐类、碱土金属硅酸盐类四大类荧光粉,研究了消解时间、温度、消解溶剂种类和用量4个条件对样品消解程度的影响。采用电感耦合等离子体质谱法(ICP-MS)测定了最佳消解条件下消解的荧光粉中杂质元素Cu、Zn、Cd和Pb的含量。结果表明:稀土氧化物和稀土磷酸盐类荧光粉的最佳消解条件为 2 mL HCl溶剂中120℃下消解3 h;碱土金属铝酸盐类荧光粉的最佳消解条件为2 mL HCl溶剂中160℃下消解6 h;碱土金属硅酸盐类的最佳消解条件为2 mL HCl+0.5 mL HF溶剂中160℃下消解3 h。荧光粉中主要共存元素对所测杂质元素Cu、Zn、Cd和Pb的检测无干扰。该法线性范围宽、检出限低、灵敏度高,是荧光粉晶体中元素检测的较佳方法。 相似文献
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稀土稀有稀散元素现代仪器测试全新方法的建立 总被引：1，自引：0，他引：1
本文系统总结了自2011年以来在三稀矿产实验测试方面取得的新进展。重点介绍了离子相稀土单元素浸泡提取实验研究、稀土原产地Nd同位素与微量元素示踪技术研究、离子吸附型稀土样品野外现场快速定性定量手持X射线荧光(XRF)分析研究成果。结果表明,采用25%硫酸铵浸泡提取,电感耦合等离子体光、质谱(ICP- AES、ICP- MS)测定,可以清晰反映出各稀土元素的浸泡提取率;采用高精度多接收电感耦合等离子体质谱仪(MC- ICP- MS)进行稀土矿石中Nd143/Nd144同位素比值测定,其比值差异可以示踪不同稀土矿石产地;通过精确测试分析不同产地稀土精矿样品中的稀土和其他微量元素含量,并进行数据相关性分析和数据分类分析,通过Y、Be和Bi三种元素含量的比较,可以判断稀土精矿来源;野外现场快速分析,20分钟可完成1件样品测试,不仅可定性判断是否为离子吸附型稀土,同时可定量各离子相稀土单元素含量,与室内精确分析结果符合性良好,可为我国离子吸附型稀土矿床的找矿快速筛查提供技术支撑。 同时介绍了混合酸微波分解样品- 电感耦合等离子体光、质谱(ICP- AES、ICP- MS)同时测定钨矿石、钼矿石、铌钽矿石中的多种稀有稀散稀土元素含量的方案。该方案的特点在于采用了耐氢氟酸体系,尤其对高含量W、Nb、Ta样品更具优势,否则易产生水解,导致测定结果系统偏低。同时梳理总结了我国常见三稀矿石地质样品的特点,针对不同矿种、不同矿床样品类型与基体特点,以及所测试元素种类的不同,研究建立了专门针对“稀有、稀散、稀土元素”现代仪器分析的10个全新的配套方法及其相应的技术指标(准确度、精密度、检出限),可满足地质矿产实验室测试质量管理的规范要求,而且为我国三稀金属矿产资源的战略调查、国家重点研发计划“深地锂资源探测”和四川甲基卡等地找矿突破做出了贡献。 相似文献
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地质样品痕量元素分析中的基体校正,前人作过大量工作。但是对于主元素(主要指铁)吸收限长波侧的基体校正还未很好解决。本文利用相对吸收的概念,计算了主 相似文献
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Ernest S. GLADNEY David B. CURTIS Daniel R. PERRIN 《Geostandards and Geoanalytical Research》1985,9(1):25-30
The nuclear and instrumental parameters for the determination of rare earth elements (REE) via thermal neutron capture prompt gamme-ray spectrometry are examined. Gamma-ray sensitivity tables adjusted for elemental abundance are presented. Only Gd and Sm can be readily measured in rocks with normal REE concentrations. Data are reported for 37 international reference samples. 相似文献
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碱熔沉淀分离-电感耦合等离子体质谱法测定伴生重晶石稀土矿中的稀土元素 总被引：3，自引：3，他引：0
采用电感耦合等离子体质谱法(ICP-MS)测定伴生重晶石轻稀土矿中的稀土元素时,Ba以及轻稀土元素La、Ce、Pr、Nd、Sm等对中重稀土造成严重的质谱重叠干扰,因此在保证矿石完全消解的同时,若能选择合适的前处理方法实现目标元素与基体的有效分离,将有利于减少质谱干扰。本文采用过氧化钠-碳酸钠熔融分解伴生重晶石的稀土矿样品,熔融物用三乙醇胺溶液提取,将沉淀过滤去除硅、铁、锰、铝等大量基体元素,而稀土元素与钡、锶、钙等留存于沉淀中,沉淀经盐酸溶解后再用氨水进行二次沉淀,将稀土元素与伴生的高含量钡、锶、钙等元素分离,分离率超过96%,从而极大地降低了由钡的氧化物和氢氧化物对~(153)Eu等元素质量数的质谱干扰。轻稀土元素对中重稀土元素的干扰则通过测定高浓度的单元素标准溶液在m/z 138～175处的表观浓度来计算干扰校正系数,对干扰量进行扣除校正。该方法通过稀土矿石标准物质GBW07187、GBW07188验证,测定值与认定值的相对误差10%;应用于伴生重晶石稀土矿石实际样品分析,相对标准偏差(RSD,n=12)为0.5%～4.6%,证明了本方法可用于分析高钡矿石中的稀土元素。 相似文献
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关键金属元素分析测试技术方法应用进展 总被引：7，自引：5，他引：2
以稀有、稀散、稀土、铂族元素为主体的战略性关键金属矿产资源,在新材料、新能源和信息技术等新兴产业中发挥着越来越关键的作用。随着我国关键矿产资源地质调查的不断深入,关键金属元素以其赋存基体复杂、不同矿物含量差异大、化学性质不稳定等特点对分析测试技术提出了新的挑战。本文根据化学组成不同,对关键金属元素主要赋存基体进行了分类,主要分为硅酸盐、碳酸盐、硫酸盐、钨酸盐、磷酸盐、氧化物、硫化物、卤化物等。对于不同的基体岩石矿物,通常采用酸溶法(硝酸-氢氟酸组合、王水)或碱熔法等传统溶样方法进行化学消解。评述了当前关键金属元素测试常用的电子探针、电感耦合等离子体质谱、电感耦合等离子体发射光谱、X射线荧光光谱等仪器的特点及应用,总结了关键金属元素分析过程中出现的样品难溶解、回收率不完全、测试过程氧化物和同质异位素干扰、样品和标准基体不一致等常见问题,并提出了相应的解决方案。微区原位分析凭借其高效率、低成本、高空间分辨率的优势,以及野外现场分析凭借其简单快速、贴近野外工作的特点是关键金属元素测试技术发展的主要趋势。 相似文献
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高分辨电感耦合等离子体质谱法测定地质样品中稀土元素的氧化物干扰研究 总被引：3，自引：3，他引：0
电感耦合等离子体质谱(ICP-MS)用于测定稀土元素经常会引起M+、MO+、MOH+离子的质谱重叠干扰,其中制约分析准确度和精密度的主要因素是多原子离子干扰,尤其是轻稀土元素的氧化物和氢氧化物对重稀土元素的干扰,以及钡的7个天然同位素形成的氧化物和氢氧化物对轻稀土元素的干扰.本文采用高温高压密闭消解地质样品,高分辨电感耦合等离子体质谱法(ICP-MS)测定其中的痕量稀土元素,研究了低、中、高三种分辨率模式下氧化物的干扰情况,确定了最佳的测定同位素和合适的分辨率.分析结果表明,在低、中分辨率模式下,轻稀土元素Ce、Pr、Nd、Sm的氧化物和Ba的氧化物干扰明显,Gd元素的测定值严重偏离;在高分辨模式下,Ba氧化物对Eu的干扰以及大部分轻稀土元素氧化物对重稀土元素的干扰基本可以消除,无需进行校正,而只有157Gd受到141pr16O的干扰突出,当样品中Pr/Gd的浓度比值大于100时,Gd的测量值必须进行数学校正. 相似文献
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Previous laser ablation‐ICP‐MS bulk analyses have been confined to volcanic glasses and glass disks or powder pellets similar to those used for XRF analysis. This study proposes a method to determine twenty trace elements (fourteen rare earth elements, Sc, Y, Zr, Nb, Hf and Ta) by LA‐ICP‐MS directly from polished thick sections and rock slabs of six fine‐grained crystalline and aphanitic rocks (five volcanic rocks and one pelitic tillite). Laser scanning of eight to ten 20 mm long linear tracks using a spot size of 160 μm, with a total ablated area of 26–32 mm2, was performed. Quantification was carried out by (a) internal standardisation using Si and (b) without applying internal standardisation. In the latter method, external determination of one element in conventional LA‐ICP‐MS quantification is no longer needed. Although the fine‐grained rocks studied contained variable amounts of volatiles (up to 4%), this method gave results that agree within 10% relative with those obtained by internal standardisation using Si. Two USGS basalt glass reference materials (BCR‐2G and BHVO‐2G) were used for external calibration. The results and the associated trace element patterns and ratios of elemental pairs obtained from both methods of quantification showed good agreement with the results from solution nebulisation ICP‐MS within 20% (mostly within 10%) relative. Fine‐grained rocks are common and include volcanic, sedimentary and low‐grade metamorphic rocks (e.g., basalt, andesite, rhyolite, shale, mudstone, tillite, loess, pelite and slate) and their trace element contents and associated ratios are important geochemical tracers in studies focusing on the composition and evolution of the crust and mantle. Our method provides a simple and quantitative way to determine trace elements in fine‐grained rocks even with those displaying complex textures. 相似文献
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Major, trace and rare earth elements of phosphatic rocks around Sonrai block of Paleo-Mesoproterozoic age having phosphatic breccia, quartzite, shale, sandstone, limestone and ironstone, have been determined to evaluate their correlation, relationship with the phosphorus content, the nature of possible substitution of various elements and regional distribution pattern over the area. The study indicates that the number of elements is substituted in the apatite structures; few of them are associated with phosphate and carbonate minerals. The variable concentration of major, trace and rare earth elements in the phosphatic rocks has been influenced by various physico-chemical processes involved during weathering and leaching of the source rocks. The distribution of the major, trace and rare earth elements is controlled by the environmental variations in the sediment water interface. The majority of trace elements were mainly influenced by the principle adsorbents like the phosphate minerals in addition to clay, iron oxides and silicate minerals. The PAAS normalized REE patterns of Sonrai block of phosphorites are characterized by negative Ce anomalies and Positive Eu anomalies. It is inferred from the distribution and interrelationship of major, trace and rare earth elements that the deposition of phosphate minerals might have occurred in highly oxidizing to slightly reducing conditions in supratidal to intertidal continental margins and shallow marine environment. The deposition was controlled by marine upwelling leading to excess charge of phosphate in certain zones of phosphogenic basins, lithologic facies variations in restricted circulations of basinal waters and electrochemical factors such as negative Eh, pH and other factors, which influenced the deposition of phosphates. The replacement, precipitation in voids and fissures and diagenesis were also important mechanisms of phosphate generation in Sonrai basin. The main source for various elements may be the minerals of cratonic mass of Bundelkhand Granitic Complex, a basement of Bijawar Basin, which also provided land derived phosphorus through weathering of the terrestrial cover. 相似文献
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南京伏牛山铜矿脉状矽卡岩稀土元素地球化学特征 总被引：2，自引：0，他引：2
介绍了南京伏牛山铜矿与成矿有关的花岗闪长斑岩及脉状矽卡岩的稀土元素组成模式及稀土元素地球化学特征。并据两者的相似性及变异性特征,探讨了脉状矽卡岩的成因。 相似文献