Determination of Ti, K, Sm and Gd Values in Geological Survey of Japan Reference Materials by Prompt Gamma Neutron Activation Analysis

Prompt gamma neutron activation analysis was applied to the determination of the titanium, potassium, samarium and gadolinium contents of nine Geological Survey of Japan (GSJ) reference materials (JB-1, 1a, 2, 3; JA-1, 2, 3; JR-1, 2). Firstly, the values in JB-1 were determined by the standard addition method: pressed powder disks of JB-1 were used for neutron irradiation and gamma-ray measurements, after known quantities of standard reagents had been added. Secondly, the contents of eight other reference materials were determined by comparison methods using JB-1 as the comparative standard. The precision of analyses were obtained by replicate determinations on these samples. The relative standard deviation was generally less than 5%. For most samples, analysed values agreed well (< 5%) with the recommended values.     

中子活化分析大洋多金属结核标准物质的研究

采用中子活化分析相对＿Ｋ０法对研制的两个深海多金属结核标准物质ＧＳＰＮ＿２和ＧＳＰＮ＿３中的２６种主量和微量元素进行了定值测定,所得结果与初定值符合;对中子辐照自屏蔽效应进行了实验测定和理论计算,结果显示了很好的一致性;同时还对这两个多金属结核标准物中的Ａｓ、Ｂａ、Ｃｅ、Ｃｏ、Ｅｕ、Ｆｅ、Ｌａ、Ｌｕ、Ｍｎ、Ｍｏ、Ｎａ、Ｓｂ、Ｓｍ、Ｓｃ、Ｔｈ、Ｙｂ和Ｚｎ的取样量与取样误差关系进行了研究。结果表明,在ＧＳＰＮ＿２和ＧＳＰＮ＿３试样中分别有８种和１１种元素,在取样量１０ｍｇ时其取样误差小于１％。     

MIBK负载泡塑吸附-中子活化法在金标样定值中的应用

试样经焙烧、王水分解后,在8％的王水介质中,MIBK负载泡塑吸附[AuCl_4]~-。灰化吸附泡塑或硫脲溶液解脱,用中子活化法测定Au。取10g样品,可测定0.000x～xxμg/g的Au。用于金标样的定值,具有良好的精密度和准确度。     

地质样品中超痕量铂族元素的中子活化分析

文章概述了中子活化分析的基本原理和地质样品中超痕量铂族元素的中子活化分析方法。其中除介绍了样品的制备方法、照射和测量条件之外，还对地质样品中铂族元素放射化学分离方法进行了说细的讨论和评述。引用文献２４篇。     

铁基样品中锰的中子活化法测定

采用热中子与超热中子照射相结合的中子活化法测定了铁高含量样品中锰的含量。实验测定和理论计算了铁对锰的干扰系数,两者符合较好。对几个标准物质的分析结果与推荐值相符。该方法适用于ｍＦｅ／ｍＭｎ小于２×１０５的样品中锰含量的测定     

Determination of Chlorine in Nine Rock Reference Materials by Isotope Dilution Mass Spectrometry

A procedure for the determination of chlorine by the isotope dilution technique (ID) using negative thermal ionisation mass spectrometry (N-TIMS) is described. Silicate samples of about 10 mg were spiked and decomposed with hydrofluoric acid, and chlorine was isolated by precipitation of silver chloride after neutralisation with Ca(OH)₂. The ammonical solution of AgCl was then subjected to N-TIMS. Replicate analyses of rock reference materials, typically of JB-1 and JR-1, demonstrated the high quality of the analyses (precision for Cl was ± 1-2%). We present here the most precise data sets of chlorine concentrations in nine igneous rock reference materials, three basalts (JB-1, JB-2, JB-3), two andesites (JA-3, AGV-1), two rhyolites (JR-1, JR-2) and two granodiorites (JG-3, GSP-1). The chlorine concentrations found ranged from 152 μg g-1 in AGV-1 to 1008 μg g^-1 in JR-1. Our results presented here are partly (but not completely) in agreement with recommended values, where they are available. The N-TIMS ID technique can thus be used as a means of determining low chlorine contents in silicate materials to high precision.     

大洋多金属结核和深海沉积物标准物质中铂族元素的中子活化分析

采用镍锍试金预富集 中子活化分析方法,测定了大洋多金属结核标准物质ＧＳＰＮ ２、ＧＳＰＮ ３和深海沉积物标准物质ＧＳＭＳ ２、ＧＳＭＳ ３中的铂族元素;根据大洋样品成分特征,对常规的镍锍试金配方和熔炼条件作了改善;计算了活化分析中的铂族元素干扰核反应,校正了Ａｕ对Ｐｔ的二级干扰;选用羰基化镍粉配料,降低了铂族元素空白值。用国家一级标准物质ＧＢＷ０７１０２作了对照分析,结果与标准值相符。     

Ion Chromatographic Determination of Fluorine and Chlorine in Silicate Rocks Following Alkaline Fusion

A simple and accurate method to determine fluorine and chlorine contents in small amounts (∼ 30 mg) in rock has been developed using ion chromatography after extraction by alkaline fusion. Powdered sample was mixed with sodium carbonate and zinc oxide at a mass ratio of 1:3:1, and was fused in an electric furnace at 900 °C for 30-40 minutes. An aqueous solution obtained by dissolving the fused silicate rock was diluted to the appropriate concentration of sodium carbonate (< ∼ 24 mmol l^-1) to minimise the tailing effect on F^- during ion chromatography caused by the large amount of carbonate species originating from the flux. Fluorine and chlorine contents were then determined by a standard additions method. Based on the relative standard deviation of the backgrounds, detection limits of both fluorine and chlorine were ∼ 4 μg g^-1, when 30 mg test portions were fused and diluted by a factor of 1200. We also report new fluorine and chlorine contents in nine GSJ (Geological Survey of Japan) reference materials, including peridotite (JP-1), granite (JG-1a), basalts (JB-1b, 2 and 3), andesites (JA-1 and 2) and rhyolites (JR-1 and 2). Fluorine and chlorine contents in the reference materials in this study were consistent with previously reported values. Reproducibilities were < 10 % for samples with F and Cl concentrations of > 20 μg g-1 and < 20 % with F and Cl < 20 μg g^-1.     

Instrumental Neutron Activation Analysis of Nine New Reference Materials from the Geological Survey of Japan

Nine reference materials, recently distributed by the Geological Survey of Japan (JA-1, JB-la, JB-2, JB-3, JG-la, JGb-1, JP-1, JR-1 and JR-2) have been analysed by instrumental neutron activation analysis using well proven experimental techniques. Results for the twenty elements determined (selected rare earth elements, Fe, Ba, Co, Cr, Cs, Hf, Rb, Sc, Ta, Th and U) are assessed for accuracy and precision and show good agreement with previously published data.     

中子活化分析方法测量金的活动态

探讨了金的活动态各相态（水浸出态，粘土吸附态，有机链合态，铁锰氧化物态）提取操作和中子活化分析测定的条件。列出了部分样品中金活动态分析结果和其测定精度范围，各相态的空白值和RSD（n=5)分别为：水浸出态0.030ng/g,4.5%-26.0%；粘土吸附态0.05ng/g,11.6%-25.2%；有机链合态0.06ng/g,3.7%-26.8%；铁锰氧化物态0.05ng/g,5.9%－31.6％。     

Boron Determination in Twenty One Silicate Rock Reference Materials by Isotope Dilution ICP-MS

The concentration of boron was determined in twenty one geochemical reference materials (silicate rocks) by isotope dilution inductively coupled plasma-mass spectrometry. Boron was extracted from the rocks using HF digestion, suppressing boron volatilisation through boron-mannitol complexation. Sample solutions, in a diluted HCl matrix, were analysed by ICP-MS without any separation of boron from the matrix elements. The results obtained were in agreement with the literature data and indicate that using the described procedure, trace amounts of boron can be very easily determined in complex matrices with rapidity and precision. With the instrumentation and reagents used in this study, this procedure can be used for the determination of 0.5 μg g⁻¹ boron in a 15 0 mg silicate rock sample. Replicate analyses of the twenty one geochemical reference materials (GRM), ranging in boron concentration from 1.35 to 15 7 μg g⁻¹, yielded precisions (relative standard deviation) varying between 0.9 and 9.8%.     

The Preparation and Characterisation of Two New Geological Survey of Japan Geochemical Reference Materials: Copper ore JCu-1 and Zinc ore JZn-1

Two new geochemical reference materials, copper ore JCu-1 and zinc ore JZn-1 have been prepared by the Geological Survey of Japan (GSJ) for the determination of major and minor elements and isotopic compositions. JCu-1 is a sample of Cu-bearing sulfide ore typical of the Kamaishi mine in Iwate Prefecture, Japan, and is composed mainly of hedenbergite, chalcopyrite, quartz and calcite. Pyrrhotite, magnetite and actinolitic amphibole were also commonly found. The Zn-rich ore, JZn-1 is a crude ore from the Kamioka Pb-Zn mine in Gifu Prefecture, Japan. The sample consists of hedenbergite, quartz, calcite, sphalerite and epidote as main crystalline phase. Homogeneity test results showed that all studied constituents including ore elements such as Cu, Pb and Zn can be considered to be homogeneously distributed. Provisional collaborative analyses were carried out in ten laboratories, and the data were evaluated using a robust statistical method using z-scores. Recommended values for a number of major elements including TiO₂, Al₂O₃, MnO, MgO, CaO, Na₂O, K₂O, Fe (total), Zn, Cu and Pb were established. In addition, information values for eighteen major, minor and trace elements are presented to support future collaborative analyses.     

Accurate Determination of Chlorine,Bromine and Iodine in U.S. Geological Survey Geochemical Reference Materials by Radiochemical Neutron Activation Analysis

Trace amounts of three halogens (chlorine, bromine and iodine) in seventeen U.S. Geological Survey (USGS) geochemical reference materials were determined by radiochemical neutron activation analysis (RNAA). The materials analysed were AGV‐2 (andesite), BCR‐2, BHVO‐2 and BIR‐1a (basalts), CLB‐1 (coal), COQ‐1 (carbonatite), DGPM‐1 (disseminated gold ore), DNC‐1a (dolerite), DTS‐2b (dunite), GSP‐2 (granodiorite), Nod‐A‐1 and Nod‐P‐1 (manganese nodules), QLO‐1a (quartz latite), SBC‐1 (marine shale), SDC‐1 (mica schist), SGR‐1b (shale rock) and W‐2a (diabase). The chlorine, bromine and iodine contents were determined to be 5.64 mg kg^?1 (BIR‐1a) to 4410 mg kg^?1 (Nod‐A‐1), 0.039 mg kg^?1 (BIR‐1a) to 52.1 mg kg^?1 (CLB‐1), and 0.041 mg kg^?1 (BIR‐1a) to 599 mg kg^?1 (CLB‐1), respectively. The RNAA data of the three halogens were compared with the corresponding data in the literature.     

Determination of Trace Elements in Selected Geological Reference Materials by Instrumental Neutron Activation Analysis

Data are presented for eight rare earth elements and ten other elements in 22 reference samples recently distributed by the University of Liege (Belgian sedimentary rock reference samples), the Geological and Mining Service (Suriname), the Geological Survey of Japan and the Venezuelan laterite. Determinations were made using a well characterised, high precision, neutron activation analysis technique.     

微堆中子活化分析测定碳酸盐岩中痕量元素

研究了微堆中子活化分析测定碳酸盐岩中痕量元素的测量条件和测定中的影响因素。一般样品采用仪器中子活化分析直接测定;痕量元素含量太低的样品,用1mol/LHCl浸取试样,在pH8的NH4Cl NH3·H2O缓冲溶液中用1 (2 吡啶偶氮) 2 萘酚沉淀富集痕量元素,去除大量的钙、镁基体,可降低方法测定下限,检出限为0.001～20μg/g。方法经国家碳酸盐岩标准物质GBW07108和GBW07114分析验证,结果与标准值相符,RSD(n=11)<12%。     

中子活化法测定铝材料中杂质元素

测定了用作反应堆的铝材料中Ｆｅ,Ｃｕ,Ｚｎ,Ｌａ,Ｓｍ,Ｍｏ,Ｈｆ等２３种杂质元素含量。对于Ｔｉ和Ｎｉ采用超热中子活化法,其它元素采用热中子活化法。实验测得了裂变系数,用于扣除Ｕ对Ｃｅ,Ｎｄ,Ｚｒ,Ｌａ,Ｓｍ等元素的干扰,计算了铝材中各杂质元素的探测极限,该方法精密度,对几个标准参考物质的分析结果与推荐值相符。     

库伦滴定法测定岩矿试样中氯

本文提出用电生Ag~ 库伦滴定岩矿样品中痕量氯的方法。经对电解液组成、不同电解电流下的电流效率、干扰元素的分离等进行了实验研究,确定了最佳分析条件。实验结果表明:当测定氯量≥100μg时,回收率达99.5～99.9％,相对标准偏差0.33～0.03％;测定氯量≥10μg,回收率为98.6～98.9％;相对标准偏差2.5～0.58%;方法准确,重现性好,操作简便。用岩石和土壤一级标准物质检验及参加建材一级标准物质协作定值,结果满意。     

Determination of Bromine and Iodine in Twenty-three Geochemical Reference Materials by ICP-MS

Trace amounts (from nanogram to microgram levels) of bromine and iodine were determined by inductively coupled plasma-mass spectrometry (ICP-MS) in twenty-three geochemical reference materials issued by the GSJ, USGS, IAEA etc. The pyrohydrolysis technique was used to separate bromine and iodine from samples analysed in the form of powder. The accuracy and precision of the experimental values were assessed by the comparative analysis of well established reference materials such as USGS AGV-1, BCR-1 and IGGE GBW07312. The measured values agreed well with reported values within a 10% error range. We also report reliable new data for these elements in these geochemical reference materials.     

Determination of Iodine in Thirty Two International Geochemical Reference Materials

Thirty two geochemical reference samples have been analysed for their iodine contents by a pyrohydrolysis extraction technique, followed by colourimetry. In spite of the existence of few reported values for iodine, limiting comparison with results from this study, the four available "reference" values show good agreement with the work reported here.