X射线荧光光谱法测定生物样品中氯硫氮磷钾铜锌溴

研究了用微晶纤维素垫底镶边粉末压片制样-X射线荧光光谱测定生物样品中的Cl、S、N、P、K、Cu、Zn和Br的分析方法。重点研究了N的分析条件和校正方式,K、Cu和Zn的内标选定,测量次数对测定结果的影响。方法的检出限、精密度和准确度基本满足生物样品的分析要求。方法用于实际生物样品的测定,结果与化学法相符。     

Rapid analysis with energy-dispersive X-ray fluorescence spectrometry for bauxite investigation on the Mambilla Plateau, North Eastern Nigeria

Bauxite exploration involves routine analysis of a large number of samples for a wide range of elements. In Nigeria, though geological field exploration for bauxite started almost three decades ago very little has been achieved, mainly due to the non-availability of facilities for evaluating the dozens of suspected bauxite deposits scattered around the country. In this regard, a procedure for the rapid, accurate and precise measurement of a number of important elements in bauxite has been developed based on the newly acquired radioisotope based EDXRF spectrometer. Elements and oxides analyzed are Al₂O₃, SiO₂, TiO₂, Fe₂O₃, K₂O, Mn, Co, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb and Pb. The richest bauxite sample has concentrations of 48.08, 18.90, 1.26, 7.71 and 1.93 wt% for Al₂O₃, SiO₂, TiO₂, Fe₂O₃, and K₂O, respectively. The other values in ppm are Mn (3 0 2), Co (5 3 2), Cu (45), Zn (51), Ga (41), Rb (32), Sr (2 2 2), Y (32), Zr (8 4 9), Nb (89) and Pb (72). The measurement errors in terms of accuracy and precision are less than 5% and 10% and 5% and 15% for major and trace elements, respectively. Statistical correlation analysis carried out on the results shows the most significant relationships to be the negative correlations of alumina with silica, iron oxide and titanium. This is believed to be related to the processes of formation of bauxite, with the Si and Fe–Ti being removed as Al was being enriched.     

能量色散X射线荧光光谱仪现场快速测定多金属矿中17种组分

直接使用粉末样品,用Minipal 4便携式能量色散X射线荧光光谱仪测定多金属矿样品中的三氧化二铝、氧化镁、二氧化硅、氧化钾、氧化钙、三氧化二铁、硫、铜、锰、锌、铋、锑、铅、镓、银、砷、锡等17种组分,方法简便、快速,用多金属矿石国家一级标准物质验证,分析结果与标准值基本符合;精密度试验表明,各组分的相对标准偏差(RSD,n=12)均小于12%,能够满足矿山和野外现场快速测定的要求。     

X射线荧光光谱法测定土壤样品中碳氮硫氯等31种组分

利用新型的ZSX Primus Ⅱ型X射线荧光光谱仪采用粉末压片法直接测定土壤样品中的C、N、S、Cl等31种元素。各元素分析晶体为N采用RX45，C采用RX61，Na、Mg采用RX25，C1、S、P采用Ge，Si、Al采用PET，其余元素均采用LiF200。结果表明，方法的检出限、精密度和准确度对绝大多数元素而言，均可满足多目标地球化学调查样品分析的质量要求：     

X射线荧光光谱法同时测定土壤样品中碳氮等多元素

报道了采用粉末压片制样-X射线荧光光谱法测定土壤样品中C、N、S、Cl、Br、Hf、Mo、Sn、Se、Na、Mg、Al、Si、P、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Rb、Sr、Y、Zr、Nb、Ba、La、Ce、U、Th、Pb等38种元素的分析方法。着重研究了C和N的分析条件、存在问题和注意事项。所拟方法的检出限，精密度和准确度大多数满足覆盖区多目标地球化学调查样品分析质量的要求。     

X射线荧光光谱分析在我国铁矿石分析中的应用

系统介绍了20世纪90年代以来X射线荧光光谱分析（XRF）在我国铁矿石分析中的应用,包括粉末压片法和熔片法两种最基本的分析手段,主要内容集中在熔片—波长色散X射线荧光光谱分析法在我国铁矿石分析方面的测试技术,重点介绍了熔剂的类型、配比、熔片方法、熔融温度以及钴内标的使用,同时介绍了基体效应校正、谱线重叠校正等方面的内容。     

铜钴矿样品X荧光快速测定技术的初步研究

使用基于Si-PIN探测器和嵌入式计算机的便携式高能量分辨率X荧光(XRF)分析仪,对采自刚果(金)的铜钴矿样品进行测量。通过对实测数据的处理与分析,分含量段建立目标元素的工作曲线,同时求出相应的基体效应校正模型,并编制到仪器内置X荧光分析应用软件中。实现仪器根据实测多道微分谱线中相关元素的特征X射线计数率,自动切换工作曲线与基体效应修正模型,快速输出Cu和Co的含量的测定结果。通过与化学分析结果比较,快速测定结果精确度较高。     

The Study Internal Structure of the Annual Layers in Lake Sediments Using Synchrotron Radiation with X-ray Focusing Optics

正1 Introduction Annually laminated(varve)sedimentary deposits are considered as one of the most important archives,since they offer precise temporal information(years)in combination with high time resolutions.Bottom sediments of the lakes contain detailed geochemical information on     

波长色散X射线荧光光谱法测定铜精矿中铜铅锌硫镁砷

采用偏硼酸锂和四硼酸锂混合熔剂熔融法制样,波长色散X射线荧光光谱法测定铜精矿中铜、铅、锌、硫、镁、砷,考察了熔剂、玻璃化试剂和预氧化条件对制样的影响。采用理论α系数和经验系数相结合的方法校正元素间的效应。测定铜精矿试样各组分的相对标准偏差(RSD,n=12)均小于3%,结果与化学分析法吻合。     

高能偏振能量色散-X射线荧光光谱法测定PM10大气颗粒物的组成

为配合X射线衍射分析(XRD)方法对可吸入大气颗粒悬浮物(PM10)的结晶物相进行定性和定量分析的研究工作,本文应用高能偏振能量色散X射线荧光光谱(HE-P-EDXRF)对Whatman玻璃纤维滤膜采集的PM10颗粒物中主、次量元素进行定量分析,着重研究了空气滤膜空白值对测定PM10颗粒物中组成的影响。结果表明,当玻璃纤维滤膜空白值中元素的面密度大于0.1μg/cm2时,需使用玻璃纤维滤膜为载体的标准样品;元素的面密度小于0.1μg/cm2时,可用聚碳酸脂膜为载体的标准样品。对HE-P-EDXRF谱仪测定PM10颗粒物中痕量重元素进行探讨,将测定元素范围扩展到62个元素,其中Na、Mg、S、Y、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu的检岀限>0.1μg/cm2;Ca、Cr、Mn、Fe、Co、Ni、Cu、Zn、Br和Rb的检岀限<0.01μg/cm2;Cl、Al、Si、P、K、Sc、Ti、V、Ge、As、Br、Se、Sr、Zr、Mo、Pd、Rh、In、Nb、Ag、Cd、Te、Sb、Sn、Ba、Cs、La、Ce、Pr、Au、Pt、W、Tl、Pb、Bi、Th和U等元素检出限为0.1～0.01μg/cm2。     

一套基于X射线荧光测量的快速找矿方法

随着X荧光测量技术的发展,产生了土壤X荧光测量、岩石X荧光测量、钻孔X荧光测量和微区X荧光测量等多种多样的工作方法。笔者将土壤X荧光测量、浅钻X荧光测量和微区X荧光测量等快速获取异常信息手段应用于航磁异常查证,查明特克斯航磁异常主要由富含磁铁矿、褐铁矿的接触带安山岩所引起。对航磁异常查证,乃至找矿勘探工作的高效开展起到了良好的指导意义。     

熔融制片-X射线荧光光谱法测定锰矿样品中主次量元素

采用混合熔剂熔融制备样片,加入碘化铵粉末,有效地驱赶了锰矿熔融制样时产生的大量气泡,用Axios型X射线荧光光谱仪测定锰矿样品中的Mn、Fe、Si、Al、Ti、Ca、Mg、Na、K、P、Ba、Cu、Zn、Ni等元素的氧化物含量,用理论a系数校正基体效应,方法简便快捷。用国家一级锰矿石标准物质GBW 07266验证,结果与标准值相符;以锰矿石考察方法的精澈（RSD,n=12）,除CuO为10．05％,其余各组分均≤8％。     

A workflow for exploration sampling in regolith-dominated terranes using portable X-ray fluorescence: comparison with laboratory data and a case study

This paper presents and validates a workflow that provides for the rapid collection of reliable and robust portable X-ray fluorescence (pXRF) data in a regolith-dominated exploration setting. The analysis of regolith material by pXRF is challenging because of its variable Fe content (e.g. 0 to >70 wt%) that results in large matrix effects, which can be mitigated with appropriate standards. Here, we present a dataset from the Western Mount Isa Inlier, Queensland, Australia, comprising soil, lag, rock and rotary air blast (RAB) samples. In the soil dataset, comparison of the laboratory and pXRF datasets for Cu, Pb and Zn have R² > 0.9, and Cu and Zn fall within 2% of the laboratory data, while Pb is 77% less than the corresponding laboratory analyses. Iron, Al, K and Ca by pXRF perform reasonably well when compared with the laboratory data (R² = 0.59 for Al, R² > 0.9 for Fe, K and Ca, <25% variation from the laboratory data), while Mn, Rb and Sr have very good correlations (<8% variation) with R² > 0.94. Titanium, Zr, Ni, Cr and As have poorer comparisons. Overall, the RAB dataset shows similar trends with Cu overestimated by 17%, Zn underestimated by 4% and Pb overestimated by 69%; R² for all elements is >0.92. Since no suitable standards are available, the solid rock dataset was uncorrected; despite this limitation, the dataset shows good correlations with the laboratory data for many elements, and Cu is overestimated by 9.8% with an R² = 0.87. The poor analytical performance of Pb in all datasets is associated with erroneous Bi concentrations being reported by the pXRF unit. When high Fe and Pb amounts are present in a sample, erroneous Pb and Bi concentrations are reported, owing to a pile-up of the Fe K_α peak (6.405 keV) at ～12.8 keV, which is proximal to the Pb L_β (12.614 keV) and Bi L_β (13.023 keV) peaks. Despite the care that is required in validating data, by using pXRF there is substantial opportunity for dynamic exploration campaigns in regolith-dominated terranes with rapid turnaround times, additional elements that may not otherwise be analysed for and low analytical costs. Decisions to stop, continue or infill drill holes while the drill rig is present can be made in near-real time, and not after laboratory results are available and the drill rig has left the area.     

XEPOS型偏振能量色散X射线荧光光谱仪分析蒙古铁矿石

以熔融玻璃片和粉末压片制样,采用XEPOS型偏振能量色散X射线荧光光谱仪,建立了铁矿石中总铁、氧化钙、氧化镁、二氧化硅、三氧化二铝、硫、磷、铜等组分的快速分析方法。着重讨论硫、磷两元素测定的可行性和Lucas-Tooth、Price数学校正模型的适应性和改善方法的途径。     

High resolution X-ray fluorescence spectrometry for water analysis of metals in East China Sea

Within the last century, water pollution has become a major problem throughout the world. Aquatic systems are endangered by many different types of pollution but one of the most threatening is contamination by heavy metals, for example, Cd, etc. The presence of these metals is mainly due to industrial wastes or mining wastes being improperly treated and dumped into the water supply. The contamination may damage marine organisms or create changes in the aquatic environment. For these reasons, monitoring the concentrations of trace elements in rivers, coastal waters and open seawater is very important for environmental conservation. Like many countries in the world, China is facing the serious problem of water pollution in its aquatic system. Areas like the Yangtze River have been industrialized very quickly, and without proper waste control practices the pollution levels have increased with the economic growth. The Yangtze River covers thousands of square kilometers and crosses more than half of China before reaching the East China Sea.     

现场X射线荧光分析技术

本文从携带式X射线荧光仪器、现场分析技术和技术应用三方面论述了现场X射线荧光分析技术的进展.从X射线激发源、X射线探测器和电子线路单元等角度,将携带式X射线荧光仪划分为四代,即以放射性同位源为激发源、以NaI(Tl)闪烁计数器为X射线探测器为技术特征的第一代仪器;以放射性同位素源和正比计数器为技术特征的第二代仪器;以放射性同位素、电制冷半导体探测器和以嵌入式微处理器为控制核心的多道脉冲幅度分析器为技术特征的第三代仪器;以低功率微型X射线发生器为激发源、电制冷半导体探测器和全数字化X射线能谱采集器为技术特征的第四代仪器.在现场分析技术方法方面,论述了X射线仪器谱解析技术、基体效应校正技术和现场原位分析中不平度效应、湿度效应、荧光颗粒不均匀效应校正技术进展.介绍了现场X射线荧光分析技术在地质矿产普查、环境污染调查、文物现场鉴定和合金分析等领域的应用进展.指出了目前国产携带式X射线荧光仪处于第三代和第四代仪器水平之间,低功率微型X射线发生器和电制冷半导体探测器还依赖于进口,全数字X射线能谱采集器还有待商品化;现场多元素分析的准确度和方法检出限都有待进一步改善;便携式仪器的应用领域有待拓宽.     

The sum of component concentrations as a quality indicator in X-ray electron probe microanalysis of minerals

X-ray electron probe microanalysis is a complete mineral analysis technique. Therefore, the sum of obtained concentrations can be used as an indicator of the quality of analysis. There are two kinds of errors of the sum of concentrations. The first is related to the deviation of the sum from the basic value and can be called a difference error. The second is the scattering of results around the mean value and can be called an averaging error. The difference error characterizes the reproducibility of the measurements and equals 0.41% at the current precision level. The averaging error characterizes the repeatability of the measurements and equals 0.23%. The difference error can be used as a quality indicator directly during analysis, while the averaging error can be used after analysis of a batch of specimens. According to the modified three-sigma rule, the acceptable sum values of separate analyses are in the range 98.8-100.8%. This range is obviously valid only for an ideal model with a basic sum value of 100%. In real analyses, the basic value deviates from 100% because of the presence of elements which are not detected in the analysis and elements with a variable valence. According to the three-sigma rule, the acceptable scattering of the sum of concentrations around the average value is ± 0.7%.     

X射线荧光光谱三十年

X射线荧光光谱分析在20世纪80年代初已是一种成熟的分析方法,是实验室、现场分析主、次量和痕量元素的首选方法之一,在无损分析和原位分析中具有不可替代的地位。文章评述了三十年来X射线荧光光谱分析的进展历程、波长色散X射线荧光光谱仪(WDXRF)、能量色散X射线荧光光谱仪(EDXRF)和现场与原位分析用X射线荧光光谱仪发展过程及显示的特色。介绍了在X射线的全反射和偏振性质基础上相继推出的偏振、微束、全反射等全新的X射线荧光光谱仪及其在众多领域的应用。回顾了基体校正发展历程和以Sherman方程为基础的基本参数法和理论影系数法在定量分析中的应用,并对学术界有关基体校正的物理意义的争论、Sherman方程的局限性以及如何提高基本参数法在常规定量分析和半定量分析结果的准确度的途径进行了探讨。总结了化学计量学与数据处理方法在XRF中的应用研究及进展,指出人工神经网络方法与基本参数法相结合的算法,对于改善基体校正的准确度和稳定性开创了一条新的途径。     

关于研制X射线荧光微分析标准物质的探讨

将经过高温处理的土壤样品进行反复研磨后，用于X射线荧光微分析标准物质的研制，当99％的粉末粒径≤30μm时，用仪器中子活化和同步辐射X射线荧光进行元素分布均匀性和最少取样量分析，结果表明24个元素的最少取样量可以降到约1mg。     

电子探针和X射线衍射仪测定新疆祖母绿宝石

新疆首次发现了质量上佳的祖母绿宝石(绿柱石),受到了国内外学者的高度关注。文章对新疆祖母绿矿物晶体进行电子探针显微分析(EPMA)和X射线衍射(XRD)测试,获得EPMA成分分析结果及XRD测试晶胞参数、衍射图谱。结果表明,新疆祖母绿化学成分中Cr2O3含量较高,一般在0.21%~0.54%;典型样品晶胞参数测定结果为a0=0.923 3 nm,c0=0.920 6 nm,Z=2,主要粉晶谱线为2.871(100)、3.257(100)、7.996(100)。