熔片制样-X射线荧光光谱法测定煤灰样品中主次量组分

采用混合熔剂熔融制备样片,用AxiosX射线荧光光谱仪测定煤灰样品中二氧化硅、氧化铝、氧化铁、氧化镁、氧化钙、氧化钠、氧化钾、二氧化钛、二氧化锰、五氧化二磷和三氧化硫等11种组分。重点研究了熔样比、熔样温度和标准样品的制备,解决了分析硫的难题。用基本参数法校正基体效应,分析方法的精密度(RSD,n=10)各组分均小于3%。用煤灰国家一级标准物质验证,结果与标准值相符。     

原子荧光光谱法测定土壤和水系沉积物国家标准物质中砷

用王水浸提法和硝酸-高氯酸-氢氟酸混合酸消解法处理样品,原子荧光光度光谱法测定土壤和水系沉积物国家标准物质样品中的砷。方法检出限为0.02 mg/kg。两种前处理方法砷的测定值与标准值相符,均可以满足土壤和水系沉积物样品中砷含量的测定要求。单纯测定样品中砷含量时,王水浸提法更好;如果在测定砷同时还要测定其他元素,则可以选用混合酸消解法。     

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。     

Li2B4O7熔融玻璃-激光剥蚀等离子体质谱法测定水系沉积物国家标准定值样品中微量元素

建立了激光剥蚀等离子体质谱法直接测定Li2B4O7熔融玻璃中微量元素的分析方法。详细讨论了内标元素的选择及Li2B4O7熔融玻璃的均一性、背景空白对分析测定的影响。以Li2B4O7熔融玻璃中低同位素丰度的6Li作内标，水系沉积物国家标准参考物质熔融玻璃建立多元素标准校正曲线，用于标准参考物质及水系沉积物定值样品的分析，测定值与标准值或溶液雾化等离子体质谱结果比较，具有较好的一致性。     

The Preparation and Certification of Two Samples of Chromium Ore

The preparation of two chromium ores as reference materials is described and the procedures used in the measurement of the homogeneity of the samples are outlined. Statistical analysis of the data submitted by 32 laboratories that resulted in the certification of the samples is presented. Certified values have been assigned for 11 constituents in the one sample and for 10 in the other sample. Provisional values have been assigned for FeO in both samples and CaO in one of the samples.     

Establishment of research methodology and workflow for the occurrence state of the critical metal cobalt in ore: A case study of the Longqiao cobalt -rich skarn iron deposit in the Luzhong BasinSCIEI北大核心CSCD

关键金属钴的赋存状态是研究关键金属成矿作用的核心问题之一。由于含钴矿物粒度较小,难以在矿床尺度查明关键金属矿物的种类、含量、粒度、分布特征以及与其他矿石矿物和脉石矿物的共生关系,因此亟需建立一套成本低且效率高的钴赋存状态研究流程。本次工作以龙桥铁矿床为例,建立了新的采样与制样流程,提高了样品的代表性,并大幅缩短了样品前处理与制样的时间。通过综合矿物分析技术(TIMA)分析,查明了不同钴含量的三类矿石样品中矿物的含量,在6个实验矿石样品中寻找到了辉砷钴矿、铁硫砷钴矿和硫铜钴矿三种钴矿物共753颗,并使用扫描电镜和能谱分析(SEM-EDS)对钴矿物进行了核验与半定量分析。最后,在同一个树脂靶上利用激光剥蚀-等离子体质谱仪(LA-ICP-MS)对磁铁矿和黄铁矿进行了原位点分析,进一步查明了样品中钴的赋存状态。本次研究建立了关键金属钴在矿石中赋存状态的研究方法和技术流程,具有制样简单便捷、分析时间短、分析费用低和分析精度高等诸多优点,为矿床尺度上关键金属空间分布规律和赋存状态研究提供了可靠的技术支撑。     

X射线荧光光谱法测定土壤中主、次、微量元素

通过实验研究和分析借鉴前人成果,制定了土壤中40个主、次、微量成分粉末压片X射线荧光光谱分析方法,方法样品制备简单、消耗成本低、快速高效,绝大多数成分的检出限、精密度、准确度可满足多目标区域地球化学调查规范分析测试质量要求。     

地壳全元素配套分析方案及分析质量监控系统

依据有关的标准和规定要求,在76种元素地球化学填图配套分析方案及分析质量监控系统的基础上,建立了地壳岩石和土壤样品中81个指标(包含76个元素)的配套分析方案和分析质量监控系统。建立了新的岩石样品无污染加工流程,主量元素采用熔融制片-X射线荧光光谱法进行测定,并进行主量元素的加和控制,提升了主量元素的分析准确度和精密度,实现了对地壳全部元素的高准确度、高精度分析。     

The systematic determination of accuracy and precision in geochemical exploration data

Regional geochemical data from the 1:250,000 map series of Great Britain produced by the Institute of Geological Sciences are processed using a computer system developed for the National Geochemical Data Bank. The system, which can be used for the selective or complete retrieval of data and for statistical analysis and plotting, incorporates a procedure for determining accuracy and precision. Changes in accuracy are monitored by analysis of standards and the redetermination of sub-sets of samples using an instrumental neutron activation method. Samples are assigned random numbers in the field and are re-ordered sequentially prior to preparation and analysis in order to determine systematic errors occurring within batches of samples.Sampling, sub-sampling and analytical precision are monitored using analysis of variance methods on the results obtained on duplicate samples and analyses. The system for the efficient processing of this information is described and examples of the different types of error presented.     

碱熔-电感耦合等离子体质谱法测定化探样品中硼和锡

样品采用氢氧化钠熔融,电感耦合等离子体质谱法同时测定化探样品中硼和锡。方法检出限分别为硼0.65μg/g和锡0.12μg/g。方法用于土壤、水系沉积物国家一级标准物质的测定,结果均在标准值的允许误差范围之内,12次测定的相对标准偏差(RSD)均小于10%。样品处理程序简单快速,污染小,线性范围宽,分析重现性好,适用于地质部门大批量化探样品的分析。     

“特殊”煤光片制备及对煤岩分析的主要影响

煤岩分析在煤相研究、地质勘查、炼焦配煤等诸多方面有广泛应用;合格的煤光片是煤岩分析的前提。为解决易碎裂样品、老化煤光片等"特殊"煤光片的制备问题,提出了一套完整的制备流程,并实际验证了流程的可行性。老化粉煤光片二次煤岩分析结果表明:镜质体反射率受二次制备影响极小,显微组分含量受二次制备影响显著,且无烟煤的显微组分含量波动最大。老化粉煤光片二次显微组分定量时,应注意区分无烟煤的镜质组和惰质组,适当增加烟煤光片检测点数,以减小煤的非均质性对结果的影响。      

岩石矿物及粉尘中游离二氧化硅的测定

改进了游离二氧化硅（fSiO2)测定中试样的分解方法，采用硫－磷混酸替代单独使用磷酸分解试样，防止了焦磷酸盐的形成，同时，氟硼酸对fSiO2的溶解率符合测定要求。改进的方法用于标准物质中fSiO2的测定，结果与标准值或磷酸溶矿重量法相符。对于ω(fSiO2)=3.26%的标样10次测定的RSD为2．4％。     

Rietveld定量方法在蒸发岩矿物组分分析中的精确度评价和误差来源

Rietveld物相定量分析(RQPA)方法在地质学中已有大量应用,在蒸发岩定量分析中,对精确度的评价和误差控制是提高分析质量的重要因素。本文对人工配制和野外采集的样品(石膏和钾盐)进行RQPA分析,并与化学分析结果对比,评价其精确度并分析其主要的误差来源。结果表明:人工配制的氯化钠-氯化钾二元物相的绝对误差为0.4%~0.9%;氯化钠-氯化钾-碳酸钙三元物相的绝对误差为0.1%~1.2%;二元物相样品10次分析的标准偏差为0.702%,相对标准偏差为1.74%(氯化钾)和1.17%(氯化钠);野外采集的石膏和钾盐样品的RQPA分析结果与化学分析结果具有很好的一致性。表明RQPA方法在蒸发岩矿物组分定量分析中具有较高的精确度,其误差主要来源于样品性质、样品制备、测试条件和精修过程等。RQPA方法具有减弱择优取向效应、无需纯样以及提高数据利用率等优点,与化学分析技术联用在蒸发岩矿产勘探、储量评价以及工业应用中具有广泛的前景。     

偏振能量色散X射线荧光光谱法测定硫化物矿石中的铜铅锌

X射线荧光光谱法用于分析矿石主成分的常规制样方法有粉末压片法与玻璃熔融法,但分析硫含量高的地质样品时,前者存在矿物效应和粒度效应问题、后者可能腐蚀贵金属坩埚。为满足矿产勘查的需要,急需一种适应于硫化物矿石主成分分析的制样方法。本文建立了一种硝酸+氢氟酸封闭消解试样,标准溶液校准,偏振能量色散X射线荧光光谱(PE-EDXRF)同时测定硫化物样品中铜、铅、锌三种元素的分析方法。用GBW 07162~GBW 07168等7种矿石国家一级标准物质进行精密度和准确度实验。结果表明,当样品中铜、铅、锌元素含量大于1%时,几乎所有样品中的铜、铅、锌元素的精密度(RSD,n=6)优于5%,检测结果与标准值一致性良好。本方法通过样品消解、直接液体进样等技术的应用,消除了粒度效应和矿物效应等基体效应对分析结果的影响,解决了因缺乏基体匹配的标准物质而造成的含量校准的问题,使PE-EDXRF技术可以在硫化物矿石分析中得到比较方便的应用。这种分析方法为实验室矿石分析提供了新手段,也为野外现场PE-EDXRF分析高矿化度样品提供了新途径。     

电感耦合等离子体原子光谱法测定土壤样品中25个元素

采用盐酸-硝酸-氢氟酸-高氯酸消解样品,电感耦合等离子体原子光谱法测定土壤中25个主量、次量和微量元素。筛选了不同溶矿方法和仪器参数条件,方法精密度(RSD,n=11)为0.57%~3.50%。方法经国家一级土壤标准物质分析验证,测定值与标准值吻合。     

Dense-media separation as a more efficient pollen extraction method for use with organic sediment/deposit samples: comparison with the conventional method

Dense-media separation, frequently adopted as a standard pollen extraction method for use with minerogenic sediment samples, was adapted for use with organic-rich sediment and peat samples. A total of 15 organic-rich sediment samples, obtained from sites in Corsica and the Southern European Alps, was treated using both dense-media separation and the conventional preparation method in order to compare the relative efficiencies of the two methods. The dense-media separation method consistently achieved a remarkably higher purity of extracted pollen grains. This was especially true for the Corsican peat samples, the dense-media separations being quite pure, whereas the classical method produced samples that were so severely polluted with organic fragments that it was impossible to carry out a satisfactory pollen analysis. The percentage values of each taxon were generally similar using both methods, showing that the two methods are compatible for pollen analytical studies. Total pollen concentrations were generally higher with the dense-media separation method (especially for gyttja samples). In conclusion, dense-media separation is an efficient method for pollen extraction from organic as well as from minerogenic sediments and deposits.     

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。     

能量色散X射线荧光光谱法测定钼矿石中钼铅铁铜

建立了能量色散X射线荧光光谱法测定钼矿石中钼、铅、铁、铜的方法,讨论了粒度效应、矿物效应的影响因素,确定了采取粉末样品,用系列标准样品建立工作曲线,通过元素间相互校正消除基体效应,用内控标准样品考察了方法的精密度(RSD,n=11)为0.44%～15.4%。实际样品的测定结果和化学法相符,可满足日常分析工作需要。     

环境样品中多环芳烃、多氯联苯和有机氯农药 同时检测的分析方法

系统地综述了土壤、沉积物等环境样品中多环芳烃、多氯联苯和有机氯农药同时测定的分析方法,对快速同时提取技术、同步分离与净化技术、仪器同步测定技术分别进行了总结与评述,并对三类化合物同时测定技术的发展进行展望。     

Electron Probe Microanalysis of Environmental Samples: Preparation of Reference Materials, Correction for Particle Size Effects and Representative Results on Sediments Recovered from Snow, Power Station Fly Ash and Bone Samples

In this paper we report the results of electron probe X-ray microanalysis (EPMA) that was used to study environmental materials. The mode of preparation and certification of reference samples based on a basaltic glass matrix for environmental applications of EPMA is described. These samples were prepared containing scandium, strontium and barium (from 0.03 up to 7% m/m) and an evaluation was made of homogeneity, their stability to local heating, followed by analysis by independent methods for certification of composition. Matrix correction procedures for the EPMA technique have been developed for particles having a size commensurable with the volume of X-ray generation. An analytical equation for the size factor is proposed and two techniques for selecting optimum conditions for the analysis of environmental samples by EPMA are reported. These procedures provided satisfactory results when utilized in analysing sediments recovered from snow, coal fly ash and the bones of animals and fish, results from which can be used as indicators for evaluating the pollution level of the lower atmosphere, surface and ground water, as well as revealing pollution mechanisms.