在线萃取－火焰原子吸收测定地质样品中的痕量金     

胡定煜  帅琴 《黄金地质》1995,(4)

利用流动注射在线萃取技术，以ＭＩＢＫ为萃取剂，用火焰原子吸收分析方法测定地质样品中的痕量金，取得了满意的效果。该法精密度好，无污染，操作简便，测定迅速，且样品不需分离。方法检出限Ａｕ为０．７８×１０－９，精密度为２．３０％。  相似文献   

探测受压岩样破裂区域的CT试验方法     

杨建辉  张志海 《CT理论与应用研究》1993,(1)

本文对应用SYC 系列声波仪探测室内受压岩样破裂区域的试验技术进行了分析,提出了一种在稳压阶段及卸荷后测量声波走时的试验方法,并通过试验对时间因素及卸荷产生的走时误差进行了初步探讨,证明这种试验方法是可行的。  相似文献   

化探样品中微量铅、锡、铬、钼和钴的发射光谱法同时测定     

张明恭  陈梅一  苏勇 《矿物岩石》1993,(1)

本文以CdCl_2·2.5H_2O为反应剂,采用“下垫上滴”缓冲刺的装样形式,通过大量镉盐的蒸发控制电极温度,使被测元素预先分馏,有效地改善了它们的蒸发行为,同时,减小了基体效应、光谱背景。本法其有良好的精密度和准确度,各元素的检出限(×10~(-5))分别为:Pb(1),Sn(0.37),Cr(1.8),Ni(3.51,Mo(0.1)和Co(0.38),其相对标准偏差(RSD)为±3.7—9.5%  相似文献   

水和土壤中微量镍测定的研究   总被引：4，自引：1，他引：4  

魏琴  马荣 《矿物岩石》1993,13(3):115-118

本文研究了PAN-S与镍的显色反应条件。镍与PAN-S反应的最佳pH范围为3.8—9.0。配合物的最大吸收峰位于560nm波长处,表观摩尔吸光系数为3.30×10~4L·mol~(-1)·cm~(-1),25ml试液中镍量在0—1μg/ml范围内服从比尔定律,方法用于水和土壤样品中微量镍的测定,结果良好。  相似文献   

结构面粗糙度统计测量最小样本数确定方法     

侯钦宽  雍睿  杜时贵  徐敏娜  曹泽敏 《岩土力学》2020,41(4):1259-1269

由于结构面粗糙度具有各质异性、各向异性、非均一性和尺寸效应等特征，结构面粗糙度系数（JRC）取值具有不确定性，工程中广泛采用统计方法来分析结构面粗糙度性质，然而以往研究往往忽略样本数不足对统计结果的影响。针对结构面粗糙度统计测量时无法确定合理样本数的问题，分别提出基于变异系数级比分析及简单随机抽样原理的最小样本数确定方法。以实际工程岩体结构面表面数据为研究对象，对比分析两种方法在系列尺寸下确定的统计测量最小样本数。实例分析表明：小尺寸样本的变异系数（CV）值明显大于大尺寸样本，且CV值随取样尺寸的增大而减小，取样尺寸为10～50 cm的CV值基本稳定在0.31～0.47之间，取样尺寸为60～100 cm的CV值基本稳定在0.21～0.31之间；最小样本数与取样尺寸基本满足幂函数关系，且最小样本数随取样尺寸的增大而减少；系列尺寸下级比分析方法在允许误差为±2%时确定的最小样本数与简单随机抽样原理在最大允许误差为10%、置信度为95%时计算的最小样本数是一致的，相似度大于0.997。该研究方法可为工程岩体中定量获取结构面粗糙度统计测量最小样本数提供依据，保证了JRC（结构面粗糙度系数）统计测量结果的准确性，对工程岩体稳定性评价中结构面力学参数的准确获取具有重要意义。  相似文献   

Pressurised Extraction Using Dilute Ammonia: A Simple Method for Determination of Iodine in Soil, Sediment and Biological Samples by Inductively Coupled Plasma-Mass Spectrometry     

Li Bing  Ma Xinrong  Han Lirong  Yang Hongxia 《Geostandards and Geoanalytical Research》2004,28(2):317-323

A simple sample treatment method for the accurate and precise determination of iodine in soil, sediment and biological samples by inductively coupled plasma-mass spectrometry (ICP-MS) is described. Iodine in samples was extracted in screw top PTFE-lined stainless steel bombs using a 10% v/v ammonia solution at 185 C for 18 hours (overnight), after which the extract was introduced into the ICP-MS for direct measurement. ¹²⁶Te was employed as the internal standard to compensate for matrix effects and instrument drift. The limit of detection (LOD, three times the standard deviation of the procedural blank solution, expressed as the concentration in the sample solution) was 0.003 ng ml-^-1. The limit of quantitation (LOQ, ten times the standard deviation of the procedural blank solution, expressed as the concentration in the solid samples, dilution factor DF = 100) was 0.01 μg g-^-1 (dry mass). The accuracy and precision of the method were demonstrated by analysing different Chinese geological certified reference materials (soils, stream sediments and a hair sample). The measured concentrations were in a good agreement with the certified values indicating that bias in the method was not significant. The precision (n = 10) for different concentrations ranged from 1.82% to 4.32% RSD. Comparison of the ammonia extraction procedure with a "sintering" method indicated that there was no significant difference in results obtained with the two methods for geological soil and stream sediment samples. However, for biological samples, such as hair, kelp, tea etc., the results obtained by the sintering method were far below those of the ammonia extraction method. The ammonia extraction has advantages, as it is simpler than the "sintering" method, and has a lower procedural blank, better detection limits and reproducibility. Due to the simplicity of the method, a high rate of sample throughput is possible.  相似文献   

Analytical Developments in Secondary Ion Mass Spectrometry 2003     

Etienne Deloule  Michael Wiedenbeck 《Geostandards and Geoanalytical Research》2005,29(1):37-40

This annual review of secondary ion mass spectrometry (SIMS) highlights significant progress in the application of the technology for the following areas: U-Pb geochronology (notably in the fields of reference material zircons), sources of uncertainty during analysis and secondary ion yields. Major publications introduced a new zircon reference sample and dealt with an intercomparison study of a suite of established calibrators, some of which have been shown to have certain limitations. Another publication claimed that the principal uncertainty in U-Pb dating is related to variations in the Pb and U relative emission yields over a complete analytical session. 2003 saw the introduction of an automated particle identification procedure applied to the analysis of a chondritic meteorite, as well as new geometries of SIMS hardware (NanoSIMS) and techniques (time-of-flight SIMS). NanoSIMS allows a two to three order of magnitude reduction in sampling volume as a result of a reduced beam diameter, and time-of-flight SIMS allows the study of sample surfaces, and can provide data for elements concurrently.  相似文献   

Determination of the Trace Refractory Elements V, Nb and Ta in Environmental Samples by ICP-MS After Separation and Preconcentration with Nanometre-Sized Alumina Microcolumns Following Chemical Modification by Gallic Acid     

Xuli Pu  Chaozhang Huang  Bin Hu  Zucheng Jiang 《Geostandards and Geoanalytical Research》2006,30(2):97-105

Nanometre-sized alumina was chemically modified with gallic acid (GA) and used as a solid phase adsorption material for the determination of trace amounts of V, Nb and Ta in natural water, soil and stream sediment samples by inductively coupled plasma-mass spectrometry. The effects of pH, sample flow rate and volume, elution solution and interfering ions on the recovery of the analytes were investigated. The results showed that V, Nb and Ta could be adsorbed at pH 4.0 and recovered with 1 ml of 2.0 mol l^-1 HCl. Under optimised conditions, the adsorption capacity of GA-modified nanometre-sized Al₂O₃ was found to be 7.0, 8.9, 13.3 mg g^-1 for V, Nb and Ta, respectively. The limits of detection were as low as 0.25, 0.24 and 0.66 ng l^-1 for V, Nb and Ta, respectively with a concentration factor of fifty. The recovery of V, Nb and Ta for spiked water samples was between 85.7 and 116%. The developed method has also been applied to the determination of trace V, Nb and Ta in soil and stream sediment certified materials, and the determined values were in a good agreement with the certified values.  相似文献   

中国大陆科学钻探（CCSD）主孔100-2000m区间磁化率的变异特征及其地质意义     

杨涛  刘庆生  吴耀  金振民  潘和平  牛一雄 《岩石学报》2006,22(7):2089-2094

对中国大陆科学钻探主孔100—2000m区间岩心样品磁化率与钻孔原位测井磁化率进行系统时比研究。结果表明,控制岩石磁化率的主要因素是岩性和退变质作用,其中蛇纹石化石榴石橄榄岩的磁化率最大,样品平均磁化率为86．277×10-3SI,正片麻岩,退变质榴辉岩,榴辉岩,副片麻岩次之,角闪岩的磁化率最小,样品平均磁化率为1．698×10-3SI。不同退变质程度榴辉岩的磁化率特征具有明显的差异:中-强程度退变质榴辉岩由于退变质过程所产生的磁铁矿和钛铁矿-钛磁铁矿,其磁化率最大;随着退变质作用的进一步加剧,这些磁铁矿和钛铁矿-钛磁铁矿被完全分解,导致完全退变质榴辉岩的磁化率最小;新鲜榴辉岩的磁化率介于两者之间。在该深度区间,约70％岩心样品磁化率与测井磁化率的比值小于4．0,其中以<2．0为主,相同岩性岩石(如榴辉岩,退变质榴辉岩和副片麻岩)磁化率的比值随深度变化较小。岩心样品磁化率和测井磁化率之间的欧氏距离位于3．0-6．4范围,且随深度变化不明显,如在100～600m和1500～2000m两个深度范围的欧氏距离分别为3．0-5．2和3．2～5．3,表现出相似的变化特征,显示了在此区间深度范围内,地层压力对磁化率的基本没有影响。  相似文献   

流动注射分析及其在地质样品痕量元素测试中的应用   总被引：1，自引：0，他引：1  

邹海峰  姜桂兰 《世界地质》1998,(2)

简述了流动注射分析方法的发展及其特点,介绍了流动注射在线分析技术,包括流动注射－原子光谱法、流动注射－分光光度法和流动注射－电化学分析法等联用技术在地质样品分析中的应用情况。  相似文献