Analysis of High Density Regional Geochemical Soil Samples at the Council for Geoscience (South Africa): The Importance of Quality Control Measures     

Hilde Maritz  H. C. C. Cloete  Jacobus H. Elsenbroek 《Geostandards and Geoanalytical Research》2010,34(3):265-273

The Council for Geoscience (CGS, South Africa) has a statutory mandate to carry out regional geochemical mapping in South Africa that needs to be rapidly and accurately analysed. Both simultaneous X-ray fluorescence spectrometry (S-XRF) and a newly developed method using inductively coupled plasma-mass spectrometry (ICP-MS) were employed. Various trace elements that could not previously be analysed by S-XRF can now be analysed by ICP-MS for the regional geochemical mapping programme, e.g., Cd, Mo, Te and Li. Using both techniques, the CGS aims to report element distributions for some fifty elements. To ensure that element concentration levels correlate over map boundaries, quality control measures in the sampling, sample preparation and analyses were of critical importance. This paper aims to discuss the sample preparation and quality control measures as applied to the ∼5500 samples of the Giyani and Tzaneen 1:100000 scale map sheets sampled at a density of one soil sample per km². ICP-MS batch- and instrumental drift-correction procedures will be discussed. As a final step, geochemical data were overlain over simplified geological maps using geographical information system software. These maps complement existing geological information of South Africa, help in the identification of exploration targets, test exploration models and initiate further geological research.  相似文献   

Determination of trace and rare-earth elements in Chinese soil and clay reference materials by ICP-MS   总被引：2，自引：0，他引：2  

Ye Liu  Chunrong Diwu  Yan Zhao  Xiaoming Liu  Honglin Yuan  Jianqi Wang 《中国地球化学学报》2014,33(1):95-102

Inductively coupled plasma mass spectrometry(ICP-MS) has become a powerful tool for providing reliable analytical results in many laboratories around the word. In this study, the mixture of HF and HNO3 acids in high-temperature and high-pressure closed-vessel digestion technique were used to decompose some Chinese reference materials, and thirty seven elements were determined by ICP-MS. Most of the results for Chinese soil reference materials were found to be in reasonable agreement with the reference values, except Cs, Ta, Li, Ge, Zn, Nd, Tb and Ta whose values need to be revised. Their precisions were typically lower than 5% RSD. However, the Precisions of Chinese clay reference materials, especially for GBW03102 and GBW03102a, were significantly different with reference values, probably reflecting the existence of a coarser-grained fraction(70 μm) in samples, and the formation of fluorides in Al-rich samples during sample decomposition by using the mixture of HF and HNO3 acids. Moreover, thirty-seven trace elements covering the mass range from Li to U in four Chinese clay reference materials were firstly provided with good precision and accuracy in this study.  相似文献   

应用电感耦合等离子体质谱/光谱法研究上扬子区新华磷块岩稀土元素特征及沉积学意义   总被引：2，自引：2，他引：0  

段凯波  王登红  何汉江  郑国栋  熊先孝  袁建国  贺宝宝  屈云燕 《岩矿测试》2015,34(2):261-267

新华磷矿床是我国重要的富集稀土元素的沉积型含稀土磷块岩矿床,本文利用电感耦合等离子体质谱/光谱法(ICP-MS/AES),辅以岩矿鉴定等分析技术,结合沉积学理论研究了新华磷块岩稀土元素地球化学特征及相关问题。结果表明,新华磷块岩稀土总量(∑REEs)较高,集中值介于800×10-6~1200×10-6,其组成属轻稀土+钇型,稀土元素主要以类质同象形式存在于胶磷矿中;新华磷块岩和昆阳磷块岩具相似的REEs配分曲线和明显铈负异常,δCe介于0.28~0.36,表明上扬子区南缘成磷环境为氧化条件,且为稳定的滨浅海被动大陆边缘沉积环境;但新华磷块岩与其上覆黑色岩系REEs配分曲线迥异,后者表现出不明显的铈、铕异常,说明黑色岩系主要形成于深海-半深海静水还原环境,从梅树村期早期至晚期经历了海平面升高的过程,地层层序整体显示向上变深的沉积相变,磷块岩和黑色岩系之间的接触面可能为三级层序甚至更小层序级别的界面。这些沉积学的认识揭示了上扬子区下寒武统层序地层学意义和海相沉积环境特征,对华南早寒武世生命大爆发和层序地层学深入研究提供了证据。  相似文献   

贵州习水洞子沟铅锌矿床闪锌矿微量元素特征与成因     

陈翠华  宋志娇  杨玉龙  杨德平  辜鹰  陈宵杰 《矿物学报》2019,39(5):485-493

贵州习水县洞子沟铅锌矿床位于桑木场背斜核部,矿体呈层状、似层状、脉状产出于灯影组白云岩中,矿石矿物以闪锌矿为主,脉石矿物主要为重晶石、白云石。对单矿物的微量元素ICP-MS分析结果表明,该矿床闪锌矿相对富集Cu、Zn、Pb、Ba、Ga、Ag、Ge等元素,而Mn、Fe、Cd、In、Mo、Se、Tl等相对较贫,其Ga/In(118.83~968.33)、Ge/In(471.88~14079.40),Zn/Cd(196.94~246.27),Zn/Fe(24.67~384.95)比值相似于中低温铅锌矿床闪锌矿,暗示其形成于中低温环境。总体上,洞子沟铅锌矿床闪锌矿微量元素组成特征与喷流沉积型、岩浆热液型铅锌矿床区别明显,而与一些典型MVT型铅锌矿(如马元铅锌矿、大梁子铅锌矿、天桥铅锌矿等)类似,结合该矿床地质特征,本文认为洞子沟铅锌矿成因类型属于非典型的MVT类型。  相似文献   

Determination of Molybdenum, Antimony and Tungsten at sub μg g⁻¹ Levels in Geological Materials by ID-FI-ICP-MS     

Akio Makishima  Eizo Nakamura 《Geostandards and Geoanalytical Research》1999,23(2):137-148

We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94% for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81%. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g⁻¹ level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was < 9%. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates.  相似文献   

Determination of Zirconium, Niobium, Hafnium and Tantalum at ng g-1 Levels in Geological Materials by Direct Nebulisation of Sample HF Solution into FI-ICP-MS     

Akio Makishima  Eizo Nakamura  Toshio Nakano 《Geostandards and Geoanalytical Research》1999,23(1):7-20

We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble M and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were > 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder.  相似文献   

贵州荔波地区2000年来石笋高分辨率的气候记录   总被引：10，自引：1，他引：9  

张美良  程海  林玉石  覃嘉铭  朱晓燕  冉景丞  杨琰  陈会明  Edwards R L 《沉积学报》2006,24(3):339-348

通过对荔波董哥洞石笋进行高精度的ICP MS或TIMS U系测年和碳、氧同位素分析,建立了荔波地区2 300a B.P.来高分辨率的古气候变化的时间序列。研究结果表明,贵州荔波地区2 300a B.P.以来石笋记录的季风气候变化,大致可分为8个气候(亚)期:① 2 300～1 800a B.P.为降温期,显示东亚夏季风减弱,东亚冬季风增强,气候干旱寒冷;② 1 800～1 080a B.P.气温有所回升,显示东亚冬季风缓慢减弱,东亚夏季风有所回升,表现为半湿润的温凉气候期;③ 1 080～680a B.P. 为降温期,气温再次下降,显示东亚冬季风再次增强,但降水相对增大,表现为寒冷湿润的气候期,是气候变化的关键转折时期;④ 680～550a B.P.温暖期,显示东亚夏季风再次增强,气温升高,降水增大,表现为温暖湿润的气候期。⑤ 550～400a B.P.寒冷期,显示东亚冬季风快速增强,气温下降,表现为寒冷湿润的气候环境,是近1 000年以来最冷的时期;⑥ 400～364a B.P.温凉期,显示东亚夏季风有所增强,气温有所回升,表现为温凉湿润气候环境;⑦ 364～324a B.P.冷凉期,显示东亚夏季风有所减弱,气温有所下降,表现为冷凉湿润气候环境;⑧ 324a B.P.至今,气候相对波动期,同位素记录曲线呈锯齿状波动,在其内包括若干个冷凉半湿润、冷湿的气候变化亚阶段。根据荔波董哥洞石笋的高分辨率的古气候变化的连续记录,揭示了荔波地区2 300a B.P.以来的一些百年尺度的重大气候事件——干旱寒冷期、隋唐温暖期(或小温暖期)、小寒冷期以及一些十年尺度的降水、温度变化。石笋记录的这种百年、十年尺度的突发性气候变化事件,与冰芯记录极为相似,反映低纬度地区石笋记录的季风气候与高纬度及北极地区的气候具有极好的相关性,这对于认识现代气候系统变化以及对未来十年—百年尺度的气候预测和演化的驱动机制,具有重要的科学意义。  相似文献   

离线固相萃取螯合富集分离-ICP-MS测定海水中的稀土元素   总被引：1，自引：0，他引：1  

刘瑶  宋金明  林强  于颖  孙玲玲  温廷宇 《海洋科学》2017,41(9):34-40

通过测定条件优化、方法比对等实验建立了一种固相萃取小柱离线螯合富集分离电感耦合等离子体质谱仪测定海水中稀土元素的方法。海水样品通过调节p H后,进入VAC ELUT SPS24 Agilent圆形固相萃取装置,其主要基体物质的去除率高于97%;萃取富集的优化条件是海水样品p H 4.0~7.0,海水进入萃取柱速率2 m L/min,硝酸洗脱液浓度为1 mol/L;方法对稀土元素的加标回收率为83%~108%,14种稀土元素的检出限为0.057~0.613 ng/L,RSD10%;该方法与氢氧化铁共沉淀法富集稀土元素比对测定结果一致,方法具有准确度与精密度高、操作简便快速等优点,可用于海水样品中稀土元素的定量精确测量。  相似文献   

The distribution of dissolved lead in the coastal waters of the East China Sea     

Yan Li  Rujun Yang  Aibin Zhang  Shirong Wang 《Marine pollution bulletin》2014

The distribution of dissolved lead in the coastal waters of the East China Sea was investigated seasonally. The average concentrations in surface waters during the spring and autumn were 0.52 nM and 0.27 nM, respectively. In the spring, the concentration of dissolved Pb in the surface waters and bottom waters ranged from 0.13 to 1.86 nM and from 0.15 to 0.94 nM, respectively. For both the surface water and the bottom water, the highest values were observed at the Yangtze River Estuary. Seasonal variability of D-Pb between spring and autumn in the ECS was observed. These results suggested that riverine inputs and atmospheric inputs may be the main sources of lead in this area, while adsorption and co-precipitation on suspended particles at the river estuary and biological process may be the major sinks.  相似文献   

CP-MS测定饮用水中Fe的方法     

孙国荣  李东雷  左宇昕  谢云欣  万飞  李淑君 《吉林地质》2009,28(4)

通过实验确定了ICP-MS检测饮用水中Fe的质量质量浓度方法。检测方法的检出限(DL)和精密度(RSD)分别达到3.29ng/mL和4.49%(n=12)。  相似文献