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1.
Development of new techniques, enabling simultaneous determination of large numbers of elements in environmental samples, can force analysts to use certified reference materials that do not contain all the elements of interest. In this paper, the mass fractions of forty‐six major and trace elements, including rare earth elements (REE), are presented in one soil (NCS DC 77302 also known as GBW 07410) and five sediment (Metranal‐1, IAEA 405, MESS‐3, NCS DC 73309 also known as GBW 07311 and NCS DC 75301 also known as GBW 07314) certified reference materials determined by high resolution inductively coupled plasma‐mass spectrometry. The selected certified materials represent a spectrum of geological matrices often analysed in environmental studies. Measured elements include certified elements, elements listed with information values as well as new elements absent from certificates, including REEs and some other elements. REE + Y mass fractions in the river sediment reference material Metranal‐1 are reported for the first time. The results obtained are in agreement with available certified or information values.  相似文献   

2.
标准物质参考值的准确性在测试仪器校准、分析数据质量监控以及方法评价等方面具有非常重要的作用.为了检验国家地质标准物质参考值的准确性,本文应用高温高压密闭溶样-电感耦合等离子体质谱法分析了国家地质标准物质的18种岩石(GBW 07103 ～ GBW 07125)、19种沉积物(GBW 07301 ～ GBW 07318)和19种土壤(GBW 07401 ～ GBW 07430)中36种痕量与稀土元素.结果表明,除个别标准样品中的几个元素(Ni、Cr、Pb、Co、Cu、Sc、Yb、Lu)外,其余国家标准物质中36种元素测定结果的相对标准偏差均小于10％;绝大部分元素测定值的相对误差小于10％,测定值与参考值能较好地吻合.将误差较大元素的测定值与其他实验室的测定值以及文献报道值进行了比较,指出已有的参考值需要修正;针对部分沉积物和土壤中的元素未提供参考值,如GBW 07306的Ni、GBW 07313的Be、Hf、Ta,GBW 07314的Li、Be,GBW 07409、GBW 07410和GBW0741 1的Hf、Ta,GBW 07426的Gd、Ta,本文给出了相应的参考值.  相似文献   

3.
The processes resulting in the formation of a coarse‐grained sand beach ridge plain at Cowley Beach, north‐east Australia have been questioned by Tamura et al. (2018). These authors now acknowledge the conclusions by Nott et al. (2009) and Nott (2014) that the dominant depositional mechanisms here are waves and inundations generated during tropical cyclones. The Tamura et al. (2018) new ground penetrating radar data highlights that scarping of incipient ridges is a common feature and occurs regularly under non‐storm conditions. The upper sedimentary units deposited during storms are not scarped and demonstrate the high preservation potential and usefulness of these deposits for reconstructing long‐term records of tropical cyclones. Tamura et al. (2018) question the robustness of the methodology used by Nott & Hayne (2001), Nott (2003) and Nott et al. (2009) in estimating the magnitude of the storms responsible for these sedimentary deposits. These supposed issues though have been dealt with in detail in a series of publications over the past nearly two decades. The shortcomings of the Tamura et al. (2018) criticisms are explained in detail here.  相似文献   

4.
Fused glass prepared without the addition of a flux is generally more homogeneous than a pressed powder pellet and thus ideal for analysis of bulk samples by LA‐ICP‐MS. In this work, a new glass‐making method using a boron nitride crucible was developed to prepare homogenous glass samples from silicate rock powder. The apparatus consisted of a small boron nitride vessel with net volume of about 34 mm3 and two molybdenum strips. Applying the summed metal oxide normalisation technique, both major and trace element contents in the fused glass were measured by LA‐ICP‐MS. Analyses of five geochemical reference materials (spanning the compositional range basalt–andesite–rhyolite) indicated that the measured SiO2, Al2O3 and P2O5 contents matched the preferred values to within 5%, and the other major elements generally matched the preferred values to within 8%. Except for the transition metals, the measured trace element contents generally matched the preferred values to within 10%. Compared with the iridium heater method developed by Stoll et al. (2008), element volatilisation during high‐temperature melting was effectively suppressed in our method, but metal segregation caused by reduction of BN may cause loss of Cr, Ni and Cu. Although analysis with a large spot size has the advantage of improving counting statistics, matrix effects induced by mass loading of the ICP may hamper the accurate determination of some elements.  相似文献   

5.
Tamura et al. (2018) refined our understanding of formative processes that have resulted in a series of coarse‐sand beach ridges at Cowley Beach in north‐eastern Australia. Nott (2018) claimed that there are several shortcomings in the findings Tamura et al. (2018) presented. However, his criticism mostly derived from his misunderstanding of the data and discussion presented in Tamura et al. (2018), which thus should be clarified here. This reply also reiterates how his method for estimating the magnitude of past tropical cyclones from beach ridges is inconsistent with our observations of beach morphology and beach‐ridge formative processes.  相似文献   

6.
高岭土作为重要的铝硅酸盐,其微量元素的含量决定着高岭土产品的性能指标.高岭土的三种国家标准物质成分GBW03121、GBW03122、GBW03122a中均未含有As、Sb等10种微量元素的标准值,在高岭土的检测中只能采用近似的岩石标准物质作为监控物质,对高岭土组分的准确分析有一定影响.本文通过微波消解技术,对比了硝酸...  相似文献   

7.
泛滥平原沉积物标准物质研制   总被引：6，自引：6，他引：0  
泛滥平原沉积物能代表流域内元素的平均分布规律并具有普遍的适用性,是地球化学填图工作的重要介质。目前国际上尚无泛滥平原沉积物标准物质,国外相似标准物质的研制注重于环境方面,定值成分较少;我国同类的土壤和水系沉积物标准物质受限于不同工作需要,研制目的各不相同,且多数标准物质不足。为满足需求,本文研制了长江流域、赣江流域、汉水流域、淮河流域、黄河流域、海河流域、黑龙江流域共7个泛滥平原沉积物国家一级标准物质(编号为GBW07385～GBW07391)。此系列标准物质采用X射线荧光光谱压片法测试了26种成分,主量成分的RSD小于1%,微量元素的RSD约为2%,所有成分的RSD均小于7%,方差检验的F值均小于临界值F0. 05(24,25)=1. 96,表明样品的均匀性良好。在23个月的考察期内,检验的24种成分未发现统计学意义的明显变化,证明样品的稳定性良好。由全国13家实验室采用不同原理的、可靠的多种分析方法共同完成了73种元素和化合物共511个特性成分的定值测试,除GBW07386和GBW07388的CO2未能赋值外,其余494个特性成分给出了认定值与不确定度,15个特性成分给出了参考值,是我国同类标准物质定值最为齐全的一个系列。该系列标准物质代表了各自流域元素的背景含量,适用于多目标地球化学调查、土地质量地球化学调查等样品的分析质量监控,亦可用作环境、农业等领域相关样品测试的量值和质量监控标准。  相似文献   

8.
The influence of non‐spectral matrix effects on the determination of twenty‐two trace elements (Rb, Sr, Y, Cs, Ba, lanthanides, Pb, Th and U) in rock samples using ICP‐MS was investigated. Three types of multi‐element solutions were synthesised containing the twenty‐two trace elements, In, Tl and ten major rock‐forming elements with varying mass fractions mimicking the compositions of basalt, peridotite and dolomite. The synthetic solutions were conditioned to have dilution factors (DF) of 1000–10000. The extent of sensitivity suppression relative to the DF = 10000 solution became more significant for smaller DF solutions, which was not constant across different elements in a single solution but displayed general dependence on m/z. This indicates that at least two internal standards (e.g., In and Tl) are required for the correction of sensitivity variation. On the basis of the results, a new isotope dilution‐internal standardisation method for the determination of twenty‐two trace elements with ICP‐MS was developed, in which the sensitivity variation was corrected by monitoring two enriched isotopes, 113In and 203Tl. This method, coupled with the quantitative correction of interference from oxides and hydroxides, achieved precise determination of twenty‐two trace elements in some rock reference materials with reproducibilities of ±2% for basaltic to andesitic samples.  相似文献   

9.
Errors in Phelps et al. ( 2014 ) arise from: (i) inclusion of the East Texas Basin and basin‐flank formations in a regional stratigraphic transect purported to represent the San Marcos Arch (axis of the Comanche Platform, central and south Texas); and (ii) revision of Edwards Group strata (Person Formation) that ignores well‐documented studies in the subsurface and adjacent outcrops in the Balcones fault zone and Edwards Plateau. Consequently, the Upper Albian Composite Sequence 104–101 of Phelps et al. ( 2014 ) should be revised from one cycle to three and the upper boundary of the Albian Supersequence should be elevated to 99·6 Ma.  相似文献   

10.
样品用HNO3-HF高压密闭消解,电感耦合等离子体质谱测定海洋沉积物中15种稀土元素。研究了消解方法、酸体系和质谱干扰对稀土元素测定的影响。结果表明,相比于电热板消解和微波消解,高压密闭消解具有酸用量少、消解完全、消解过程损失少等优点;HNO3-HF体系能有效地分解海洋沉积物样品;利用干扰离子校正方程,能有效地校正Ba和轻稀土元素所形成的多原子离子干扰。15种稀土元素的方法检出限为3～15 ng/g。使用水系沉积物标准物质GBW 07309和GBW 07311、海底沉积物标准物质GBW 07313进行验证,测定值与标准值基本吻合,相对标准偏差和相对误差均低于5%。方法用于长江口沉积物样品的测定,精密度(RSD,n=6)小于5%,加标回收率为95.8%～104%。该方法检出限低,精密度和准确度高,适用于大批海洋沉积物样品的分析。  相似文献   

11.
采用低压聚乙烯镶边垫底的粉末样品压片制样,用PW2440X射线荧光光谱仪对多目标地球化学调查样品中Na2O、MgO、Al2O3、SiO2、P、K2O、CaO、Ti、Mn、Fe2O3、Co、Nb、Zr、Y、Sr、Rb、Pb、Th、Zn、Cu、Ni、V、Cr、Ba、La等组分进行测定。重点讨论了微量元素的背景选择和谱线重叠校正问题。使用经验系数法和康普顿散射线作内标校正基体效应,经标准物质分析检验,结果与标准值吻合,用GBW07308和GBW07310水系沉积物国家一级标准物质作精密度试验,统计结果RSD(n=12)除La、Cr、Co和Th<14.00%以外,其余各组分均小于6.00%。  相似文献   

12.
A new, rapid and highly efficient method for the determination of trace amounts of refractory elements (titanium, zirconium, hafnium, vanadium, niobium, tantalum, molybdenum) using micro-column separation/pre-concentration combined with fluorinating electrothermal vaporisation-inductively coupled plasma-mass spectrometry (FETV-ICP-MS) has been developed. In this method, trace amounts of the analytes were selectively adsorbed by a conical micro-column packed with the solid phase extraction material N -benzoyl- N -phenylhydroxylamine loaded on microcrystalline naphthalene at desired pH values. Various factors influencing the separation/pre-concentration, such as pH, sample flow rate and sample volume were studied in detail, and the influences of the organic matrix and the pre-ashing temperature on the determined results were also investigated. Under optimal conditions, the detection limits for Ti, Zr, Hf, V, Nb, Ta and Mo were 0.016, 0.011, 0.010, 0.007, 0.005, 0.006 and 0.003 ng ml−1, respectively, and the relative standard deviations ranged from 3.3% (Nb) to 9.6% (Hf) ( C = 0.20 ng ml−1, n = 9). In order to validate the method, the proposed method was applied to the analysis of three certified reference materials (soils GBW07401 and GBW07425; sediment GBW07301a) and the results obtained were in good agreement with the reference values. The method was also successfully applied to the analysis of real seawater samples with satisfactory results.  相似文献   

13.
海洋沉积物常用的分析方法如敞开消解或高压密闭消解结合电感耦合等离子体质谱(ICP-MS)或电感耦合等离子体发射光谱(ICP-OES)测定,粉末压片或熔片结合X射线荧光光谱法(XRF)测定,分别存在消解不完全、速度慢、检出限高等缺点,导致样品前处理效率低、待测元素少。针对上述问题,本文采用偏硼酸锂为熔剂分解样品,5%硝酸浸取,用ICP-MS法进行测定,建立了一种快速分析海洋沉积物中48种元素的方法。使用海洋沉积物国家标准物质作为高点绘制标准工作曲线,确定了助熔剂偏硼酸锂用量、稀释倍数、各待测元素的分析同位素及内标元素、仪器测定模式及个别元素的干扰校正方程等,得到最佳分解条件及测定条件。结果表明:由于高温损失,P、As、Se、Cd、Hg等元素无法得到准确结果,可改用微波消解等方式前处理后再进行测定;Cu、Zn、Cr、Ni、Co等共计48种元素使用本法均能得到准确结果,各元素方法精密度(RSD)均小于9.7%。本方法应用于分析海洋沉积物国家标准物质GBW07333、GBW07314、GBW07335、GBW07336,测定值和认定值相符;分析海洋沉积物实际样品,各元素加标回收率介于83.6%~118.6%。本方法可测定元素多,极大提高了分析效率,适合大批量样品分析。  相似文献   

14.
Coastal lagoons and beach ridges are genetically independent, though non‐continuous, sedimentary archives. We here combine the results from two recently published studies in order to produce an 8000‐year‐long record of Holocene relative sea‐level changes on the island of Samsø, southern Kattegat, Denmark. The reconstruction of the initial mid‐Holocene sea‐level rise is based on the sedimentary infill from topography‐confined coastal lagoons (Sander et al., Boreas, 2015b). Sea‐level index points over the mid‐ to late Holocene period of sea‐level stability and fall are retrieved from the internal structures of a wide beach‐ridge system (Hede et al., The Holocene, 2015). Data from sediment coring, georadar and absolute dating are thus combined in an inter‐disciplinary approach that is highly reproducible in micro‐tidal environments characterised by high sediment supply. We show here that the commonly proximate occurrence of coastal lagoons and beach ridges allows us to produce seamless time series of relative sea‐level changes from field sites in SW Scandinavia and in similar coastal environments.  相似文献   

15.
采用低压聚乙烯镶边垫底的粉末样品压片制样，用ARL ADVANT’XP＋型X射线荧光光谱仪对土壤和水系沉积物样品中C、N、Na2O、MgO、Al2O3、SiO2、P、S、Cl、K2O、CaO、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Nb、Zr、Y、Sr、Rb、Pb、Th、Ba、As、Br、Hf、La、Ce和Nd等36个组分进行测定。重点研究了C、N等元素的测定务件和痕量元素的背景选择和谱线重叠校正问题。使用经验系数法和康普敦散射作内标校正基体效应。经标准物质校验，结果与标准值吻合。方法的检出限、精密度和准确度能满足多目标地球化学调查样品的分析要求。用GBW 07404土壤国家标准物质进行测试，12次重复测定的精密度（RSD），除N和Cl〈11．0％，其余各组分均〈6．0％。  相似文献   

16.
由于电感耦合等离子体质谱(ICP-MS)分析不是在封闭的真空系统中进行,在测定过程中,气体、水和酸产生的一些离子都可能进入检测系统,产生干扰,严重影响痕量元素的准确分析。文章采用氢氟酸-硝酸封闭压力酸溶分解样品,ICP-MS法同时测定地质样品中Cu、Zn、Eu、Gd、Tb,研究了Ti、Ba、Ce、Pr、Nd对Cu、Zn、Eu、Gd、Tb的干扰情况。实验选择质量数65Cu、66Zn、153Eu、157Gd、159Tb作为测定同位素,用干扰系数脱机校正法校正分别来自Ti、Ba、Ce、Pr、Nd的氧化物重叠干扰,有效地解决了被干扰元素在测定时数值准确度低的问题。方法检出限(稀释因子1000)为:Cu 0.47μg/g、Zn 0.82μg/g、Eu 0.002μg/g、Gd 0.004μg/g、Tb 0.002μg/g,方法精密度(RSD,n=12)<5%,准确度(RE)<5%。方法用岩石、土壤、水系沉积物国家一级标准物质进行验证,测定值与标准值相符,适用于地质样品中Cu、Zn、Eu、Gd、Tb的测定。  相似文献   

17.
采用硝酸-氢氟酸-过氧化氢于微波消解仪中分解样品,电感耦合等离子体质谱法测定贵州遵义地区某黑色页岩中稀有稀土元素的含量。对页岩标准物质(GBW 07107)和水系沉积物地球化学成分分析标准物质(GBW07305、GBW 07310)的分析,测定值与标准值相一致。对黑色页岩的分析结果较好,方法精密度(RSD,n=6)各元素均小于4%,加标回收率为97.9%~100.1%。方法准确度高、简单、快捷,一次溶样可同时测定多种元素。  相似文献   

18.
凹凸棒黏土是具有层链状结构的含水富镁铝硅酸盐矿物,矿床成因不同导致凹凸棒黏土中微量元素的组成存在差异,其中Be、Cr、Ni、As、Cd、Sb、Hg、Pb会对健康和环境产生不利影响,而V、Mn、Co、Cu、Zn、Mo、Sn、Ba作为凹凸棒黏土的重要微量元素影响其性能和应用范围,因此,对凹凸棒黏土中微量元素进行精准分析可为凹凸棒黏土的高效增值深加工提供理论依据。采用电感耦合等离子体质谱法(ICP-MS)测定岩矿中微量元素具有检出限低和灵敏度高的特点,但因存在复杂质谱干扰,即使采用碰撞反应池(CRC)技术也很难完全消除。本文应用电感耦合等离子体串联质谱法(ICP-MS/MS)来消除质谱干扰,建立了准确测定凹凸棒黏土中微量元素Be、V、Cr、Mn、Co、Ni、Cu、Zn、As、Mo、Cd、Sn、Sb、Ba、Hg、Pb含量的分析方法。实验中采用由硝酸、盐酸、氢氟酸组成的混合酸对凹凸棒黏土样品进行微波消解,不仅加快了样品的消解速度,而且保持了消解溶液中分析元素的稳定。针对分析过程中所面临的质谱干扰,在MS/MS模式下,通过向CRC内加入O 2和NH3/He为反应气,利用质量转移反应生成相应的氧化物离子和团簇离子消除干扰,选择质量数相近且质谱行为相似的内标元素校正基体效应,稳定了分析信号。应用本方法对国家标准参考物质玄武岩(GBW07105)中16种微量元素进行测定,分析元素的相对误差在-9.60%~8.21%之间,相对标准偏差(RSD)≤6.0%。在选定的分析条件下,各元素的检出限为0.13~51.6ng/L。本方法有效减少了质谱干扰,提高了某些特定同位素在复杂介质中的准确性和灵敏度,适合凹凸棒黏土中16种微量元素的快速测定。  相似文献   

19.
微波消解-石墨炉原子吸收光谱法测定痕量银的研究   总被引：2，自引：0，他引：2  
传统的应用石墨炉原子吸收光谱法测定化探样品中的痕量银,一般采用盐酸-硝酸-氢氟酸-高氯酸电热板加热溶样,使用铱、铂为基体改进剂,但存在分析流程繁琐、成本高等缺点。相比于电热板消解法,微波消解技术的高压密闭消解和微波快速加热等特点,具有酸用量少、消解完全、消解过程损失少等优点。本文对传统的微波消解和仪器工作参数进行了改良,确定了最佳测定条件。建立了HNO_3-H_2O_2高压密闭消解样品,石墨炉原子吸收法测定水系沉积物、土壤、岩石中痕量银的方法。采用65%的HNO_3和H_2O_2微波消解溶样,加入12 g/L硫脲为介质,消除了基体干扰。方法检出限为0.018μg/g,将所建立的分析方法用于沉积物标准物质(GBW07309、GBW07311)、土壤标准物质(GBW07402、GBW07404)和岩石标准物质(GBW07103、GBW07104)验证,结果显示测定值与推荐值吻合,准确度△lg C(GBW)≤±0.024、RE(GBW)≤±5.71%,精密度RSD(GBW)≤5.97%。该分析方法适用于大批化探样品中痕量银的测定。  相似文献   

20.
Laser ablation multi-collector-inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) has become a valuable tool for the in situ measurement of the boron isotope composition of geological samples at high (tens to hundreds of μm) spatial resolution. That said, this application suffers from significant analytical challenges. We focus in this study on the underlying processes of two of the main causes for inaccuracies using this technique. We provide empirical evidence that not only Ca ions (Sadekov et al. 2019, Standish et al. 2019, Evans et al. 2021) but also Ar ions, that are reflected within the flight tube of the mass spectrometer, are the source for previously reported issues with spectral baselines. We also address the impact of plasma conditions on the instrumental mass fractionation as a source for matrix- and mass-load-related analytical biases. Comparing experimental data with the results of a dedicated release and diffusion model (RDM) we estimate that a close to complete (~ 97%) release of boron from the sample aerosol is needed to allow for consistently accurate LA boron isotope measurement results without the need for corrections.  相似文献   

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