微波消解-电感耦合等离子体质谱法测定土壤中稀土元素条件优化     

张祎玮  蒋俊平  李浩  沈讷敏 《岩石矿物学杂志》2021,40(3):605-613

稀土元素因其用途广泛,已经得到了越来越多的关注,被应用于各个行业。研究表明,稀土元素对作物的光合作用、产量、抗逆、品质、发育和养分吸收等具有重要作用。作物中的稀土元素主要来自对土壤中稀土元素的吸收,因此,有效分解并快速测定土壤中的稀土元素,可以合理指导稀土元素的施用,对作物的生长和土壤的营养状况具有重要作用。本文比较了敞口酸溶、密闭消解、微波消解和碱熔等4种消解样品前处理方法,最终确定采用微波消解-电感耦合等离子体质谱法(ICP-MS)快速测定土壤中的稀土元素,并通过优化微波消解的条件,选择合适的试剂用量、消解温度、消解时间,对方法的检出限、精密度、准确度、回收率进行了实验,结果显示其测定均值与标准值基本吻合,相对误差(RE)绝对值为0.16%～3.39%,精密度为0.27%～5.09%,均小于10%,加标回收率为93.1%～106.0%。该方法准确度高、稳定性好,可以有效地应用于土壤中稀土元素的分析测定。  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   

微波消解-电感耦合等离子体质谱法测定土壤和沉积物中痕量稀土元素   总被引：11，自引：6，他引：5  

陈永欣  黎香荣  韦新红  吕泽娥  谢毓群  蔡维专 《岩矿测试》2011,30(5):560-565

建立了微波消解-电感耦合等离子体质谱法测定土壤和沉积物中15种痕量稀土元素的分析方法。研究了溶样试剂、微波消解程序、标准溶液配制、质谱干扰与内标元素对稀土元素测定的影响。加入氢氟酸能有效打开样品,以HNO3-HF-H2O2混合酸溶解样品,稀土元素的溶出率较高。采用模拟土壤、沉积物中稀土元素天然组成比值的校正溶液,对稀土元素间的干扰具有明显的抑制作用。通过测定单个La、Ce、Pr、Nd和Ba的氧化物及氢氧化物产率,计算出等效干扰浓度,进而校正多原子离子干扰。利用103Rh内标校正系统,有效地抑制了分析信号的动态漂移。方法检出限为1.2～7.1 ng/g,精密度(RSD)≤5.3%(n=6),加标回收率为86.1%～110.1%。使用土壤、沉积物标准物质进行验证,测定结果与标准值相符。建立的方法样品处理程序简单快速、线性范围宽、分析重现性好、结果准确,适用于大批量地质样品的分析。  相似文献   

Relationship among geochemical elements in soil and grapes as terroir fingerprintings in Vitis vinifera L. cv. “Glera”     

《Chemie der Erde / Geochemistry》2017,77(1):121-130

Prosecco, one of the most popular sparkling wines in the world, is produced in Italy. For this reason, it is important to develop a scientific method for determining geographic origin in order to prevent fraudulent labelling. To establish the relationship between geochemistry of vineyard soil and chemical composition of grape, a geochemical characterization of “Glera”, a Vitis vinifera cultivar from Italian Region, Veneto was undertaken. We evaluated the relationship between major and trace elements in soil and their concentrations in “Glera” grape berries in vineyards belonging to five localities in the Veneto alluvial plain, all included in the Controlled Designation of Origin (DOC) area of Prosecco. A statistically significant correspondence between the soil and grape was observed for Sr. Multivariate analysis (LDA) allowed discrimination of samples of soil and grape berries from each single winery according to the geographic origin. The elements that could establish a reliable correspondence between the geolithological features of the vineyard soil and the chemical composition of grape berries are: Sr, Ba, Ca, Mg, Al, K, Zn, B, Ni, Co.  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   

Origin of highly siderophile and chalcogen element fractionations in the components of unequilibrated H and LL chondrites     

《Chemie der Erde / Geochemistry》2017,77(1):105-119

Osmium isotopic compositions, abundances of highly siderophile elements (HSE: platinum group elements, Re and Au), the chalcogen elements S, Se and Te and major and minor elements were analysed in physically separated size fractions and components of the ordinary chondrites WSG 95300 (H3.3, meteorite find) and Parnallee (LL3.6, meteorite fall). Fine grained magnetic fractions are 268-65 times enriched in HSE compared to the non-magnetic fractions. A significant deviation of some fractions of WSG 95300 from the 4.568 Ga ¹⁸⁷Re-¹⁸⁷Os isochron was caused by redistribution of Re due to weathering of metal. HSE abundance patterns show that at least four different types of HSE carriers are present in WSG 95300 and Parnallee. The HSE carriers display (i) CI chondritic HSE ratios, (ii) variable Re/Os ratios, (iii) lower than CI chondritic Pd/Ir and Au/Ir and (iv) higher Pt/Ir and Pt/Ru than in CI chondrites. These differences between components clearly indicate the loss of refractory HSE carrier phases before accretion of the components. Tellurium abundances correlate with Pd and are decoupled from S, suggesting that most Te partitioned into metal during the last high-temperature event. Tellurium is depleted in all fractions compared to CI chondrite normalized Se abundances. The depletion of Te is likely associated with the high temperature history of the metal precursors of H and LL chondrites and occurred independent of the metal loss event that depleted LL chondrites in siderophile elements. Most non-magnetic and slightly magnetic fractions have S/Se close to CI chondrites. In contrast, the decoupling of Te and Se from S in magnetic fractions suggests the influence of volatility and metal-silicate partitioning on the abundances of the chalcogen elements. The influence of terrestrial weathering on chalcogen element systematics of these meteorites appears to be negligible.  相似文献   

ICP-MS及其联用技术在海洋地质研究中的应用前景     

刘昌岭  贺行良 《海洋地质前沿》2006,22(8):30-34

电感耦合等离子体质谱(ICP—MS)具有灵敏度高、检出限低、选择性好、线性范围宽、能进行多元素和同位素比测定等优点,广泛应用于环境、地质、医药、食品和高纯物质等领域。ICP—MS与其他进样及分析技术的联用,大大地扩展了其应用范围。重点介绍了ICP—MS与激光烧蚀(LA)、高效液相色谱(HPLC)及气相色谱(GC)的联用技术,探讨了它们在海洋地质研究中的应用前景。  相似文献   

High resolution micromill sampling for analysis of fish otoliths by ICP-MS: effects of sampling and specimen preparation on trace element fingerprints     

Arslan Z  Secor DH 《Marine environmental research》2008,66(3):364-371

Otoliths are calcified structures in the head of fish that record environmental information about fish's life history. Gathering the elemental information from the core of an otolith corresponding to the juvenile period of fish's life is critical to discriminate the adult fish to their natal habitats reliably. A high resolution micromill has been used to isolate the otolith core from a whole otolith for elemental analysis. The effects of micromilling procedures (e.g., sectioning, embedding and drilling) on contamination to otolith trace element levels were examined using paired blackfin tuna (Thunnus atlanticus) otoliths. Otoliths were decontaminated by dilute hydrogen peroxide and nitric acid throughout to remove surface contamination. A preconcentration procedure was used to determine the trace elements from the small core material by ICP-MS. It was found that micromilling procedures introduce significant contamination to otoliths, especially for Al, Cu, Pb and Zn. The sectioning procedure caused significant contamination for Co and Cu, while the embedding procedure resulted in contamination for nearly all trace elements (Al, Cd, Co, Cu, Ga, Mn, Ni, Pb, V and Zn). The combined sectioning, embedding and drilling procedure also resulted in contamination for most trace elements. Despite the contamination across all procedural steps, the decontamination procedure effectively removed the surface contamination with the exception of Pb and Zn. Bias (e.g., residual contamination) on Pb was small in comparison to overall concentration of Pb expected to occur in fish otoliths, therefore, its effect may be minor in discriminating individuals. Bias on Zn was larger that could limit its application in discriminating individuals.  相似文献   

厦门海域鱼体稀土元素的生态化学特征   总被引：3，自引：0，他引：3       下载免费PDF全文

郭卫东  胡明辉  杨逸萍  弓振斌  吴玉梅 《海洋与湖沼》2003,34(3):241-248

于1995—1996年在厦门海域采集了28种鱼类样品，用ICP—MS法测定了15种稀土元素(REE)的含量，研究了鱼体稀土元素的组成和分布模式及与海水环境之间的关系。结果表明，厦门海域鱼体REE总量介于12．4—596．5ng／g，平均为(77．5l2．8)岭g。鱼体明显官集轻稀土，同时轻、重稀土之间则存在较大的分馏作用，说明轻稀土的生物学效应比重稀土更为显著。鱼类稀土元素分布模式总体上与海水REE分布模式接近，并且鱼类REE含量与近岸陆架海水REE含量之间有很好的相关性，说明海洋鱼类对稀土元素的利用遵从丰度规律。鱼类对稀土元素的富集系数在103以上。稀土元素沿厦门海域食物链的迁移传递没有表现出明显的生物放大作用。  相似文献   

Os水吸收液ICP-MS测量信号强度衰减原因研究     

周利敏  李超  李欣尉  赵鸿  屈文俊  杜安道 《岩矿测试》2018,37(4):431-438

蒸馏法能从样品中有效分离出OsO_4,吸收液直接用于ICP-MS测定,是辉钼矿Re-Os定年的关键技术环节。但实验发现,长时间放置的吸收液中Os信号强度显著降低。根据OsO_4化学性质推测原因在于一是挥发使吸收液Os含量减少,二是还原使+8价Os变成低价态,气态比例降低,若雾化效率不变,进入质谱仪的Os减少,两者都会导致信号降低,但具体影响情况不明,需深入研究。本文利用辉钼矿标准物质制备不同放置时间、酸度和温度的吸收液,对比上述条件对ICP-MS信号强度的影响。实验时将残余吸收液与稀释剂、氧化剂封入Carius管加热蒸馏,测定Os含量。结果表明:吸收液放置时间越长,酸度越低,温度越高,信号降幅越大,幅度达到3.2%~68.6%。室温下放置相同时间,低酸度吸收液的Os保存率高于高酸度吸收液,但Os信号强度低于后者,证明了挥发和还原共同导致信号衰减,且还原是主导原因。本文提出,冷冻(-18℃)可抑制OsO_4挥发,提高酸度(约3.5 mol/L)可减弱OsO_4还原,两者结合抑制信号衰减,提高了蒸馏法的灵活性和适用性。  相似文献