甲基膦酸二甲庚酯(P(350))——吸附树脂萃取色层分离连续测定矿石中铀和钍

本文选用水溶性比TBP小30倍而对钍、铀分离效率高的P350为萃取色层的固定相和对有机萃取剂吸附容量大、传质速度快的新型大孔吸附树脂x-5(聚二乙烯苯)为支持体,以含15％HNO_3和15％NH_4NO_3(或7％Al(NO_3)_3)及2％酒石酸的混合液为铀、钍上柱液,采用5N HCl及0.2％NaF分别解脱钍和铀,分光光度法分别测定之。     

TRPO萃取分离测定化探样品中微量铀、钍

本文根据有关文献介绍三烷基氧磷(简称TRPO)为含磷的有机化合物,具有萃取铀、钍的特性。在1molL~(-1)HNO_3介质中萃取铀和钍,其分子式为UO_2(NO_3)_2·2TRPO和Th(NO_3)_4·TRPO;然后用草酸溶液反萃取钍,其络合物为Th(C-2O4)_4·6H_2O;再用混合络合剂反萃取铀。     

TOPO萃取光度法连续测定地球化学样品中的铀和钍

铀、钍在地壳中的含量平均约3ppm至8ppm。地球化学探矿样品一般要求测定低于地壳平均值的含量,如1—2ppm的铀或钍。在一次分离的溶液中测定两个痕量元素是最可取的。 Pollock在抗坏血酸存在下以硼酸掩蔽氟,用TOPO(三辛基氧膦)的环已烷溶液一次萃取铀和钍;由于要分取萃出液测定,故不能充分降低检出限。陈文华等先用氟掩蔽钍TOPC萃取铀,再用铝掩蔽氟连续萃取钍,虽弥补了上文之不足,但需两次萃取。本文采取一次萃取铀、钍,然后用0.8％氟化铵的2N硝酸溶液反萃取钍,分别在有机     

一次分解试样测定地质样品中~(230)Th,~(232)Th和~(234)U/~(238)U,~(230)Th/~(232)Th

试验了用~(234)Th示踪,一次分解试样测定~(234)Th,~(232)Th和~(234)U/~(238)U,~(230)Th/~(232)Th的快速方法。试样经Na_2O_2熔融分解,并以P350萃取色层法分离铀、钍。然后分别电沉积制备无自吸收铀、钍α源进行α谱测量。本法适用于铀矿石、岩石和土壤试样的测定。     

阳离子交换树脂填充纸吸附、X—射线荧光光谱法测定矿石及选冶样品中的钍

本文叙述了阳离子交换纸对钍的予富集、吸附条件及干扰情况。发现在保温条件下,静态吸附10分钟就可以获得分离富集目的。这样就大大简化了操作手续,缩短了实验流程;为钍的快速测定提供了简便方法。 对含量为0.1％钍的样品,本法15次测定变动系数为3.26％。本方法可测定样品中0.00x—x％钍。 试验部分 一、试剂: 钍的标准溶液:准确称取高纯硝酸钍[Th(NO_3)_4·4H_2O]2.380克,2NHCl加热溶     

用铀试剂Ⅲ光电比色法测定天然原料中的钍

薩卡文曾在1959年合成了铀试剂Ⅲ,并建议用光电比色法测定釷、铀、锆。在著作中提出了于鋯石中不用分离居外元素(包括锆元素)而测定钍的方法。在论文中叙述了在岩石中使钍呈氟化物分出后进行钍的测定。在著作中詳细地阐明了铀试剂Ⅲ与钍的反应操作条件,并提出了用这些试剂以萃取光电比色法测定钍。文章也谈到使钍吸附在阳极上分离后测定少量钍。     

方钍石晶质铀矿单矿物分析

Cl—5208萃淋树脂是中性膦类树脂,具有对铀、钍吸附容量大,水溶性少,流速快等优点。本文研究了用Cl—5208树脂吸附分离铀,钍及其他元素的条件,拟定了采用铂坩埚偏硼酸锂熔矿,ICP—AES和AAS法测定方钍石、晶质铀矿中的钍、铀、铅、铁、铝、钙、镁、钛、锰、钾、钠、硅等12个元素的方法。在本实验条件下,钍60μg/ml、铀40μg/ml均能定量上柱并回收,且与铅20μg/ml、硅10μg/ml、铁、铝、钙、镁8μg/ml、锰、钛4μg/ml定量分离(以上均不是最大试验量)。本法具有取样量少(5mg),操作简便,快速,并适于其它铀钍矿物分析。     

辐射损伤与萤石颜色的初步研究

由于萤石(CaF_2)的钙离子半径(1.06)与钍离子半径(1.10)、特别是与四价铀离子半径(1.05)相似,所以铀和钍常常置换萤石中的钙而进入萤石晶格。此外,铀和钍还能以吸附形式赋存在萤石裂隙中或其表面上,或者成为独立的矿物以固体包体形式存在于萤石中。因此,萤石常含有铀和钍,加之周围岩石中也经常含有放射性元素,从而形成了放射场。萤     

青海西部尕斯库勒盐湖沉积物中铀和钍地球化学特征探讨

文章以柴达木盆地西部尕斯库勒盐湖沉积物为研究对象,通过对钻孔沉积物和地表沉积物中铀和钍含量的研究,探讨了盐湖沉积物中铀和钍的地球化学特征。分析表明,钻孔沉积物中铀和钍之间存在明显的正相关关系。在横向上,随地表取样点逐渐远离湖表卤水,沉积物中铀和钍的含量先增高后又急剧降低,且受补给水铀含量影响大;在纵向上,同一个晶间卤水层或者碎屑物沉积层内铀含量垂直分异明显,铀含量随深度增加而递增。就沉积物中铀和钍的赋存形式而言,2/3的铀被黏土质点吸附,1/3的铀夹杂在盐类矿物中;而90%以上的钍被黏土质点吸附,10%以下的钍夹杂在盐类矿物中。干盐滩中毛细蒸发和淋滤等化学沉积分异作用造成盐湖沉积中心的沉积物铀含量相对较高。     

用萃取色谱法测定地质样品中的铀和钍

本文推荐一种用萃取色谱法测定地质样品中的铀和钍的方法。溶样后，用Fe(OH)3沉淀法预富集铀和钍，再用UTEVA树脂分离，使分离的铀和钍电沉积在不锈钢圆盘上，再用α能谱法测定。用晶质铀矿、珊瑚和花岗岩标准物质评价该法。测得的铀和钍含量及^234U/^238U和^230Th/^234U活性比值与标准值十分一致。发现钚的存在会干扰分离，但利用氨基磺酸亚铁还原就可解决此问题。该法的化学回收率与阴离子交换法相近，但萃取色谱法能用较少试剂进行较快分离。     

TOPO萃取光度法连续测定地球化学样品中的铀和钍

铀、钍在地壳中的含量平均约3ppm至8ppm。地球化学探矿样品一般要求测定低于地壳平均值的含量,如1—2ppm的铀或钍。在一次分离的溶液中测定两个痕量元素是最可取的。Pollock在抗坏血酸存在下以硼酸掩蔽氟,用TOPO(三辛基氧膦)的环己烷溶液一次萃取铀     

An Acetic Acid‐Based Extraction Protocol for the Recovery of U,Th and Pb from Calcium Carbonates for U‐(Th)‐Pb Geochronology

A new method for the simultaneous recovery of U, Th and Pb from ca. 0.5 g calcium carbonate samples for the purpose of U‐(Th)‐Pb geochronometry is presented. The protocol employs ion‐exchange chromatography. Standard anion exchange resin (AG 1‐X8 100–200 mesh) was used as the static phase, and 90% acetic acid was used as the mobile phase to elute the unwanted matrix components; dilute nitric acid was used to elute the U, Th and Pb. Blanks of 1.8 pg Th, 6.4 pg Pb and 8.4 pg U were obtained. The protocol was evaluated by determining the isotopic composition of U‐Th‐Pb separates obtained from an in‐house reference material (prepared from a natural speleothem) by MC‐ICP‐MS. An independently dated speleothem was also reanalysed. Based on these tests, the extraction protocol had an acceptable blank and produced a Pb separate sufficiently free of matrix‐induced instrumental biases to be appropriate for U‐Th‐Pb chronology.     

能谱特征参数与之差异及古铀量计算公式的修正

本文提出并论证了区域性钍铀比计算古铀量时所采用的正确表达式是　，而不是目前人们常用的　，并据此将古铀量计算公式　修正为     

LA-MC-ICP-MS独居石微区原位U-Pb同位素年龄测定

独居石富含U、Th, 同时具有较低的初始普通Pb含量, 是U-Pb和Th-Pb同位素定年的理想对象。由于普遍存在于多种岩石中, 独居石的U-Th-Pb定年具有广阔的应用前景。本文报道利用193 nm ArF准分子激光剥蚀系统和NEPUNE多接收器电感耦合等离子体质谱仪, 对独居石进行微区原位U-Pb同位素年龄测定的新方法。运用这一新方法对独居石样品AL01、BL02和CL03进行微区原位U-Pb同位素年龄测定, 获得AL01和BL02号样品的206Pb/238U年龄加权平均值分别为(288.3±1.1) Ma (n=19)和(446.8±2.3) Ma (n=41); CL03号样品的U-Pb等时线年龄为(396.8±8.8) Ma (n=55), 取得了令人满意的结果。     

Melt generation beneath ocean islands: a U-Th-Ra isotope study from Lanzarote in the Canary Islands

New major and trace element data, and Sr, Nd, Pb, U, Th and Ra isotopes are presented for prehistoric and historic lavas from Lanzarote in the Canary Islands. These rocks are amongst the most primitive found on intraplate ocean islands ranging in composition from basanite to alkali basalt, with MgO contents >9.3% and Mg numbers >67. The youngest are from two of the three 1824 vents, the largest group of samples is from the best known eruption episode, the 1730–36 Timanfaya eruptions, a smaller group of samples are from the northeast Corona region (∼50 ky) and the oldest samples are from the Famara complex and basement massif. The rocks have some of the characteristics of HIMU OIB, including high Ce/Pb, Nb/Ce and low Nb/U and restricted ⁸⁷Sr/⁸⁶Sr (0.70209–0.70332). There is significant ²³⁰Th/²³⁸U disequilibrium (²³⁰Th excesses range from 6–76%) with some of the intermediate silica composition Corona samples showing the greatest disequilibrium. The historic samples exhibit ²²⁶Ra excess. The major and trace element data have undergone fractionation corrections to Mg numbers of 70, requiring <5% olivine fractionation, and these inferred primary compositions are used to evaluate a number of melt generation and mixing models.The fractionation-corrected compositions for the 1824 and the 1730–36 have been modelled as 1–4% melts of a source similar to primitive mantle. However, Yb is incompatible, and so the amounts of residual garnet were < ∼5%, suggesting that there was no significant contribution from garnet pyroxenite source rocks. Rather the REE and the FeO contents are both consistent with melting in the garnet-spinel transition, at depths of 60–70 km. (²³⁰Th/²³⁸U) increases slightly with increasing La/Yb in the younger rocks, and they require some form of dynamic melting model. In the preferred model the upwelling rate is kept constant, and the differences in the degrees of melting are attributed to different lengths of the melt column, with the smaller degree melts being extracted from greater depths. Strikingly, (²²⁶Ra/²³⁰Th) increases with increasing degrees of melting, and so it reflects the time since extraction from the melt column rather than variations in the melting processes. Intra-suite minor and trace element variations are due to magma mixing, and not to progressive changes in the degrees of partial melting, and it is envisaged that such magma mixing occurred during the dynamic melting processes. Dynamic melting at depths of 60–70 km suggests that the regional uplift around the Canary Islands is at least in part due to thermal erosion of the underlying lithosphere.Variations of average Ce/Yb, Tb/Yb, (²³⁰Th/²³⁸U), SiO₂ and lithospheric age for different OIB highlight how the smaller degree melts tend to be generated at greater depths, and the mean pressure of melting increases with the thickness of the lithospheric lid. However, there is no general link between (²³⁰Th/²³⁸U) and the lithospheric age or thickness, and hence the integrated degrees of melting. High buoyancy fluxes result in higher degrees of melting and low (²³⁰Th/²³⁸U) (Chabaux and Allegre, 1994), but for OIB generated within low buoyancy plumes, (²³⁰Th/²³⁸U) and the degrees of melting primarily depend on the depths of melt extraction. Differences in the average composition of low buoyancy OIB depend on the thickness of the overlying lithosphere Ellam 1992, Haase 1996, and the differences within an OIB suite, such as between the 1730-36 and 1824 lavas on Lanzarote, depend on the depth of extraction from the melt column.     

U and Th zonation in Fish Canyon Tuff zircons: Implications for a zircon (U-Th)/He standard

The inability to accurately determine the distribution of U and Th in zircon crystals analysed using (U-Th)/He is a major source of error, and limits the confidence in subsequent data interpretation. The Fish Canyon Tuff (FCT) zircon standard shows (U-Th)/He age reproducibility in excess of ±10%. We have tested the extent to which this is due to U and Th zonation using a combination of cathodoluminescence and ion probe analysis of a population of FCT zircons. Primarily we find that FCT zircons exhibit extreme U and Th zonation, and the population has large inter-crystalline variability. Furthermore, the net cathodoluminescence intensity from the FCT zircons is negatively correlated with U and Th concentration, allowing cathodoluminescence emission to be used as a proxy for U and Th zonation. This correlation was exploited to constrain the U and Th zonation within the crystal population, and to show that the poor age reproducibility of the FCT zircons is consistent with the observed zonation.     

阿尔金奇克山斜长角闪岩同位素年龄及其地球化学特征

阿尔金奇克山地区侵入于地层中的斜长角闪岩原岩为辉长岩,岩石地球化学组成显示斜长角闪岩的SiO_2和Al_2O_3含量较高为49.29%~51.03%和12.27%~14.49%,Na_2O+K_2O含量低为2.35%~4.37%,MgO和Mg~#值为6.48%~10.12%和48.7~59.6,具Eu负异常,样品的MgO对SiO_2、Al_2O_3、TiO_2及Cr-Rb和Rb/Nb-Rb/Zr关系图显示明显相关性,表明其为地幔岩浆经分异演化形成。岩石富集Rb、Th和U,亏损Nb、Sr和P,且Th/Ta为1.05~2.771,Nb/La为0.88~1.02,多小于1,显示岩石在演化过程中受到了地壳轻微混染,推断岩石形成于板内伸展环境。利用LA-ICP-MS微区原位定年获得斜长角闪岩~(206)Pb/~(238)U-~(207)Pb/~(235)U谐和年龄503±5 Ma和~(206)Pb/~(238)U加权平均年龄为479±6 Ma,该年龄段为阿尔金峰期变质阶段,指示岩石形成于479 Ma以前。     

TIMS测定铀矿石样品中^234U/^238U、^230Th/^232Th、^228Ra/^226Ra的方法研究

研究了TIMS测定铀矿石样品中234U/238U、230Th/232Th、228Ra/226Ra的方法。建立了铀矿石密闭混酸一次溶样的方法和采用阴离子、阳离子和Sr特效树脂逐级离子交换分离纯化U、Th和Ra的流程,满足了TIMS测量要求。测定结果表明：100～1000 ng的天然铀中234U/238U,其测量精密度从静态多接收的2.34%提高到动态多接收的0.47%;对230Th与232Th丰度接近、质量为1μg左右的钍,采用三带点样技术和法拉第多接收技术测定230Th/232Th,其内精度平均值为0.0048%,外精度为0.028%;采用单带加钽发射剂,ETP跳峰测定50～100 fg镭-228稀释剂中的228Ra/226Ra,其内精度小于0.10%,外精度小于0.20%。比较TIMS和HR-ICP-MS、α能谱法测定234U/238U、230Th/232Th、228Ra/226Ra结果,三者结果相吻合。TIMS测量法样品用量少、快速、准确、精密度高,是U、Th、Ra同位素比值测定方法的又一补充。     

Understanding melt generation beneath the slow-spreading Kolbeinsey Ridge using U, Th, and Pa excesses

To examine the petrogenesis and sources of basalts from the Kolbeinsey Ridge, one of the shallowest locations along the global ridge system, we present new measurements of Nd, Sr, Hf, and Pb isotopes and U-series disequilibria on 32 axial basalts. Young Kolbeinsey basalts (full-spreading rate = 1.8 cm/yr; 67°05′-70°26′N) display (²³⁰Th/²³⁸U) < 1 and (²³⁰Th/²³⁸U) > 1 with (²³⁰Th/²³⁸U) from 0.95 to 1.30 and have low U (11.3-65.6 ppb) and Th (33.0 ppb-2.40 ppm) concentrations. Except for characteristic isotopic enrichment near the Jan Mayen region, the otherwise depleted Kolbeinsey basalts (e.g. ⁸⁷Sr/⁸⁶Sr = 0.70272-0.70301, ε_Nd = 8.4-10.5, ε_Hf = 15.4-19.6 (La/Yb)_N = 0.28-0.84) encompass a narrow range of (²³⁰Th/²³²Th) (1.20-1.32) over a large range in (²³⁸U/²³²Th) (0.94-1.32), producing a horizontal array on a (²³⁰Th/²³²Th) vs. (²³⁸U/²³²Th) diagram and a large variation in (²³⁰Th/²³⁸U). However, the (²³⁰Th/²³⁸U) of the Kolbeinsey Ridge basalts (0.96-1.30) are inversely correlated with (²³⁴U/²³⁸U) (1.001-1.031). Samples with low (²³⁰Th/²³⁸U) and elevated (²³⁴U/²³⁸U) reflect alteration by seawater or seawater-derived materials. The unaltered Kolbeinsey lavas with equilibrium ²³⁴U/²³⁸U have high (²³⁰Th/²³⁸U) values (?1.2), which are consistent with melting in the presence of garnet. This is in keeping with the thick crust and anomalously shallow axial depth for the Kolbeinsey Ridge, which is thought to be the product of large degrees of melting in a long melt column. A time-dependent, dynamic melting scenario involving a long, slowly upwelling melting column that initiates well within the garnet peridotite stability zone can, in general, reproduce the (²³⁰Th/²³⁸U) and (²³¹Pa/²³⁵U) ratios in uncontaminated Kolbeinsey lavas, but low (²³¹Pa/²³⁵U) ratios in Eggvin Bank samples suggest eclogite involvement in the source for that ridge segment.     

ICP测定地质样品中的痕量稀土元素

岩石中痕量稀土元素的含量与配分,是研究岩石成因、形成条件、演化过程以及岩石分类的重要依据,因此要求以痕量级的精密度和准确性来测定稀土元素,用常规方法测定稀土元素是不能满足这个要求的,然而电感耦合等离子体发射光谱法却是目前测定痕量稀土元素中的一种比较理想的手段。我们在原工作的基础上,改用小型离子交换柱,仪器采用法国Jobin Yvon公司的Jy38型单道扫描光电直读光谱仪,经选用