New Reference Materials and Assessment of Matrix Effects for SIMS Measurements of Oxygen Isotopes in Garnet

Accurate ion microprobe analysis of oxygen isotope ratios in garnet requires appropriate reference materials to correct for instrumental mass fractionation that partly depends on the garnet chemistry (matrix effect). The matrix effect correlated with grossular, spessartine and andradite components was characterised for the Cameca IMS 1280HR at the SwissSIMS laboratory based on sixteen reference garnet samples. The correlations fit a second‐degree polynomial with maximum bias of ca. 4‰, 2‰ and 8‰, respectively. While the grossular composition range 0–25% is adequately covered by available reference materials, there is a paucity of them for intermediate compositions. We characterise three new garnet reference materials GRS2, GRS‐JH2 and CAP02 with a grossular content of 88.3 ± 1.2% (2s), 83.3 ± 0.8% and 32.5 ± 3.0%, respectively. Their micro scale homogeneity in oxygen isotope composition was evaluated by multiple SIMS sessions. The reference δ¹⁸O value was determined by CO₂ laser fluorination (δ¹⁸O_LF). GRS2 has δ¹⁸O_LF = 8.01 ± 0.10‰ (2s) and repeatability within each SIMS session of 0.30–0.60‰ (2s), GRS‐JH2 has δ¹⁸O_LF = 18.70 ± 0.08‰ and repeatability of 0.24–0.42‰ and CAP02 has δ¹⁸O_LF = 4.64 ± 0.16‰ and repeatability of 0.40–0.46‰.     

离子色谱法检测土壤样品水溶态中的七种阴离子

采用离子色谱法测定土壤样品水溶态中的F^-、Cl^-、NO2^-、SO4^2-、Br^-、NO3^-、PO4^3-。通过优化提取条件,得出最优条件下7种阴离子的加标回收率为94.4%～102.5%,精密度为3.1%～4.6%。对实际样品进行测试,结果表明,该方法适用于土壤样品水溶态中7种阴离子的定性、定量分析。     

4A沸石吸附模拟核素Sr,Cs后的组分变化和结构表征

通过4A沸石吸附模拟核素Sr,Cs前后的化学成分分析、X衍射分析和红外光谱分析等手段方法,分析探讨了模拟核紊Sr,Cs在4A沸石的赋存状态,结果表明：4A沸石与模拟核素Sr,Cs之间主要以离子交换的方式发生作用,Sr^2 ,Cs^ 取代4A沸石中的可交换离子Na^ ,占据4A沸石a笼中的6元环和8元环。导致4A沸石的晶胞参数增大,晶格发生畸变。     

C10TAB,C14TAB,C18TAB柱撑蒙脱石层间域有机柱排布研究

用十烷基三甲基溴化铵（C10TAB）、十四烷基三甲基溴化铵（C14TAB）和十八烷基三甲基溴化铵（C18TAB）制备有机柱撑蒙脱石,并对产物进行X射线衍射表征。研究结果表明：柱化剂的浓度和烷基季铵离子的性质能影响烷基季铵离子在蒙脱石层间的排布模式。在柱化剂浓度较低时易形成平卧排列,柱化剂达到一定浓度时石蜡型结构方能形成,且直链烷基越长,烷基季铵离子在蒙脱石层问越易形成石蜡型倾斜排列。在平卧结构向石蜡型结构转化过程中可出现多种排列共存。     

Inter‐laboratory Characterisation of Apatite Reference Materials for Chlorine Isotope Analysis

Here we report on a set of six apatite reference materials (chlorapatites MGMH#133648, TUBAF#38 and fluorapatites MGMH#128441A, TUBAF#37, 40, 50) which we have characterised for their chlorine isotope ratios; these RMs span a range of Cl mass fractions within the apatite Ca₁₀(PO₄)₆(F,Cl,OH)₂ solid solution series. Numerous apatite specimens, obtained from mineralogical collections, were initially screened for ³⁷Cl/³⁵Cl homogeneity using SIMS followed by δ³⁷Cl characterisation by gas source mass spectrometry using both dual‐inlet and continuous‐flow modes. We also report major and key trace element compositions as determined by EPMA. The repeatability of our SIMS results was better than ± 0.10‰ (1s) for the five samples with > 0.5 % m/m Cl and ± 0.19‰ (1s) for the low Cl abundance material (0.27% m/m). We also observed a small, but significant crystal orientation effect of 0.38‰ between the mean ³⁷Cl/³⁵Cl ratios measured on three oriented apatite fragments. Furthermore, the results of GS‐IRMS analyses show small but systematic offset of δ³⁷Cl_SMOC values between the three laboratories. Nonetheless, all studied samples have comparable chlorine isotope compositions, with mean 10³δ³⁷Cl_SMOC values between +0.09 and +0.42 and in all cases with 1s ≤ ± 0.25.     

配位滴定法同时测定金属离子浓度的研究

将多元校正分析法应用于配位滴定中，以ＥＤＴＡ为滴定剂，玻璃电极为指示电极，饱和甘汞电极为参比电极。依据电位滴定原理，对混合三组分：Ｃｕ￣（２＋）、Ｃｄ￣（２＋）、Ｚｎ￣（２＋）、及Ｃｕ￣（２＋）、ＣＯ￣（２＋）、Ｎｉ￣（２＋）进行测定，各金属离子之间的△ｌｏｇＫ在０．０４～２．３４之间，计算误差一般小于土１０％。     

海洋钙离子非保守行为及海洋钙问题

钙离子是海洋11种常量离子之一,与钠、钾等离子的保守性不同,钙离子在海洋中的分布表现出微小但系统的变化。钙离子的变化往往与海洋碳酸钙的形成和溶解过程有关,所以,钙离子可直接指示海洋碳酸钙通量（深层海洋碳通量的主要组成部分）。同时,碳酸钙沉淀或溶解又会改变总碱度和溶解无机碳,通过钙离子变化也能间接探讨海洋碳酸盐系统和海洋吸收CO2的能力。介绍了以碳酸钙溶解形成超额钙为主的海洋钙离子多种非保守行为及其控制过程,讨论这些过程对海水组成和海洋碳酸盐系统的影响,探讨未来海洋酸化条件下钙离子可能的变化及其潜在的效应,最后展望在南海开展钙离子精细行为的研究意义。      

渤海湾盆地石炭纪-二叠纪煤中基质镜质体飞行时间二次离子质谱研究

利用飞行时间二次离子质谱仪（简称ＴＯＦ－ＳＩＭＳ）对渤海湾地区Ｃ－Ｐ太原组和山西组煤中基质镜质体进行了对比研究,结果表明,在接收到的正二次离子中都含有一定的烯基和烷基碎片,这些脂族碎片离子的出现说明它们具有富氢及较好的生烃性质。同时,该仪器的实际应用结果表明,它对研究煤及源岩中有机显微组分的化学成分和结构具有独特的优势。     

柱撑粘土矿物的研究新进展——新矿物材料研究综述之一

柱撑粘土矿物作为一种大层间距的多酸型层柱微孔材料,是一种性能优异的催化剂和吸附剂,本文在较全面分析前人资料的基础上,结合笔者所做的工作,对柱撑粘土矿物的制备性能表征及其应用最新研究进展进行综述与展望。     

离子质谱计测定地质样品中镁同位素组成方法学研究

应用信通公司研制的离子质谱计（ＳＴ－ＩＭＳ），建立了地质样品镁同位素分析的实验流程和误差分析方法，为进一步分析微量地质样品中镁同位素组成和分布奠定了基础。