ICP-AES测定葡萄糖酸钙中Pb、As、Cd等9个杂质元素

本文应用ICP-AES直接测定了葡萄糖酸钙中的Pb、As、Cd等9个杂质元素,对样品的消解方法、基体和酸介质的影响等进行了讨论.用基体匹配法消除钙基体的干扰,9个杂质元素测定的测定范围为:Pb 0.0008%-0.08%,Cu、Mg 0.0001%-0.01%,其余元素0.0003%-0.03%.加标回收率为95.8%-100.0%,相对标准偏差为0.16%-3.61%.     

沉淀法制备EPDM-g-MAH/CaCO_3复合材料及其性能的表征

提供了三元乙丙橡胶(EPDM)交联的一种方法.以二甲苯为溶剂,溶液法制备马来酸酐(MAH)接枝EPDM,然后向溶液中加入适量碳酸钙(CaCO3),与已接枝的马来酸酐(MAH)反应.待反应完全后,滴加丙酮作为沉淀剂,沉淀物真空干燥,制得EPDM-g-MAH/CaCO3弹性体复合材料.溶解、溶胀及拉伸性能测试结果表明,复合材料样品已形成有效的交联,且材料的抗张强度、断裂伸长率和模量均得到较大幅度的提高,当CaCO3含量达到体系总重的20%时,复合材料呈现最佳力学性能.上述实验结果是因为碱性的CaCO3的Ca2+可以与接枝在EPDM上的MAH发生配合反应,进而成为EPDM的交联中心,形成有效交联,从而促进了EPDM机械性能的提高,ATR-FTIR和TGA的测试结果被用于证实上述观点.     

蟹,虾壳微观形貌与结构研究

用Ｘ射线衍射与扫描电镜研究了蟹壳，虾壳的形貌与微观结构，蟹壳中以方解石晶型存在的碳酸钙分布在网状结构的有机质中，网孔的尺寸约５～２５μｍ有机基质脱去蛋白后留下的甲壳质呈片层状结构，它的重复距离为０．９６ｎｍ。     

Mixed ligand complexes of AEE hexafluoroacetylacetonates with diglyme: Synthesis,crystal structure and thermal behavior

The novel mixed ligand complexes [Ca(hfa)₂(diglyme)(H₂O)] (I), [Sr(hfa)₂(diglyme)(H₂O)] (II) and [Ba(hfa)₂(diglyme)₂] (III) (Hhfa = 1,1,1,5,5,5-hexafluoropentane-2,4-dione, diglyme = 2,5,8-trioxanonane) were synthesized by the reactions of the alkaline earth element (AEE) carbonates in n-hexane with a mixture of Hhfa and diglyme, and they were characterized by elemental analysis, ¹H and ¹³C NMR, and FTIR spectroscopy. The crystal structures of I–III, consisting of mononuclear isolated molecules, have been determined. The thermal behavior and composition of the vapor phase have been studied for I–III by thermal analysis at low pressure and mass spectrometry using a Knudsen cell. The stability of the mixed ligand complexes [M(hfa)₂(diglyme)_n] to the removal of diglyme molecules under heating decreases in the row I > II ≈ III, and only I evaporates as the mixed ligand complex after water removal.     

Improved Calcium Ion-Selective Electrode Based on a Neutral Carrier

Abstract

The performance of a liquid-membrane electrode using a synthetic, neutral carrier in o-nitro-phenyl-n-octyl-ether as membrane component in a PVC matrix, in the presence of sodium tetra-phenyl-borate, is described. Selectivities, working range, lifetime and anion interference are discussed. The electrode makes possible the measurement of calcium ion activities in the range 10^?1M to 10^?6M in unbuffered and in the range 10^?1M to 10^?8M in calcium buffered systems respectively. The selectivities of calcium over protons, magnesium, sodium and zinc are 25,000, 26,000, 2,800 and 7,100, respectively, and are far superior than those reported for other calcium sensors.     

烷基苯磺酸盐表面活性剂对水合硅酸钙形貌和结构的影响

利用十二烷基苯磺酸钠(SDBS)为模板剂, 研究了SDBS的浓度、 Ca ²⁺和Si {\mathrm{O}}_3^{2-} 离子的浓度、 是否搅拌和反应时间等条件对水合硅酸钙(CSH)形貌特征和分散性能的影响, 并提出了不同CSH球壳形貌特征的形成机理. 结果显示, 溶液中Na₂SiO₃·9H₂O浓度增大、 SDBS浓度增大及反应时间延长均会使CSH的结晶度变好, 聚合度增大, Q ²结构的相对含量增加, 其中Na₂SiO₃·9H₂O和SDBS浓度是主要控制因素. SDBS在溶液中形成的球形胶束具有极强的模板作用, 能有效改变CSH的结晶生长方式; 通过调节SDBS浓度和钙硅比例, 并适当延长CSH的生长时间, 能够获得球壳完整、 分散性好且稳定性强的CSH.     

花椰菜状碳酸钙的"一步法"制备及表征

以碱土金属锶的硝酸盐为添加剂, 采用“一步法”制备了大小均一、 分散性良好的花椰菜状碳酸钙粒子. 考察了反应温度、 反应时间等因素对碳酸钙结晶行为的影响, 确定了最佳反应条件. 利用扫描电子显微镜(SEM)、 X射线衍射仪(XRD)、 X射线能谱仪(EDAX)等对所得产物的结构和性能进行了表征, 并探讨了其反应原理.     

High-field MRS studies in brain slices

We are applying multi-nuclear high-field (500 MHz) MR spectroscopy of metabolising whole tissue preparations of the mammalian brain to studies on individual components of convulsions, which include prolonged depolarization, metabolic deprivation, and the effects of excitotoxins. The responses of glial cells and neurones can be partially distinguished by following labelling patterns of metabolic intermediates from ¹³C-labelled glucose or acetate (which enters only glial cells). This approach clearly confirmed our earlier indications that the metabolic response to depolarization (40 mM extracellular K⁺) occurs essentially in glial cells. Some evidence for metabolic shuttling between glia and neurones was obtained from the changes in C3/C4 ratios of glutamate and glutamine, and the C2/C3 of GABA. Mechanisms for metabolic support of neurones by glia may be of importance in neuronal protection under such metabolic stress as occurs in epilepsy. Changes in free intracellular divalent cations ([Ca²⁺]_i and [Zn²⁺]_i) were monitored using the ¹⁹F-MRS indicator, 5FBAPTA. Large increases in [Ca²⁺]_i and decreases in PCr were produced by excitotoxins (glutamate and NMDA), depolarization or ischaemia, but intracellular Zn²⁺ appeared only after exposure to the excitotoxins. The NMDA receptor blocker, MK801, removed all of the responses to NMDA, but only prevented the appearance of Zn²⁺ observed with glutamate. These results indicate that the damage caused to neurones by such insults as convulsions is not due simply to the presence of excessive excitotoxic glutamate.     

草酸钙结石形态的红外光谱分析

草酸钙结石主要是以一水草酸钙(COM)、二水草酸钙(COD)的形式存在。在解决缺少COD标样的难题后,将制备的COD样品与COM标样混合,然后采用红外光谱法对混合物进行分析研究,采用谱带比值法,确定了COD和COM在660和610 cm-1处与780和520 cm-1处的吸收度比值(R)与质量分数(w)的关系式,其线性回归方程分别为:R=11.95×10-3wCOD 0.873 61,r=0.983 63;R=4.74×10-3wCOD 0.886 52,r=0.992 44。同时为了减少压片、测定等因素引起的误差,采用零点交叉一阶导数法,测定在1 320 cm-1处吸收度一阶导数与COD质量分数(w)的关系式,其线性回归方程I=5.5×10-5w 9.2×10-5,r=0.996 60。线性良好。     

火焰原子吸收和发射光谱法测定盐湖卤水中的钙

在波长422.7nm下,用火焰原子吸收和发射光谱法测定了盐湖卤水中钙的含量,考察了酸度及共存离子对测定结果的影响,并对两种方法的优缺点进行了比较.结果表明,原子吸收光谱法受酸度及共存离子的影响较小,火焰发射光谱法测定钙的灵敏度比原子吸收光谱法高,两种方法的RSD均小于2%,加标回收率介于103.7%-107.2%.