Precise and Accurate Doping of Nanoporous Silica Gel for the Synthesis of Trace Element Microanalytical Reference Materials          下载免费PDF全文

William O. Nachlas 《Geostandards and Geoanalytical Research》2016,40(4):505-516

This study presents an experimental procedure to fabricate high‐purity silica glass containing a selected element at a specified mass fraction. The procedure was used to prepare glasses doped with trace‐level mass fractions of Ti with the goal of improving analytical confidence when measuring trace elements in quartz. Systematic tests were performed to determine the ideal conditions and procedures for doping nanoporous silica gel with the highest efficiency of dopant recovery. Silica gel was cleaned in concentrated HCl, immersed in a non‐polar doping medium at a controlled pH and doped with precise quantities of ICP‐MS standard solution. Using liquids composed of longer chain molecules as the doping medium diminishes recovery, suggesting that large molecules could obstruct nanopores to inhibit capillary uptake of the dopant. A control experiment using crystalline quartz reinforced the effectiveness of nanoporous silica gel for doping with trace‐level precision. Layered aggregates of silica gel doped with different Ti mass fractions were hot‐pressed to create multi‐layered reference materials that were analysed with multiple techniques at a variety of spatial scales. Analyses at the intra‐grain scale (cathodoluminescence scanning electron microscopy, electron probe microanalysis), at the single grain scale (SIMS), at the sample layer scale (EPMA, laser ablation‐ICP‐MS) and at the bulk scale (ICP‐OES) demonstrated acceptable homogeneity at sample volumes characteristic of most microanalysis techniques and show that nanoporous silica gel holds promise as a highly retentive doping substrate for preparing reference materials for laser‐, electron‐ and ion‐beam microanalysis.  相似文献   

胶州湾沉积物-海水界面硅的交换速率及其影响因素探讨   总被引：2，自引：1，他引：1  

汪雅露  袁华茂  宋金明  李学刚  李宁  曲宝晓  康绪明  王启栋  邢建伟  梁宪萌 《海洋学报》2016,38(12):55-65

采用实验室培养法在原位温度和溶氧条件下测定了胶州湾沉积物-海水界面硅的交换速率,并探讨了相关环境因子对界面交换速率的影响机制。结果表明,胶州湾沉积物-海水界面硅的交换表现为从沉积物向水体释放,其交换速率在947~4 889 μmol/（m2·d）范围内,平均速率为1 819 μmol/（m2·d）。表层沉积物中叶绿素a（Chl a）和总有机碳（TOC）是影响胶州湾沉积物-海水界面硅交换速率的主要环境因子,同时表层沉积物的含水率（φ）、生源硅（BSi）和粘土含量以及间隙水中溶解硅酸盐（DSi）对沉积物-海水界面硅的交换也有重要影响。由此可推知,胶州湾沉积物-海水界面硅的交换速率主要受生物活动和溶解-扩散双重过程调控,而表层沉积物粒度与底层水体中DSi对胶州湾硅的释放影响较小。  相似文献   

Nutrient Cycling and a Stoichiometric Model in Epidavros, a Deep Basin in the Aegean Sea     

Nicholas  Friugos 《Marine Ecology》1986,7(1):43-57

Abstract. The nutrient cycling of Epidavros, a deep basin in the Saronikos Gulf, was studied in relation to various environmental factors during 1973–1976 at a station characterized by stagnant conditions. The regeneration of nutrients was related to the consumption of oxygen, and a seasonal nutrient cycle occurred with low nutrient concentrations in the spring and summer, followed by high nutrient levels in autumn and winter. In addition high values of nitrate and silicate were observed in the deeper waters, which tended to be anoxic, although the water masses were renewed during spring 1974. The distribution pattern of nutrients together with nutrient ratios were compared with previous studies of the same and neighbouring areas as well as of other isolated basins. A stoichiometric model indicates that plankton organisms in the Epidavros basin have approximate atomic ratios for C: N: P of 150: 14:1, while the ratio of change for nitrogen and phosphorus in the water is only 8.8:1 by atoms. This is probably because of the slow rate of regeneration of nitrogenous material and/or assimilation and regeneration in organic forms. The water/plankton relation in the Epidavros basin appears to be very similar to that in the Baltic Sea.  相似文献   

藻酸双酯钠粘度的影响因素     

万忠良 《中国海洋大学学报(自然科学版)》1992,(Z1)

通过实验讨论影响藻酸双酯钠特性粘度[η]升降的几个因素。  相似文献   

Marine diatom Thalassirosira weissflogii nutrient drawdown and its physiological status variation challenged to zinc and cadmium exposure     

LI Chundi  LONG Aimin  YAN Wen  MA Fujun  CHEN Shaoyong 《海洋学报(英文版)》2007,26(6):51-61

The uptake of zinc and cadmium by a species of marine diatom Thalassirosira weissflogii and the nutrient variation (phosphorus and silicon) in the culture medium were estimated when exposed to zinc and cadmium stress under controlled laboratory conditions.It was found that low cadmium addition could stimulate the culture to grow with a relatively high rate and exert its toxicity at the elevated concentration.The cellular uptake of zinc and cadmium by the diatom varied in the ranges of 1.21~3.75 and 0.060~0.629 fmol per cell respectively in the whole cultivation period.The mean cellular phosphorus and silicon drawdowns were constant with 0.26~0.42 and 0.30~0.46 pmol per cell respectively in those healthy cultures.It is illustrated that the algal cells can adjust some physiological mechanisms to decrease metal accumulation and keep metal homeostasis in the organism.The correlation analysis results further indicate that the cellular cadmium uptake might be closely related with the cellular phosphorus, silicon drawdown and the growth rate of diatom (P<0.05, 0.001, 0.01); and the cultures grow better in good conditions, the lower amount of phosphorus, silicon materials are consumed by a single cell to keep a high efficiency of utilization.  相似文献   

稻壳灰作为海水硅酸盐肥料的肥效和安全性研究     

吕静静  张光涛 《海洋科学》2019,43(7):53-60

增加硅酸盐供给可缓解海域硅酸盐相对缺乏现象,稻壳灰中含有大量无定形态SiO2,是一种理想的海水硅酸盐肥料。为验证稻壳灰的硅酸盐释放性能以及在环境中应用时的安全性,我们在实验室内将稻壳灰添加到海水中测定了Si、P、N营养盐的释放能力及释放周期,并将稻壳灰放于自然海域浸泡一段时间后测定其4种重金属及Mg元素含量的变化。实验结果表明,稻壳灰在海水中可持续缓慢地释放硅酸盐,释放周期可达3个月以上,同时释放少量磷酸盐,不会增加水体中无机氮营养盐含量;稻壳灰向海水中释放极少量的Cd,但不易造成重金属污染,而对海水中的Cu、Pb、Hg有一定地吸附效果,吸附量远小于Mg离子。  相似文献   

高平4水平井组双保钻井液技术     

胡祖彪  骆胜伟  孟凡金  陈秉炜  石仲元  金虎 《海洋地质译丛》2009,(1):110-115

高平4井组水平井主要用于开发安塞长10组油藏。针对该井组上部直罗组和富县组易坍塌、下部地层钻速相对较慢、地层易造浆的特点，研究应用了环保型聚硅酸盐-黄胞胶钻井液体系。该体系具有抑制性强、润滑和剪切稀释性好的特点，有利于安全快速钻井，对环境污染极小。通过小型配浆实验确定钻井液施工方案，中测后稀释钻井液，降低钻井液滤失量和密度，加强固相控制，使用保护油层的酸溶性暂堵剂和降滤失剂，可最大限度地保护油层。  相似文献   

Colorimetric determination of nanomolar concentrations of silicate in natural waters after liquid-liquid extraction using methyl isobutyl ketone     

REN Jingling  MI Tiezhu  DOU Weiwei  LIU Sumei  ZHANG Jing 《海洋学报(英文版)》2008,27(1):137-146

A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.  相似文献   

地质样品中硫化物形式铁的分离和测定   总被引：1，自引：0，他引：1  

周佳琦  胡超涌  马仲武  谢树成 《海洋地质与第四纪地质》2010,(2)

提出一个利用次氯酸钠氧化铁硫化物碱性磺基水杨酸提取并直接测定碳酸盐相中铁硫化物的方法。结果表明,30%的NaClO溶液浸泡样品40h以上,可以完全释放铁硫化物并形成氢氧化铁胶体。0.1g/mL的碱性磺基水杨酸溶液则较容易地溶解新生成的氢氧化铁胶体,形成黄色的铁-磺基水杨酸络合物,可被分光光度法定量测定。该方法集选择性分离、富集和测定于一体,分析流程简单,结果可靠,适合地质样品中硫化物形式铁的测定。  相似文献   

过硫酸钠修复土壤中多环芳烃的准确测定     

杨清 《岩矿测试》2022,(3):404-411

多环芳烃(PAHs)是一类具有致癌、致突变、致畸的碳氢化合物,具有较高的辛醇-水分配系数,易被土壤颗粒吸附而影响环境和人体健康。过硫酸钠(Na₂S₂O₈)氧化法是近些年来国内外修复PAHs污染土壤较为常用的方法,但现阶段在测定修复后土壤中PAHs含量、进行土壤修复效果评估时亟待解决的问题是：经该方法修复的土壤,若土壤中残留有过硫酸钠,在样品前处理过程中由于提取温度较高,可能会进一步加速多环芳烃的氧化反应,从而影响土壤中PAHs的准确测定。本文建立了一种在修复后土壤中加入还原剂抗坏血酸,与残留的过硫酸钠反应生成脱氢抗坏血酸,采用索氏提取结合气相色谱-质谱法(GC-MS)同时测定土壤中16种PAHs的方法,PAHs加标回收率为76.2%～110.0%。而修复后土壤若不加还原剂直接进行索氏提取,用GC-MS测定,可能会使部分PAHs及替代物的测定不准确,PAHs加标回收率仅为6.0%～72.4%。通过对比分析表明,在样品提取前加入还原剂,可以有效地消除残留过硫酸钠的影响,提高测定修复后土壤中PAHs含量的准确性。  相似文献