电感耦合等离子体质谱法测定岩石样品中的锆铌铪钽两种预处理方法的比较

研究了微波消解酸溶和过氧化钠碱熔两种测定岩石样品中锆、铌、铪、钽前处理方法,利用电感耦合等离子体质谱法进行测定。对所选用不同种类的岩石国家标准物质样品进行了条件实验,结果表明:采用过氧化钠碱熔法处理岩石样品后,锆、铌、铪、钽的测量值准确度高,且相对标准偏差(RSD,n=10)小于6%,该方法更适用于岩石样品中锆、铌、铪、钽的测定。     

原子荧光光谱测定土壤和水系沉积物中硒的干扰来源及消除方法

原子荧光光谱法(AFS)具有灵敏度高、结构简单、容易操作等优点,但目前测定土壤和沉积物中的硒等元素的标准方法所采用的消解过程繁琐,易产生干扰。沸水浴可以把土壤和水系沉积物中硒提取完全,本文根据样品中元素丰度和仪器性能,将AFS测定Se的干扰分为Cu和Pb两大类,根据实验提出在水浴消解液加入浓盐酸(不宜加入硫脲-抗坏血酸),通过增加溶液酸度和Cl~-浓度,即保持样品中盐酸浓度高于23%,可抑制Cu~(2+)还原为Cu~0和Pb~(4+)生成PbH_4,有效降低了Cu的负干扰和Pb的正干扰,提高了AFS测定Se的精密度和准确度。本方法测定Se的检出限为0.008mg/kg,测试标准物质的相对标准偏差为0.5%～11%,相对误差为-16.3%～9.5%;比行业标准HJ 680—2013的检出限(0.01mg/kg)、精密度(0.79%～23.1%)和准确度等技术指标更佳。     

Comment on: Mass Fractions of Forty‐Six Major and Trace Elements,Including Rare Earth Elements,in Sediment and Soil Reference Materials Used in Environmental Studies. Fiket et al. (2017), Geostandards and Geoanalytical Research, 41, 123–135

This paper is intended to be a constructive discussion of Fiket et al. (2017, Geostandards and Geoanalytical Research , 41 , 123–135), who dealt with the determination of major, trace and rare earth elements in several sediment and soil certified reference materials. In the present author's view, the paper by Fiket et al. (2017) suffers from a lack of reference to several publications in which somewhat similar results had already been reported. The present contribution therefore provides a comparison of previously published results with those of Fiket et al. for the CRMs soil NCS DC 77302 (GBW 07410), stream sediment NCS DC 73309 (GBW 07311), marine sediments MESS‐3 and NCS DC 75301 (GBW 07314) and estuarine sediment IAEA‐405. It is argued that this fuller consideration (a) allows critical evaluation of the quality of the results presented by Fiket et al. and (b) highlights the advantages of their work. Finally, attention is drawn to the (possible or real) problems that can arise during simultaneous determination of multiple trace elements.     

ROCKS & MINERALS DETERMINATION AND ANALYSIS

正20141456 Chen Juan(Laboratory of High Temperature and High Pressure Study of the Earth’s Interior,Institute of Geochemistry,Chinese Academy of Sciences,Guiyang550002,China);Tang Hongfeng Progress in Analytical Methods of Tungsten Isotope and Experimental Research on Digestion of Whole     

Effects of the peat acid digestion protocol on geochemically and morphologically diverse tephra deposits

Tephra shards for electron probe microanalysis are most efficiently extracted from peat using acid digestion, which removes organic material that hinders density separation methods. However, strong acids are known to alter glass chemical compositions, and several studies have examined how acid digestion affects rhyolitic volcanic glass. The focus on rhyolitic tephra in these studies leaves considerable uncertainty, as the dissolution rates of natural glasses (including tephra) are determined by the chemical composition and surface area/volume ratio, both of which vary in tephra deposits. Here, we use duplicate samples of basaltic, trachydacitic and rhyolitic tephra to examine physical and geochemical alteration following acid digestion. Scanning electron microscope imagery reveals no discernible degradation of glass surfaces, and electron probe microanalysis results from duplicate samples are statistically indistinguishable. These findings suggest the acid digestion protocol for organic peats does not significantly alter glass geochemistry regardless of shard morphologies or geochemical compositions.     

水准网闭合差自动解算的新方法

介绍一种在水准测量中独立闭合环或附合路线自动搜索及闭合差自动解算的新方法。该方法将间接平差函数模型转化为条件平差函数模型,利用条件方程式的所有信息,搜索出独立闭合环或附合路线并快速解算出闭合差,与给定的限差进行比较,较好地检验并剔除粗差。最后经过编程实现该方法,用实例验证了该方法的正确性和用之进行观测值质量检核的有效性。     

磷矿中P2O5的快速测定

本文用自行设计的一种简易,安全的聚四氟乙烯溶样罐,与新型,高效的微波溶样技术相结合,进行磷矿的分解,溶样时间仅需２ｍｉｎ,并首次将该技术与流动注射一分光光度法联用,测定其中Ｐ２Ｏ２质量分数,结果准确,可靠,实现了从溶样到测定的一套快速分析方法。     

埋设地下光缆对武都地电影响的分析

着重探讨武都地电台测区埋设地下光缆后北西道地电阻率测值急剧上升的原因.通过实际观测、理论分析和实验,总结出了这种变化的机制,定量地解释了埋设地下光缆对地电观测的影响,从而为以后判断地电测值变化是干扰还是地震异常提供了依据.     

Comparative Assessment of Sludge Pre‐Treatment Techniques to Enhance Sludge Dewaterability and Biogas Production

Effectiveness of ultrasonication, microwave technologies, and enzyme addition prior to anaerobic digestion is investigated using sludge samples taken from the secondary settling tank of a domestic wastewater treatment plant to improve methane production, enhance dewaterability characteristics of the sludge, and to reduce excess sludge. Microwave pre‐treatment (1500 W, 10 min at 175 °C) results in better extra digester performance (compared to the control reactor) in terms of methane production (25 m³ ton^?1 suspended solids (SS)) than ultrasound (no improvement) and enzyme pre‐treatment (11 m³ ton^?1 SS). While methane production is not improved as a result of ultrasonication pre‐treatment (15 000 kJ kg^?1 SS), a noticeable increase (19%) is observed in the case of microwave pre‐treatment. Higher compactibility values are obtained after ultrasonication and microwave application compared to the control (i.e., from 7.1 to 8.7 and 9.2%, respectively) before anaerobic digestion. Although ultrasonication and microwave application decrease the dewaterability of the raw sludge (capillary suction time (CST) from 827 to 1364 and 2290 s, respectively), similar dewaterability results are obtained at the end of the anaerobic digestion process for all pre‐treated sludge samples. An economic assessment of this study shows that pre‐treatment with microwave results in more than 10‐fold less net cost compared to the enzyme application.     

低压密闭消解-电感耦合等离子体发射光谱法测定地质样品中的硼

采用酸溶-电感耦合等离子体发射光谱法(ICP-OES)测定地质样品中的全硼量,关键环节在于如何防止样品消解过程中硼元素的损失,降低测量过程中的基体干扰、光谱干扰和记忆效应。基于以上问题,本文采用氢氟酸-硝酸-高氯酸-磷酸在低压密闭溶样罐中消解样品,溶出的硼元素与少量磷酸充分络合,防止硼的挥发损失;以基体及主成分浓度与样品相类似的地质类固体标准物质绘制标准曲线做线性校准,有效匹配和降低样品的基体干扰;采用仪器自带的操作软件,观察分析谱线附近是否存在其他元素的干扰,来确定背景扣除最佳的位置及宽度,降低ICP-OES测量中的光谱干扰;以10%的王水作为进样系统的冲洗液,有效消减测量过程中的记忆效应。当稀释因子为200时,方法的检出限(3SD)为1.2μg/g,定量限(10SD)为4.0μg/g;用岩石、土壤及水系沉积物国家一级标准物质对精密度及准确度进行分析验证,11次测定相对标准偏差为1.8%～7.9%,相对误差为-3.6%～6.3%;以外检分析结果为参考,对硼含量在定量限以上的样品测定,相对误差为-9.3%～12.5%。