ICP-MS同时测定土壤样品中的镓铟锗

建立了测定土壤样品中镓铟锗元素的ICP-MS方法,电感耦合等离子体质谱仪(ICP-MS)具有灵敏度高、干扰少、可同时进行多元素分析等优点,现已广泛应用于不同领域各种类型样品中痕量元素的分析测定。试样加入硝酸、氢氟酸,在微波消解仪中进行消解,取出后在电热板上蒸干,1+1硝酸提取使待测元素完全溶解,以Rh元素作为内标校正干扰,电感耦合等离子体质谱仪(ICP-MS)测定样品中镓铟锗元素。方法的检出限为Ga0.03 ug/g、In0.01 ug/g、Ge0.05ug/g,精密度优于5%。整个方法检出限低、简单、快速和准确,经过国家一级地球化学标准物质的分析验证,结果与标准值吻合。     

ICP-MS测定植物样品中痕量硒

采用电感耦合等离子体质谱（ICP-MS）的KED技术,对植物中痕量硒进行了分析研究,实现了准确快速地测定不同植物样品中的痕量硒含量。分别对电热板敞开消解和微波密闭消解两种前处理方法进行了比较,采用微波密闭消解法虽然溶解完全干扰少,但取样量太少,仪器信号波动对结果影响较大,对植物样品中痕量硒电热板敞开消解法可多取样增加仪器信号强度,结果更准确可靠。所加试剂引起的干扰通过空白实验予以消除。硒谱线强度与P（Se）的在0～1 000 μg/L范围内呈良好的线性关系,相关系数R为0.999 9。检出限为3.9 ng/g,方法用于标准样品分析,准确度△lgC(GBW)≤±0.059、RE(GBW)≤±14.49%,精密度RSD(GBW)≤7.26%,测定值与认定值相符,方法准确,适合大批量植物样品中痕量硒的分析测试。     

电感耦合等离子体质谱法测定煤中多种微量元素

采用低温灰化煤样及混合酸消化处理煤灰,应用电感耦合等离子体质谱法(ICP-MS)同时测定待测溶液中的12种微量元素。实验证明:选择合适的工作条件可使电感耦合等离子体质谱法的检出限低及精密度好,其相对标准偏差在1.82%～4.86%范围内;对煤炭、土壤、岩石标准样品多种微量元素的测定结果与推荐值一致;对煤炭样品进行加标回收实验,其回收率在80%～120%范围内;采用ICP-MS测定煤中多种微量元素,其具有简便快速、重复性好、结果准确等优点。     

流动注射-离子交换分离-二溴邻硝基苯基荧光酮光度法测定煤中锗

针对国家标准测定煤中锗存在的缺点，研究了流动注射-离子交换分离-二溴邻硝基苯基荧光酮光度法测定煤中锗含量的分析方法.该法采用流动注射技术进行痕量锗的离子交换分离与富集，在0.40 mol/L的HCl介质中，Ge⁴⁺与Cl-形成络阴离子，被阴离子交换树脂交换富集，用0.60 mol/L的HNO₃-1.5%柠檬酸溶液洗脱，用二溴邻硝基苯基荧光酮（DBoN-PFO）光度法测定锗，大量共存离子不干扰锗的测定.测定样品的相对标准偏差为2.67%~5.02%（n=8），加标回收率为96.39%~103.63%，方法的检出限为0.18μg/L，其准确度和精密度均满足国家标准的要求.     

微波消解ICP-MS测试铅精矿中的铟和锗

本文提出了铅精矿通过微波消解,ICP-MS测试得到铟和锗含量的方法。通过加标回收试验,得到铟的回收率在99.9%~101.60%,锗的回收率在96.8%~102.8%。通过检出限试验得到铟的检出限为0.001μg/g,锗的检出限为0.02μg/g。     

GD-MS法测定高纯钨锭中多种痕量杂质元素

采用辉光放电质谱法(GD-MS)同时测定了高纯钨锭中66种痕量杂质元素。主要杂质元素(K,Ba等)的测定值与电感耦合等离子体质谱法(ICP-MS)定量分析结果经F检验和T检验均验证在显著性水平为10%时,两者无显著性差异。试验表明GD-MS法对高纯钨锭的无标准样品的快速分析有较高的准确度。与ICP-MS法相比,GD-MS能直接分析固体样品,并具有分析元素多、测定范围广、检测限低、分析速度快等众多优点,已被公认为是最佳的高纯金属痕量杂质元素分析方法之一。     

ICP-MS测定四川石棉低品位碲矿中碲铋铜钴镍锑硒元素含量

本文采用电感耦合等离子体质谱(ICP-MS)法测定四川石棉低品位碲矿中碲以及铋铜钴镍锑硒的含量,探究了高压罐消解法-ICP-MS测定低品位碲矿中Te、Bi、Cu、Co、Ni、Sb和Se七种元素的检出限、定量限、精密度和回收率高低。结果表明,该方法在测定七种元素时,检出限为0.008～0.437μg/L,定量限为0.027～1.450μg/L;相对标准偏差均低于7%,具有良好的精密度;两种样品加标回收率均在89.7%～106%之间,具有较高的重复性,分析结果准确可靠。同时该方法操作简便、可用于大批样品的处理,是一种高效、准确的测定低品位碲矿中各元素含量的方法。     

氢化物-原子荧光光谱法测定高纯铅中微量铋的方法研究

研究了高纯铅中微量铋的氢化物 -原子荧光光谱简便、快速测定方法。详细考察了最佳测定条件、干扰情况和干扰消除方法及酸度。结果表明 ,采用硝酸溶解样品 ,蒸至有硝酸铅析出后 ,加入盐酸酸度达 2 0 %时 ,基体铅以氯化铅形式沉淀 ,消除基体铅的影响 ,其它共存离子也不干扰铋的测定。测定铋的检出限 (3σ)为 0 3 2ng/mL。按操作步骤对样品进行分析 ,铋的检出下限可达 0 1μg/g ,样品加标回收率在 97 2 %～ 10 5 0 %之间     

电感耦合等离子体法测定地质样品中的铷

建立了电感耦合等离子体质谱法测定地质化探样品中铷的方法。样品经HCl-HNO₃-HF-HClO₄敞口酸溶后, 用电感耦合等离子体质谱仪测定其中的铷含量。该法用于土壤、岩石中铷的测定, 检出限为3.2 ng/g, 相对标准偏差小于3%, 加标回收率在90%～120%之间。     

发射光谱法测定勘查地球化学样品中的银、锡

本法采用Al2O3、K2S2O7、NaCl的混合物为缓冲剂,Ge为内标,电弧发射光谱法测定勘查地球化学样品中Ag、Sn。方法检出限为Ag0.015μg/g、Sn0.25μg/g。方法精密度(RSD,n=12)为Ag4.5%～11.5%、Sn3.0%～7.5%。测定了国家一级地球化学标准物质,结果与标准相符,其各项技术指标均满足1∶5万化探要求。     

Bench-Scale and Pilot-Scale Treatment Technologies for the Removal of Total Dissolved Solids from Coal Mine Water: A Review

Coal mine water (CMW) is typically treated to remove suspended solids, acidity, and soluble metals, but high concentrations of total dissolved solids (TDS) have been reported to impact the environment at several CMW discharge points. Consequently, various states have established TDS wastewater regulations and the US EPA has proposed a benchmark conductivity limit to reduce TDS impacts in streams near mining sites. Traditional CMW treatment effectively removes some TDS components, but is not effective in removing major salt ions due to their higher solubility. This paper describes the basic principles, effectiveness, advantages, and disadvantages of various TDS removal technologies (adsorption, bioremediation, capacitive deionization, desalination, distillation, electrochemical ion exchange, electrocoagulation, electrodialysis, ion exchange, membrane filtration, precipitation, and reverse osmosis) that have at least been tested in bench- and pilot-scale experiments.     

低射频功率-电感耦合等离子体质谱法测定高纯石英样品中痕量钾

碱金属元素钾作为高纯石英产品中重要的杂质元素,其含量的准确测定对科学评价、开发高纯石英产品意义重大。采用常压混酸浸取—高温挥发除酸的方式进行高纯石英样品的化学前处理,基于电感耦合等离子体质谱仪,在低射频功率下,以50 ng/mL铷为内标元素,大幅消除了钾元素测定中背景产生的质谱干扰,实现了高纯石英样品中痕量钾元素的测定。对测试过程中的样品称样量、质谱测定中的射频功率、采样深度、载气流速等进行了条件优化。最终在称样量1.000 0 g、射频功率800 W、采样深度5.6 mm、载气流速1.06 L/min的最优条件下,经测定钾质量浓度在0.100~50 ng/mL范围内与其质谱强度呈线性相关,相关系数为0.999 6。以1.000 0 g称样量计,方法对高纯石英中钾的检出限为0.057 μg/g,定量限为0.191 μg/g。选择典型商品化高纯石英样品进行本方法的应用试验,每个样品平行测定9次,并进行加标回收率试验和方法比对试验,测定值与石墨炉原子吸收光谱法的测定结果基本一致,相对标准偏差(RSD)在2.9%~5.1%之间,加标回收率在96.4%~105.4%之间。      

Evaluating Relationships Between Total Dissolved Solids (TDS) and Total Suspended Solids (TSS) in a Mining-Influenced Watershed

Mine Water and the Environment - Measurement of total suspended solids (TSS) and total dissolved solids (TDS) loadings in streams is often used to assess potential impacts from mining on surface...     

The utilization of forward osmosis for coal tailings dewatering

The feasibility of dewatering coal tailings slurry by forward osmosis (FO) membrane process was investigated in this research. A prototype cell was designed and used for the dewatering tests. A cellulosic FO membrane (Hydration Technology Innovations, LLC, Albany, OR) was used for the dewatering studies due to its high fouling resistance. Representative samples of coal tailings slurry were collected from the thickener outflow at American Coal Company (Galatia, Illinois). Characterization studies were conducted to obtain particle size distribution (PSD), total dissolved solids (TDS) and the solids content of the slurry. The impact of the slurry properties such as solids weight percent, osmotic pressure, and particle size on the dewatering rates was determined. Furthermore, the impact of slurry conditioning by the addition of flocculant and gypsum on the rate and extent of dewatering was also investigated. Dewatering to a total solids content of more than seventy weight percent from an initial solids content of approximately thirty percent was achieved in all cases. The dewatering rate and extent were found to be a function of particle size, particle shape, TDS content, and mixing. The membrane material was shown to withstand repeated use over a period of thirty trials without deterioration of performance. The results obtained from this research suggest that osmotic dewatering of coal refuse slurry is feasible.     

Treatment of a Jordanian Phosphate Mine Wastewater by Hybrid Dissolved Air Flotation and Nanofiltration

Approximately 10,000?m3/day of untreated wastewater is produced during phosphate beneficiation at Eshydia phosphate mine in southern Jordan. The effluent contains 21?wt% phosphates (P₂O₅) and 12–14?wt% solids. Dissolved air flotation (DAF) and subsequent nanofiltration (NF) were investigated as potential treatment methods. DAF combined with the use of a commercial flocculant effectively removed the suspended solids and decreased total dissolved solids (TDS) by 50?%; NF effectively treated the DAF effluent and produced water with only 860?ppm TDS. The treated water can be recycled for use by Eshydia phosphate mine or for irrigation.     

用等离子体质谱法测定化学物相浸出液中的铼

采用电感耦合等离子体质谱法(ICP-MS)测定了铼化学物相分析浸出液中痕量铼, 系统研究了不同相态铼(Re₂O₇、ReO₂、ReO₃、金属铼及ReS₂等相)浸出液中痕量铼测定的相关影响因素, 并分析了几种钼矿石和焙砂样品, 结果准确可靠。实验证明, ICP-MS用于痕量铼的测定, 简便快速, 值得推广。     

煤矸石中溶解性有机质(DOM)溶出的动力学变化

以神华神东煤炭集团公司补连塔煤矿采空区取得的煤矸石作为研究对象,通过淋滤实验,探索室温条件下煤矸石中溶解性有机质的溶出动力学规律。研究结果表明:煤矸石淋出液的p H值从最大值8.74下降到7.64,电导率(EC)和溶解性总固体(TDS)均经过了快速下降、慢速下降至稳定的3个阶段,并且硝酸盐和氨氮的含量很低。淋出液中溶解性有机碳(DOC)、UV254经过了快速增大、减小至稳定的3个阶段,且DOC和UV254具有一定的线性相关关系,这说明煤矸石水溶性DOM中含有一定的苯环类芳香族化合物。DOM样品中主要有3类荧光峰,即类芳香族蛋白峰、溶解性微生物代谢产物峰和海洋腐殖酸峰,其中,93.3%的样品中出现有类芳香族蛋白荧光峰。样品的荧光指数FI值从1.85逐渐上升到最大值2.77,SUVA254最大值为0.7 L/(m·mg),生物源指数BIX在0.78~1.23间波动,均可证实煤矸石中DOM主要是以微生物源(内源)有机质为主,且与生物或细菌活动密切相关。