偏硼酸锂熔矿-超声提取-电感耦合等离子体发射光谱法测定岩石水系沉积物土壤样品中硅铝铁等10种元素

采用偏硼酸锂熔矿分解样品,超声波振动提取,电感耦合等离子体发射光谱法同时测定同一份溶液中的硅、铝、铁、钙、镁、钾、钠、磷、锰、钛等组分。通过对岩石、水系沉积物和土壤国家一级标准物质测定验证,方法的准确度、精密度能够满足样品中各元素定量分析的要求。     

食品级氯化钾制备工艺和杂质检测方法的研究进展

食品级氯化钾的制备工艺主要为热溶结晶法,其间通过加入晶种、酸、碱、助滤剂等去除原料中的镁离子、钙离子、硫酸根、有机物等杂质。氯化钾中杂质的检测方法可采用滴定法、电感耦合等离子体光谱法、原子吸收分光光度法、紫外可见分光光度法等。随着食品级氯化钾市场规模的逐渐扩大,行业对产品质量要求也不断提高,其制备工艺技术和杂质检测方法也需不断改进和完善,进一步促进行业有序发展。     

含锂卤水中锂资源高效利用与绿色分离的新型萃取体系

针对现有高镁锂比盐湖卤水、碳酸锂产业排放的碱性料液、废旧锂电池回收液等含锂溶液的萃取分离技术现状以及高效、清洁、高值化利用的重大需求及关键基础科学问题,设计合成出数十种酰胺类、磷酸酯类以及双酮类锂特效萃取剂,通过对该类萃取剂的表征与不同放大规模的研究,筛选出多个具有工业应用前景的锂萃取体系,研发出适合我国盐湖卤水锂资源特点的、经济上可行的具有自主知识产权的分离提取锂的新萃取体系与工艺,突破高镁锂比盐湖卤水提锂这一世界性技术难题。经过产业化应用研究,萃取法从高镁锂比盐湖卤水中分离提取锂的技术,在锂镁选择性分离以及资源高效利用率方面已经凸显出了比现有任何提锂工艺更加优异的效果,为我国盐湖资源高效、清洁、高值化利用提供科学依据,提升我国在盐湖锂分离领域的国际地位和竞争力。     

A review of Australian salt lakes and associated mineral systems

This study reviews the available information for over 1200 Australian salt lakes including in areas that have little or unreliable data. Publicly available groundwater hydrogeochemical datasets for the Australian arid zone are particularly sparse, inconsistent and of variable quality. Many datasets in the vicinity of salt lakes only report salinity or total dissolved solids, with no data for constituent cations and anions, and no appreciation of the hydrological and geomorphic evolution of the lakes. To overcome these limitations and to provide a broad-scale context, we developed mineral systems models to assess the potential of Australian salt lakes for potash, lithium and boron deposits. These models show that an important control on the potential of salt lake systems to form economic deposits of potash, lithium or boron is hydrogeological connectivity between leachable source rocks and the lakes. The assessment of the mineral potential was carried out in two stages. The first stage selection was based on the presence of favourable source rocks in the salt lakes’ catchments. The mean values of concentration in each catchment were derived from whole rock, sediment and groundwater geochemical datasets by averaging the values in samples (separately for each of the three datasets) located in the catchment and assigning this value to the catchment's salt lakes. The second stage selection was carried out by analysing available chemical data of groundwater in proximity to the salt lake systems delineated in the first stage. As a result, six regions were identified as having the highest potential, for potash in particular, but also for lithium and/or boron deposits. These are: the Lake Frome/Central Gawler Region of South Australia; two regions in the Northern Territory: the central western region extending into Western Australia, and the Lake Woods region; and, in Western Australia, the Lake Disappointment region, the north east Yilgarn and south east Yilgarn regions.     

Ephemeral stream chemistry below the elevation of near‐zero net infiltration

Stormwater along ephemeral arroyos and areal infiltration in nearby boreholes were studied in the Amargosa Desert Region of Southern Nevada, USA. Chemical composition of ephemeral stream runoff was measured at elevations below where areal infiltration generally occurs in arid environments using lysimeters designed for this study. Borehole cuttings from several wells were evaluated in terms of chloride migration. Analysis of the borehole data indicates that net areal infiltration has been insignificant for the past 10 000+ years. This is associated with an environment where chloride and other soluble salts accumulate in shallow sediments and potentially in runoff waters. Measured storm events during the 4‐year study period were small and localized but sufficient to produce surface runoff, at least near the lysimeters. Composition of storm runoff captured by the lysimeters was found to be a combination of the water chemistry types found in precipitation and from leaching tests of near‐surface sediments. All major cations and bicarbonate increased relative to chloride when precipitation interacted with sediments to form ephemeral stream runoff. The changes were consistent with calculated saturation indices. Despite the long‐term accumulation of chloride in soils and deep sediments caused by complete evapotranspiration of infiltrating precipitation, runoff waters were characterized by low chloride and total dissolved solids. This study presents a limitation of the chloride mass‐balance method, as chloride and water migration were disassociated from each other in the study area. Copyright © 2014 John Wiley & Sons, Ltd.     

Aspect control of water movement on hillslopes near the rain–snow transition of the Colorado Front Range

In the Colorado Front Range, forested catchments near the rain–snow transition are likely to experience changes in snowmelt delivery and subsurface water transport with climate warming and associated shifts in precipitation patterns. Snowpack dynamics are strongly affected by aspect: Lodgepole pine forested north‐facing slopes develop a seasonal snowpack, whereas Ponderosa pine‐dotted south‐facing slopes experience intermittent snow accumulation throughout winter and spring. We tested the degree to which these contrasting water input patterns cause different near‐surface hydrologic response on north‐facing and south‐facing hillslopes during the snowmelt period. During spring snowmelt, we applied lithium bromide (LiBr) tracer to instrumented plots along a north–south catchment transect. Bromide broke through immediately at 10‐ and 30‐cm depths on the north‐facing slope and was transported out of soil waters within 40 days. On the south‐facing slope, Br^? was transported to significant depths only during spring storms and remained above the detection limit throughout the study. Modelling of unsaturated zone hydrologic response using Hydrus‐1D corroborated these aspect‐driven differences in subsurface transport. Our multiple lines of evidence suggest that north‐facing slopes are dominated by connected flow through the soil matrix, whereas south‐facing slope soils experience brief periods of rapid vertical transport following snowmelt events and are drier overall than north‐facing slopes. These differences in hydrologic response were largely a function of energy‐driven differences in water supply, emphasizing the importance of aspect and climate forcing when considering contributions of water and solutes to streamflow in catchments near the snow line. Copyright © 2012 John Wiley & Sons, Ltd.     

Soil profile evolution following land‐use change: implications for groundwater quantity and quality

Soil and vadose zone profiles are used as an archive of changes in groundwater recharge and water quality following changes in land use in an area of the Loess Plateau of China. A typical rain‐fed loess‐terrace agriculture region in Hequan, Guyuan, is taken as an example, and multiple tracers (chloride mass balance, stable isotopes, tritium and water chemistry) are used to examine groundwater recharge mechanisms and to evaluate soil water chloride as an archive for recharge rate and water quality. Results show that groundwater recharge beneath natural uncultivated grassland, used as a baseline, is about 94–100 mm year^?1 and that the time it takes for annual precipitation to reach water table through the thick unsaturated zone is from decades to hundreds of years (tritium free). This recharge rate is 2–3 orders of magnitude more than in the other semiarid areas with similar annual rainfall but with deep‐rooted vegetation and relatively high temperature. Most of the water that eventually becomes recharge originally infiltrated in the summer months. The conversion from native grassland to winter wheat has reduced groundwater recharge by 42–50% (50–55 mm year^?1 for recharge), and the conversion from winter wheat to alfalfa resulted in a significant chloride accumulation in the upper soil zone, which terminated deep drainage. The paper also evaluates the time lag between potential recharge and actual recharge to aquifer and between increase in solute concentration in soil moisture and that in the aquifer following land‐use change due to the deep unsaturated zone. Copyright © 2012 John Wiley & Sons, Ltd.     

What can be deduced from chemical measurement in an open-field raingauge? An example in the Maures Massif,southeastern France

Abstract

The deposition of chemical elements in a catchment occurs through three different processes: wet, dry and cloud deposition. Total deposition cannot be inferred from measurements made with open-field raingauges, and still constitutes a challenge to scientific method. The chemical composition of samples from an open-field raingauge (bulk precipitation) was analysed over a period of several years in a small Mediterranean catchment in the Maures Massif, France. The input of chloride measured in this way was two times lower than the output, despite the fact that this element is reputed to be conservative, which means input and output should roughly balance. This implies that input has previously been underestimated. Analysis of the bulk precipitation data was carried out taking into account both the history of rain events and of sampling. This study allowed the relative parts of the different deposition processes to be quantified. Dry deposition can provide from 20% to more than 80% of the anthropogenic and terrigenic elements (Ca²⁺, Mg²⁺, K⁺, NO₃ ^?, SO₄ ^2-, SiO₂) to the rain samples. The occult deposition of marine elements on the catchment area (50% of total deposition) was found to be mostly due to cloud deposition during wet periods.     

加速溶剂萃取技术提取海洋沉积物中游离态脂肪酸的方法研究

脂肪酸是沉积物中含量最丰富的脂类标记物之一,其存在形式主要有游离态脂肪酸和结合态脂肪酸。游离态脂肪酸可由溶剂直接提取,结合态脂肪酸是在已提取出游离态脂肪酸的沉积物残渣中加入酸碱加热后再用溶剂提取。加速溶剂萃取技术(ASE)因成本低和操作毒性小,在脂肪酸研究中得到了广泛的应用。本文采集东海近海海域沉积物作为研究样本,由于其中游离态脂肪酸含量丰富,而结合态脂肪酸含量过低,测定结果精密度差,难以作为方法研究对象,因此主要针对游离态脂肪酸应用加速溶剂萃取法进行提取,研究了各种实验条件,包括萃取剂、萃取温度、静态萃取时间和循环次数的选择与优化。分析结果表明,甲醇-二氯甲烷(V:V,1:3)更适合作为萃取剂;随着萃取温度、静态萃取时间、循环次数的增加,不同类型脂肪酸的提取效率各不相同,以涵盖碳原子数最多为先决条件,以脂肪酸的萃取效率最大化为依据,确定了加速溶剂萃取的实验条件是:萃取温度110℃,静态提取时间10 min,循环3次。用这种处理方法5次测定沉积物样品中游离态脂肪酸的精密度为3.3%~19.0%,其替代物回收率为72.2%~104.6%。该方法应用于分析实际海洋沉积物样品,相比于传统的索氏提取法,流程简单,极大地提高了工作效率。     

熔融制样X射线荧光光谱法测定锑矿石中的锑和14种微量元素

锑矿石分析通常分别采用酸分解系统和碱熔系统,萃取分离后应用容量法、原子吸收光谱法、原子荧光光谱法等分析手段进行单项测定,样品处理繁琐、操作复杂,分析过程常因熔矿不完全而导致结果偏低或失真,难以满足地质测试的需要。本文建立了玻璃熔融制样,波长色散X射线荧光光谱测定锑矿石中的锑及14种次量元素与伴生元素(Cu、Pb、Zn、As、Co、Ni、W、Ba、S、SiO₂、Al₂O₃、TFe、CaO、MgO)的快速分析方法。用国家标准物质和人工合成标准参考物质拟合校准曲线,对熔融条件进行了研究。确定样品与四硼酸锂-偏硼酸锂-氟化锂复合熔剂的熔融稀释比例为1:20,以硝酸铵为氧化剂,碳酸锂为保护剂,700℃预氧化,在1050℃温度下熔融完全,有效地防止了As、S的挥发损失,解决了化学法测试样品处理复杂、不能同时测定多元素、测试元素偏少的问题。一些元素的检出限为Sb 0.14%,Cu 0.0027%,Pb 0.0025%,Zn 0.0046%,As 0.0028%,S 0.021%;方法精密度(RSD,n=12)小于5%;选用合成标准物质和实际生产锑矿试样进行验证,测定结果与参考值或化学值一致性良好。本法大部分元素检出限都要稍高于粉末压片法,但操作简单,测试范围更宽,适用于实验室对不同锑矿矿种批量样品中多元素快速、准确检测的需要。