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稀土元素以及钪、钇等十七个元素,化学性质十分相似,因此相互间的分离及其分量的测定一直是分析化学中的难题之一。近年来,稀土元素的应用越来越广泛(如稀土超导材料的研究应用),同时各学科的发展对稀土杂质要求测定下限越来越低,成为分析测试中急待解决的问题之一。 目前测定稀土元素的方法较多,有光度法、原子发射光谱法、原子吸收光谱法、电化学分析法、活化分析法、质谱法、原子荧光法、化学发 相似文献
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电感耦合等离子体原子发射光谱(ICP—AES)已应用测定地质样品中从镧(La)到镥(Lu)(铽除外)稀土元素(REE)。REE的组分离首先用过氧化钠和样品熔融,以便除去大量的基体,然后用钇(Y)载体形成氟化物沉淀。这样使光谱干扰减至最小,并且为在地壳各处的分布量的浓度标准提供适合的炅敏度。对于绝大多数元素其精密度是3～5％,对于接近测定极限浓度的某些低含量元素,其精密度大约为10％。把测定一系列参考样品所获得的结果同文献的值相比较,表明该方法是为地球化学研究提供稀土元素分布数据的有效方法。 相似文献
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一、稀土元素的地球化学特徵稀土元素是指周期表上原子序数从57到71的十五个元素而言。“稀土”一詞源出于拉丁文Terrae Rarae。当时对“稀”的理解是指在自然界中提取这类元素的矿物很少,而所謂的“土”则是指元素的成盐氧化物成土状,有如土族元素氧化物。所有稀土元素的原子結构都很相似,因之它們在化学和物理性质上也都十分相近,統称为镧族元素或稀土金属。周期表中与稀土元素同属于第Ⅲ族的钇,往往与稀土元素共同存在于一些矿物中,并具有着大致相同的地球化学特性,而钇的离子半径、盐基性、盐溶解度等許多化学性质皆具有镧族收縮現象,因而元素钇也就有条件地被列入稀土元素之中。稀土元素原子結构的特点是电子层的外两层(O层与P层)的电子数是相同的,排列情况也是近似的。 相似文献
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高分辨电感耦合等离子体质谱法测定地球化学样品中钪钇和稀土元素 总被引：4，自引：2，他引：2
建立了高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定地球化学样品中钪、钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥的分析方法。样品经氢氟酸-硝酸-硫酸-王水消解,试液直接用HR-ICP-MS测定钪、钇和14种稀土元素。用高分辨模式有效地避免了多原子离子及难熔氧化物离子对待测元素测定的干扰,为钪、钇和14种稀土元素选择了最佳的测定同位素和合适的分辨率;用地球化学标准物质制备的溶液优化仪器工作参数,确定了最佳的仪器测定条件。方法检出限(6σ)为0.003～0.013μg/g(稀释因子为1000),相对标准偏差(RSD,n=12)小于6%。方法经国家一级地球化学标准物质验证,测定值与标准值吻合。 相似文献
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火焰发射光谱法测定卤水中铷和铯 总被引：2，自引：0，他引：2
选择LaCl3 作电离缓冲剂,用火焰发射光谱法测定卤水中的Rb和Cs,有效地降低了基体干扰,提高了方法的灵敏度。方法的测定下限为: 18μg/LRb, 1. 8μg/LCs;加标回收率在92. 4% ~105. 0%。方法用于实际样品分析,结果与KCl电离缓冲剂原子吸收光谱法相吻合,且减少了预先测定K 的操作。对卤水样品中Rb和Cs11次平行测定,计算方法的RSD分别为5. 78%和8. 11%。 相似文献
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二苯硫脲泡塑富集-原子吸收光谱法连续测定化探样品中金和银 总被引：3，自引：2，他引：1
传统的发射光谱、化学光谱、泡塑富集分离-原子吸收光谱法测定化探样品中的金和银,分析结果不稳定,效率低。本研究提出用50%的王水分解化探样品,负载二苯硫脲泡塑吸附金银,石墨炉和火焰原子吸收光谱法对金和银进行联合测定。在二苯硫脲浓度、吸附酸度、吸附温度、振荡时间等优化的实验条件下,金和银的回收率分别达到97.9%和98.8%,检出限为0.25 ng/g和0.038μg/g,准确度(RE,n=9)为2.0%～14.0%和7.7%～13.3%,精密度(RSD,n=9)为3.1%～12.4%和5.1%～13.2%。经国家标准物质分析验证,测定值与标准值基本相符。该方法实现了在同一份溶液中同时测定金和银,与现行的石墨炉原子吸收光谱测定金、发射光谱测定银的方法相比,称样量达到10 g,样品的代表性显著增加,提高了准确度和精密度,简化了金银分析的程序,化学试剂用量少,分析成本低。 相似文献
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ICP发射光谱法测定矿样中痕量稀土分量本文讨论了以ICP-AES法测定矿样中痕量稀土元素分量方法.实验曾借鉴岩矿测试所的方法.此方法是将试样经阳离子交换富集,浓缩至小体积,加入内标后,通过气动雾化器将溶液输送到ICP激发,摄取光谱.不同稀土元素的检出限分别为0.00X～0.Xμg/g各被测元素光谱测定相对标准偏差为1.8～4.1%.经GSD-1～GSD-8标样三次分析,以及经半年多来五批样品的生产实践证明,本方法流程简单,分析速度快,易于推广,检出限和精确度基本上能满足需要. 相似文献
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电热蒸发—电感耦合等离子体原子发射光谱及其在痕量稀土分析中的应用 总被引：4，自引：0，他引：4
评述了电热蒸发电感合等离子体原子发射光谱分析（ＥＴＶ－ＩＣＰ－ＡＥＳ）联用技术的新近进展及其在痕稀土元素检测中的应用。从原理、分析性能、方法及应用诸方面对以聚四氟乙烯（ＰＴＦＥ）悬本为化学改进剂的氟化辅助电热蒸发（ＦＥＴＶ）－ＩＣＰ－ＡＥＳ新技术作了全面的介绍,引用参考文献２８篇。 相似文献
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原煤的开采、储存、运输及其加工利用过程是多环芳烃(PAHs)污染的主要来源。由于缺乏相关系统调查数据,其对煤矿复垦区土壤环境质量的影响尚不明确。平朔煤矿复垦土地主要作为耕地利用,了解其PAHs污染状况直接关系粮食安全和人体健康。该研究通过野外实地调查,开展了平朔煤矿复垦区表层土壤中多环芳烃(PAHs)的毒性风险分析研究。在整个平朔煤矿45 km2范围内,以500 m×500 m间距为基准,按照不同用地类型,采集了0~20 cm深度土壤样品179个,再按照1 km×1 km单元格组合后分析。使用安捷伦高分辨气相色谱低分辨质谱进行目标物的检测。加入代用标准2氟联苯(2 FBP)以进行回收率控制。研究结果表明：土壤中16种EPA PAHs的含量范围为213.60~2 513.20 ng·g-1,均值为717.09 ng·g-1。PAHs成分特征显示主要以3~4环为主(52%),5~6环次之(42%),2环所占比例最低(6%)。使用相关分析法判定,主要污染来源为原煤。毒性风险分析结果显示,平朔煤矿土壤PAHs存在一定生态风险,当土地重新作为农田加以利用时,需要加以关注。 相似文献
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北京密云房山地区土壤中多环芳烃的组成与分布特征 总被引：15，自引：2，他引：15
选择北京城近郊房山与密云地区的土壤进行了多环芳烃的定量分析，同时探讨了多环芳烃在土壤中的分布特征与来源。研究结果显示：密云、房山两地土壤中多环芳烃的含量值具有明显差异，提示了两地工业活动影响强度的不同；各采样区土壤中多环芳烃总量的平均值在45．98～388．23ng／g变化，根据多环芳烃的特征参数可以推测研究区土壤中的多环芳烃主要来自于化石燃料的不完全燃烧。 相似文献
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Accumulation and risk assessment of polycyclic aromatic hydrocarbons (PAHs) in soils around oil sludge in Zhongyuan oil field, China 总被引：1，自引：0，他引：1
In this paper, the contents of polycyclic aromatic hydrocarbons (PAHs) in soil samples around three different oily sludge
plants in winter were analyzed by high performance liquid chromatography (HPLC) and the pollution degree with PAHs in soil
samples was determined. Soil samples were collected from the agricultural soil around three different oily sludge plants (the
Third Wenming Plant, the Third Mazhai Plant, and the Fourth Wener Plant) along with the leeway in Zhongyuan oil field. The
distances from collected sample sites to oily sludge plants are 10, 20, 50, 100, 200, and 500 m, respectively. The results
show that the contents of PAHs in soil samples decrease dramatically with the increase of the distance from the oily sludge,
and that the PAHs with 2–4 rings are major pollutants in the oily sludge and soil samples. The main factors, which influenced
the distribution of PAHs are discussed. Based on Nemero Index P, the classification evaluation shows that the soils around
the oily sludge are heavily polluted in winter. The health risk assessment and ecological risk assessment of the soils around
the oily sludge in Zhongyuan oil field in winter are analyzed. 相似文献
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Compositional fractionation of polyaromatic hydrocarbons in the karst soils, South China 总被引：1，自引：0，他引：1
Yinghui Wang Rui Xue Jie Li Hongxiang Zhu Yiyin Xu Baoming Xue Shihua Qi Daoxian Yuan Oramah I. Theodore 《Environmental Earth Sciences》2012,66(7):2013-2019
This study aims to explore the condensation and fractionation trends of persistent organic pollutants (POPs) in the karst soils. The tiankeng is a karst surface expression that can act as a focal point for introduction of contaminants to a karst aquifer, which may serve both as condenser for vapor phase POPs and as barrier/sink for particulate associated less volatile POPs. The fractionation of POPs in soils from the upper rim and floor of tiankeng is of interest in understanding the role of tiankeng in the long-distance transport of POPs. In the present study, polycyclic aromatic hydrocarbons (PAHs) in the surface soils from the upper rim and floor of Dashiwei tiankeng in Southern China were analyzed. The total PAH concentrations in soils were 23.40–190 ng g−1, with phenanthrene being the most abundant. The distribution patterns of PAH compounds in the soil samples matched well with their properties. It indicated the heavy PAHs were susceptible to retention by the floor soils of tiankeng than light PAHs. A plot of Cfloor/Crim against PAH molecular weight gave a good positive relationship in the molecular weight range of 152–276. It is suggested that the floor soils can be focal points of more concentrated PAH and deserve attention. The concentrations of total PAHs in the floor soils (43.40–190 ng g−1, mean 87.76 ng g−1) were higher than those in the upper rim (23.40–88.94 ng g−1, mean 57.74 ng g−1). In addition, there was a shift in compound pattern with an increase in the proportion of light PAHs (2–3 rings), a decrease in heavy PAHs (5–6 rings) and a relatively stable content of 4-ring PAHs. A combination of particulate scavenging and cold condensation is proposed as the major mechanism for the compositional fractionation of PAHs in the soils from the upper rim and floor of tiankeng. 相似文献
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Characterization and source apportionment of polycyclic aromatic hydrocarbons (PAHs) in sediments in the Yellow River Estuary, China 总被引：3，自引：0，他引：3
Ning-jing Hu Peng Huang Ji-hua Liu De-yi Ma Xue-fa Shi Jian Mao Ying Liu 《Environmental Earth Sciences》2014,71(2):873-883
Concentrations and sources of polycyclic aromatic hydrocarbons (PAHs) were investigated in surface sediments of the Yellow River Estuary (YRE). The isobath-parallel tidal and residual currents play important roles in the variation of PAH distribution, such that the contamination level of PAHs in fine-grained sediments is significantly higher than in the relatively coarse grain size sediments. Both diagnostic ratios and principal component analysis (PCA) with multivariate linear regression (MLR) were used to apportion sources of PAHs. The results revealed that pyrogenic sources are important sources of PAHs. Further analysis indicated that the contributions of coal combustion, traffic-related pollution and mixed sources (spills of oil products and vegetation combustion) were 35, 29 and 36 %, respectively, using PCA/MLR. Pyrogenic sources (coal combustion and traffic-related pollution) contribute 64 % of anthropogenic PAHs in sediments, which indicates that energy consumption could be a predominant factor in PAH pollution of YRE. Acenaphthylene and acenaphthene are the two main species of PAHs with more ecotoxicological concern in YRE. 相似文献
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The aim of this study was to determine the sources and contamination characteristics of polycyclic aromatic hydrocarbons (PAHs) in various environmental media in a karst underground river system. For this purpose, air, underground river water, sediment, and soil samples were collected from a typical underground river in southern China in the dry and wet seasons of 2013–2014, and the compositional spectra, distribution, and ratio characteristics of 16 PAHs were determined for comparative analysis. The results show that three 2–3-ring PAHs (naphthalene, phenanthrene, and fluoranthene) mainly occur in air and underground river water. In sediments and soils, 4–6-ring PAHs are the main components. The PAH concentrations in the air in the wet season are clearly greater than those in the dry season, while it is the opposite in the underground water. Seasonal differences in the concentration of PAHs in the sediments and soils are minor. The concentrations of PAHs in the environmental media overall showed variation in the following order: upstream < midstream < downstream, and this is related to pollutant discharge, adsorption, etc. The main source of PAHs in the upstream area is the combustion of grass, wood, and coal, while it is petroleum in the midstream area, and combustion of grass, wood, coal, and petroleum near the outlet of the underground river. It is necessary to change the energy structure in the study area, improve the efficiency of environmental protection facilities, reduce the emission in vehicle exhaust, and control pollution by PAHs at their sources. 相似文献
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Fifty soil samples collected from agricultural land in four regions of Poland with different anthropopressure were analysed for their content of 16PAHs by GC/MS. The regions correspond to Polish administrative units (voievodeships): Podlaskie and Lubelskie are situated in the rural East part of the country and more industrialised Slaskie and Dolnoslaskie voievodeships – in the South-West part. Basic physicochemical properties as well as the content of selected potentially harmful metals (Pb and Zn) were included in the soil analysis. Overall accumulation of Σ16PAHs in the upper soil layer was within the range 73–1800 μg kg−1 with a geometric mean (GM) of 252 μg kg−1, while the mean benzo(a)pyrene (BaP) load was 20 μg kg−1. This corresponds with data for other European countries. Carcinogenic compounds contributed nearly in 50% to the total PAHs loads. In uncontaminated rural regions the mean Σ16PAHs and BaP contents were 113–159 μg kg−1 and 11–13 μg kg−1, respectively. Regional conditions strongly influenced the accumulation of PAHs ?4-rings, which were highly dependent (over 95%) on local anthropopressure expressed as dust and 4PAHs emission indexes. Soil acidity was the main soil parameter related to the accumulation of higher molecular weight PAHs in soils. In more contaminated regions a significant link between soil OM and PAH loads was noted. The same regions were characterised by associations between PAHs and potentially harmful metals implying common sources of pollution. Those relationships were not observed in the uncontaminated part of the country. The lower molecular weight PAHs contributed to a smaller extent (about 20%) to the total PAHs content in soils, and were less affected by anthropogenic factors. 相似文献
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Xue Song Wang 《Environmental Earth Sciences》2013,70(6):2855-2864
Polycyclic aromatic hydrocarbons’ (PAHs) concentrations in bulk samples are commonly used to assess contamination but PAHs are unevenly distributed among particle-size fractions. Seventeen urban surface soil samples from the city of Xuzhou, China, were collected and then fractionated into five size fractions (2,000–300, 300–150, 150–75, 75–28, and <28 μm). The concentrations of 12 US EPA PAHs were measured using gas chromatograph/mass spectrometry in various fractions, and the bulk soil samples and distribution patterns of PAHs in different particle-size fractions were investigated. The mean concentration of total PAHs in bulk soil samples was 1,879 ng/g. The median concentrations for all individual PAH were higher for the 75–2,000 μm fraction than for the <75 μm fraction. The distribution factors for various PAHs in <28 μm soil fraction were closely correlated (r = ?0.661, p < 0.019) to bulk soil fugacity capacity. The values of PAH isomer indicated that traffic emissions might be the major origin of PAHs in Xuzhou surface soils. Spearman correlation analysis was performed and the result suggested that soil organic carbon might be a factor controlling the concentrations of PAHs in soils. 相似文献
20.
Pollution characteristics of polycyclic aromatic hydrocarbons （PAHs） in oily sludge from the Zhongyuan Oilfield and its peripheral soils 总被引：1，自引：1，他引：0
The purpose of this study is to determine the degree of contamination caused by polycyclic aromatic hydrocarbons (PAHs) in
oily sludge and soils around it in the Zhongyuan Oilfield. The contents of polycyclic aromatic hydrocarbons in oily sludge
samples were determined with HPLC. The contents of PAHs of oily sludge from three different oil production plants vary from
high to low in the order of the Wenming oily sludge dumping site of No. 3 Oil Production Plant (3W)>the Mazhai oily sludge
dumping site of No. 3 Oil Production Plant (3M)>the Wen’er oily sludge dumping site of No. 4 Oil Production Plant (4W). Naphthalene,
acenaphthylene, acenaphthene, fluorine and phenanthrene are the major pollutants of PAHs in oily sludge. The contents of PAHs
in soil samples around the oily sludge dumping sites vary widely from 434.49 to 2408.8 ng/g. Naphthalene, acenaphthene, fluorine,
phenanthrene and pyrene are the characteristic factors of PAHs in soil samples of 3M and 3W, and naphthalene, acenaphthene,
fluorine and phenanthrene are the characteristic factors of PAHs in soil samples of 4W. According to these data and the ratios
of Fl/Py, PAHs in oily sludge samples come mainly from petrogenic sources, and soil samples are divided into petrogenic soil
samples and mixed-source soil samples, and both petrogenic and pyrogenic soil samples in terms of the sources of PAHs. The
classification by Nemero index P indicates that soils around the oily sludge dumping sites have been seriously polluted. 相似文献