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231.
232.
土壤中单环芳烃定量分析的基质效应研究 总被引:1,自引:0,他引:1
来源于燃料油泄露的单环芳烃对土壤的污染已经成为一个很普遍的现象,因此,准确、高效地检测土壤中的挥发性单环芳烃是一个很关键的问题。文章通过在标准系列中加入石英砂和土壤两种基质,比较水、水-石英砂、水-土壤3个定量库中得到的标准曲线的斜率,研究基质效应对土壤样品定量的影响。结果表明,芳香烃类物质在土壤基质中的斜率总体小于在石英砂基质中的斜率,在石英砂基质中的斜率比在水基质中的斜率小1%(苯)~9%(正丁苯),在水基质中得到的斜率最大;只有苯在土壤基质和水基质中的斜率相当,其余组分在土壤基质中的斜率比在水基质中的斜率小9%(丙苯)~24%(1,2,4-三氯苯)。单环芳烃在土壤基质中相对斜率的大小与化合物本身的沸点以及辛醇-水分配系数呈负相关。研究表明,在对土壤样品进行校准的过程中,选择合适的基质建立定量库是一个非常关键的因素。 相似文献
233.
Kevin R. Chamberlain Axel K. Schmitt Susan M. Swapp T. Mark Harrison Norbert Swoboda-Colberg Wouter Bleeker Tony D. Peterson Charles W. Jefferson Andrei K. Khudoley 《Precambrian Research》2010
An in situ U–Pb SIMS (IN-SIMS) method to date micro-baddeleyite crystals as small as 3 μm is presented with results from three samples that span a variety of ages and geologic settings. The method complements ID-TIMS geochronology by extending the range of dateable crystals to sizes smaller than can be recovered by physical separation. X-ray mapping and BSE imaging are used to locate target grains in thin section, followed by SIMS analysis on a CAMECA ims 1270, using the field aperture in the transfer column to screen out ions from host phases. Internal age precisions for the method are anticipated to range from 0.1% for Precambrian rocks to 3–7% for Phanerozoic rocks. Results establish a 2689 ± 5 Ma age for mafic dikes in the Wyoming craton, USA, a 1540 ± 30 Ma age for a subaerial lava flow from the Thelon Basin of northern Canada, and a 457 ± 34 Ma age for mafic dikes in the platform sequence of southeastern Siberia. The method is ideal for relatively non-destructive dating of small samples such as extraterrestrial rocks and precious terrestrial samples. 相似文献
234.
This review describes developments major and in trace element determination using atomic absorption spectroscopy (AAS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), instrumental neutron activation analysis (INAA), and X-ray fluorescence (XRF) spectrometry that were reported in 2008 and 2009. Publication levels were comparable to those of previous years, except for XRF which showed an increase in the number of articles published in the past 2 years. In terms of number of publications and impact, the most active field was AAS, while INAA was the least active. As expected for well-established and mature methods, novel developments for all four analytical techniques were relatively sparse. For AAS, the most notable publications concerned developments in sample introduction, particularly focussing on solid samples, increasing analyte sensitivity, and higher sample throughput. For ICP-AES, publication of developments in sample introduction, remediation of matrix effects and calibration continues. Compared with past years, there was a clear focus on sample preconcentration methods, but very few publications reporting new hyphenated speciation methods. For INAA, there were several publications exploring the accuracy and robustness of the method, as well as the requirements for INAA to meet criteria for a primary method of measurement. Two other related techniques, delayed neutron activation analysis, and prompt gamma activation analysis, were also described. Hyphenated XRF techniques showed interesting developments in enabling XRF and XRD analysis on the same spot, and further work characterising and calibrating three-dimensional micro-XRF shows promising results for investigating sample heterogeneity. 相似文献
235.
原子荧光测定食品中总砷方法的改进与探讨 总被引:1,自引:0,他引:1
针对国标《GB 5009.11—2003食品中总砷及无机砷的测定》中的原子荧光-湿法消解测定总砷的方法中存在的难于控制完全消解样品、测定结果不稳定,试剂用量大的问题,对原方法进行了3点改进。一是利用浓硫酸沸点高,能脱水碳化破坏有机物的特性,通过高温浓缩硫酸对样品进行两次脱水碳化消解,使样品消解的更完全,且节省试剂;二是针对样品中砷形态的多样性,加强温度控制,低温消解、降低易挥发砷化合物的损失,高温加速样品消解,缩短操作时间;三是加盖小漏斗制造回流,减少易挥发砷化合物的损失,使方法易操作、节省试剂。用改进的方法测定菠菜粉(GBW10015)、海带粉(GBW08517)和虾粉(CNAS T0442)中的总砷,不少于6个平行样的测定结果均位于参考值范围的中间部分,且RSD值均小于7%,表明改进的方法准确、稳定。结果还表明,200℃的硫酸、高氯酸的混合酸和高温浓硫酸均能有效消解样品中砷甜菜碱和砷糖类化合物。 相似文献
236.
以太平洋鳕鱼为原料,从鳕鱼脑中分离硫苷脂,确立了提取及纯化的条件,并对硫苷脂的纯度和分子种进行分析。首先,采用氯仿/甲醇(2∶1,v/v)提取总脂。然后,依次采用氯仿/甲醇/水(7∶3∶0.3,v/v/v)洗脱硅胶柱层析,含0.2mol/L乙酸铵的氯仿/甲醇/水(30∶60∶8,v/v/v)洗脱DEAE Sephadex-A25离子交换柱层析,40%甲醇脱盐和100%甲醇洗脱反相C8柱层析,获得硫苷脂纯品。最后,利用500YMC Diol液相色谱柱(3.0mm×250mm,5μm)分离,以正己烷/异丙醇(70∶30,v/v),异丙醇/水/甲酸/氨水(100∶13∶1∶0.14,v/v/v/v)为流动相梯度洗脱,采用负电喷雾电离(ESI)和母离子扫描模式,用液相色谱-串联质谱(LC-MS/MS)法分析了鳕鱼脑硫苷脂的纯度和分子种组成,并比较了其与哺乳动物脑中硫苷脂分子种组成的异同。结果表明,本实验制得的鳕鱼脑硫苷脂纯度为90.74%,与哺乳动物类似,鳕鱼脑硫苷脂的长链碱基以鞘氨醇为主,主要分子种为d18∶1-C24∶1,但脂肪酸的羟基化程度略低,且含少量独特的分子种,如d18∶1-22∶1和d18∶2-25∶2。 相似文献
237.
We analyze a two-year time-series of chromophoric dissolved organic matter (CDOM) light absorption measurements in the upper 400 m of the water column at the BOUSSOLE site in the NW Mediterranean Sea. The seasonal dynamics of the CDOM light absorption coefficients at 440 nm (acdom(440)) is essentially characterized by (i) subsurface maxima forming in spring and progressively reinforcing throughout summer, (ii) impoverishment in the surface layer throughout summer and (iii) vertical homogeneity in winter. Seasonal variations of the spectral dependence of CDOM absorption, as described by the exponential slope value (Scdom), are characterized by highest values in summer and autumn at the surface and low values at the depths of acdom(440) subsurface maxima or just below them. Variations of acdom(440) are likely controlled by microbial digestion of phytoplankton cells, which leads to CDOM production, and by photochemical destruction (photobleaching), which leads to CDOM degradation. Photobleaching is also the main driver of Scdom variations. Consistently with previous observations, acdom(440) for a given chlorophyll a concentration is higher than expected from Case I waters bio-optical models. The total non-water light absorption budget shows that surface waters at the BOUSSOLE site are largely dominated by CDOM during all seasons but the algal bloom in March and April. These results improve the knowledge of CDOM absorption dynamics in the Mediterranean Sea, which is scarcely documented. In addition, they open the way to improved algorithms for the retrieval of CDOM absorption from field or satellite radiometric measurements. 相似文献
238.
微波等离子体炬质谱技术快速鉴别天然石材与人造石材 总被引:1,自引:1,他引:0
天然石材主要有大理石、花岗岩等;人造石材多以不饱和聚酯树脂为基料,添加适量的无机物粉料和添加剂固化制成。由于石材种类繁多,并且各种石材的岩体所含矿物成分也有差异,当前很少应用化学成分分析方法准确、快速鉴别天然和人造石材,仅有的红外光谱法由于对待测物纯度的要求较高而具局限性。本文基于微波等离子体炬源(MPT)同时具有热解吸与强电离能力,能在短时间内离子化待测物的特点,采用微波等离子体炬质谱(MPT-MS)技术,无需样品复杂预处理直接对天然与人造石材进行分析,获得正离子检测模式下在m/z 50~1000之间的石材的指纹谱图,并运用化学计量学的主成分分析(PCA)方法处理所获取的数据,实现了不同建筑石材的区分。结果表明,MPT-MS能够获得石材丰富的指纹谱图,结合PCA方法能够快速鉴别天然石材与人造石材,天然石材中解吸出的物质主要为CO2和H2O的团簇分子;而人造石材中解吸出的主要成分为有机物(人为添加的黏合剂等)。本研究采用的MPT-MS技术无需采用喷雾、激光、基质和加热等方法辅助,并且无需对石材进行任何复杂的处理即可进行质谱分析,从而获取石材表面及内部物质的质谱信息,为快速直接鉴定石材样品提供了一种新的质谱分析方法。 相似文献
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