102 resultados para ICP-AES
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本文介绍了一种新型延长炬管的设计。该炬管使在电感耦合等离子体原子发射光谱仪(ICP-AES)上同时测定氮及其它金属元素成为可能,并且在不同程度上改善了一些金属元素的检测限。本文利用该炬管,在ARL3520光谱仪上同时测定了生物标准样品中的氮及Fe、Mn、CuZn等四种金属元素。结果与定值吻合,相对标准偏差均小于5%。
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本论文由三部分组成。第一部分是文献综述。首先从检出限、基体效应、光谱干扰及其校正、实际应用四个方面介绍了ICP-AES用于稀土元素分析的研究概况。然后,较全面深入地评述了有机试液的ICP-AES光谱分析技术的研究进展,讨论了有机溶剂对ICP放电稳定性的影响及提高稳定性的途径,有机试剂对背影和分析元素谱线强度的影响及其原因,比较了“有机ICP”和“水溶液ICP”的分析化学特性,详细地介绍了ICP-AES在各种有机试液直接分析中的应用。第二部分是稀土元素的ICP-AES分析的研究。首先测定了十五种稀土元素192条灵敏线的ICP-AES摄谱法的检出限和工作曲线线性范围。然后重点进行了乙醇溶剂的预去溶研究,即把预去溶进样的特点和乙醇的较高挥发性结合起来借以提高玻璃同心雾化器的进样效率,合稀土元素谱线速度显著增大,检出限改善5-12倍;同时研究了进样效率提高的机理以及去溶装置的去溶效率,发现残余乙醇进入ICP对谱线强度有抑制作用。详细地研究了由于乙醇导入ICP而产生的CN带对稀土元素灵敏线的干扰及CN带强率与ICP工作条件的关系,指出适当增加炸管的外管长度可以十分有效地抑制CN带。最后以纯Y_2O_3的ICP-AES分析为例,研究了基体对分析元素谱线强度的影响及基体效应的产生机理,提出用外加内标法代替通常的基体匹配法来克服基体效应,分析方法用于纯Y_2O_3中十四个稀土杂质的测定,获得较为满意的结果。第三部分是乙醇导入时ICP激发特性的研究,主要包括以下内容。(1)观察了乙醇对谱线强度的影响及这些影响与元素电离电位和谱线激发电位的关系,发现随乙醇浓度增大,经溶液进炬速率校正以后的“硬线”强度单调减小,而“软线”强度则出现极小值,以此结果为基础确定了某些未分类稀土元素光谱线的电离态并估测了它们的激发电位。(2)详细地研究了乙醇对ICP激发温度、气体温度、电子数密度以及易电离元素基体效应的影响,讨论了乙醇导入时分析元素在ICP中的电离过程的变化及“有机ICP”的热平衡特性。(3)研究了乙醇对ICP能量输适的影响,发现随乙醇浓度增大,等离子体电流减小,导致等离子体短体积增大(即“有机ICP”的扩张效应),可能使分析物在等离子体中的往向扩散得到增强。最后列出了305篇参考文献。全文共有图66个、表33个。
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揭示苔藓植株元素含量及其时空差异性是深入开展利用苔藓植物指示环境和筛选理想监测藓种的科学基础。采用微波消解(ICP-AES)方法对九寨沟自然遗产地原始林景点停车场周围三个采样带:I为停车场植被小岛(PS),向外约120 m半径为II带(D120),再向外距离约1,000 m为III带(D1000)和3个方向上的大羽藓和毛尖青藓2种苔藓中13种元素(A1, S, Ca, P, Cu, Fe, K, Mg, Mn, Pb, Ni,Zn和Cd)含量进行了测定和比较,并对采自边坡方向(PS-3)上2005和2007年的4种苔藓植物(南木藓、大羽藓、平藓和厚角絹藓)也进行了13种元素含量的测定和比较。同时对九寨沟自然遗产地、黄龙自然遗产地、夹金山和梦笔山的冷杉原始林4个地区的3种苔藓中(大羽藓、锦丝藓和塔藓)的A1、Ca、Cu、Fe、K、Mg、P、Zn、C和N 10种元素含量进行测定和比较。 对大羽藓和毛尖青藓2种苔藓植物内13种元素的测定发现:1)同种苔藓对不同元素的富集能力不同。A1、Ca、K、Mg和P的元素含量在苔藓中的富集较其他元素的要高。2)不同种苔藓植物对同种元素的富集能力不同,毛尖青藓较大羽藓能够监测出更多的元素;对于被检测出的元素,毛尖青藓监测出的累积量大于大羽藓,其中累积量最大的元素是Ca为10 874.286 μg.g-1.year-1,最小的是Cu元素为5.438 μg.g-1.year-1。对05年和07年的平藓、大羽藓、南木藓和厚角絹藓元素含量的测定表明:元素在两年中的积累量是不同的。综合分析表明,苔藓生物监测方法可有效监测景点停车场机动车尾气中排放出的典型元素(如Cu、Pb、Ni、Zn、Cd等)含量,而毛尖青藓较大羽藓能更可靠的监测九寨沟自然遗产地单景点汽车尾气金属元素种类及其排放量。 对4个地区3种苔藓10种元素监测发现:1)Ca、Mg、Zn、K和Cu元素在黄龙地区的含量高于在其它地区的含量;P元素在梦笔山地区的含量为最高;Fe和Al元素在夹金山地区的含量高于在其它地区的含量。2)C元素在其它因素一致的情况下,进行不同年龄间的元素含量比较,结果显示元素含量在各年龄间并不存在明显的差异性;N元素含量与年龄的差异出现在黄龙林下及林窗的塔藓、九寨沟林下的锦丝藓及塔藓和梦笔山的塔藓中,而在锦丝藓中未出现元素含量与年龄的差异性;塔藓能检测出更多的元素种类其含量与年龄间存在显著差异,锦丝藓检测到的元素种类次之;除锦丝藓(锦丝藓在林窗中几乎检测不到元素含量与年龄间的差异性)外,其他两种藓在林窗中能检测出的元素种类大于在林下的检测种类。3)元素含量与生境间存在差异性的元素分别有:黄龙大羽藓中的Ca、P和Mg元素;九寨锦丝藓中的Zn元素;夹金山塔藓中的Al、Fe和Zn元素;梦笔山大羽藓中的Al、Fe和Mg元素及锦丝藓中的Ca元素。4)区域、年龄和生境因素对苔藓植株元素含量均达到了显著水平,但两两之间及三者之间的交互作用由于元素种类的不同存在差异。综合分析表明,苔藓植物中的元素含量受年龄、区域的影响较生境的更大。 The revelation of mosses elements content and its spatiotemporal differences is the scientific foundation of moss monitoring. To determine the feasibility of moss monitoring metal depositions derived from travel bus emiss ions in scenic spot, we collected one year-growth samples of two mosses Brachythecim piligerum and Thuidium cymbifolium with different distance (island center, 120m,1000m ) and different direction (north, south and east) far from parking site island from Yuanshilin Spot at Jiuzhaigou World Nature Heritage in the Western Sichuan of China and determined thirteen element (A1, S, Ca, P, Cu, Fe, K, Mg, Mn, Pb, Ni, Zn, Cd)contents by ICP-AES analysis method. And picked 4 kinds of mosses (Macrothamnium macrocarpu m(Reinw. etHornsch.)Fleisch.,Thuidium cymbifolium,Entodon concinnus (De Not.) Par., Neckera pennata) from the direction PS-3 in 2005 and 2007, determined 13 element contents. Collected 3 kinds of moss (Thuidium cymbifo lium, Actinothuidium Hookeri (Mitt.) and Hyolcomium splendens (Hedw.) from Jiuzhaigou natural heritage, Huanglong natural heritage, Mt. Jiajin and Mt. Mengbi in primeval forest with two habitat (undergrowth and forest gap), determined element contents of A1, Ca, Cu, Fe, K, Mg, P, Zn, C and N. We found that, 1) The elements content are difference in same type of moss. Content of A1, Ca, K, Mg and P are higher than others. 2) While the contents of A1, S, Ca, P, Cu, Fe, K and Zn had significant correlation with the different distances from parking site, the nearer the distance was, the more accumulation was; 2) Comparing to Thuidium cymbifolium, Brachythecium piligerum can test more elements which contents show the significant correlation with distances. And Brachythecium piligerum can have greater element accumulation than Thuidium cymbifolium. The element contents in two years (2005 and 2007) are different. The present study found that moss can reliably bio-indicate metal deposition from traffic emissions in one scenic spot and Brachythecium piligerum is a good moss for bio-indicating element content from traffic emissions at Jiuzhaigou World natural Heritage. Determined the 10 element contents in 4 areas through 3 kinds of moss we found that, 1) Ca, Mg, Zn, K and Cu element content is higher in the Huanglong area than in other areas, The P element content in Mt. Jiajin is higher than other areas, Fe and Al element content is higher in the Mt. Jiajin than in other areas. 2) The content of C had no significant correlation with age. As for N, this significant correlation found in Hyolcomium splendens (Hedw.) with 2 habitat in Huanglong, Actinothuidium Hookeri (Mitt.) and Hyolcomium splendens (Hedw.) with undergrowth in Jiuzhai, Hyolcomium splendens (Hedw.) in Mt. Mengbi. The types of elements which content showt he significant correlation are most in Hyolcomium splendens (Hedw.) and least in Thuidium cymbifolium. Except Actinothuidium Hookeri (Mitt.), the types of elements that content had significant correlation with age in forest gap are more than in undergrowth. 3) The elements which content had significant correlation with habitat are P, Ca and Mg in Thuidium cymbifolium in Huanglong, Zn in Actinothuidium Hookeri (Mitt.) in Jiuzhai, Al, Fe and Zn in Hyolcomium splendens (Hedw.) in Mt. Jiajin, in Mt. Mengbi Al, Fe and Mg in Thuidium cymbifolium and Ca in Actinothuidium Hookeri (Mitt.). 4)The region, the age and the habitat factor has coeffect element content. The correlationship between element contents and the age, the region is closer than habitat.
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采用微波消解、电感耦合高频等离子体原子发射光谱(ICP-AES)的方法,对62份不同小麦品种(系)中锌、铁、铜、钙、钠和钾的含量进行了测定。同时利用红外线品质测定仪对主要品质指标粗蛋白、湿面筋、沉降值进行了测定。结果表明,不同小麦品种(系)中各种矿质元素的含量存在差异,2006年小麦品种中铁含量变幅为18.55-58.19 ug/g,平均为30.83ug/g ,最高与最低的相差39.64ug/g;锌含量变幅为5.70-25.80 ug/g,平均为15.13ug/g ,最高与最低相差20.10ug/g。2008年小麦品种(系)中铁含量变幅为16.68-52.25 ug/g,平均为30.10ug/g,最高与最低相差35.58ug/g;锌含量变幅为12.29-33.47 ug/g,平均为21.11ug/g,最高与最低相差21.18ug/g;钙含量变幅为167.53-348.80ug/g,平均为248.59ug/g,最高与最低相差192.59ug/g;铜含量变幅为2.32-5.83 ug/g,平均为2.98ug/g,最高与最低的相差3.61ug/g;钾含量变幅为1822.71-4414.91 ug/g,平均为2617.87ug/g,最高与最低的相差2634.72ug/g;钠含量变幅为10.25-39.82 ug/g,平均为23.05ug/g,最高与最低的相差29.57ug/g。 两年不同小麦品种(系)中矿质元素的含量分析结果表明:铁、铜、钙、钠和钾含量年际变化不明显,说明小麦对铁、铜、钙、钠和钾的吸收较稳定;锌含量变化较大,可能受环境的影响比较大。分析各矿质元素含量与粗蛋白、湿面筋、沉降值及元素之间的相关关系,结果表明,锌含量与粗蛋白含量呈极显著正相关关系,相关系数为0.317,与湿面筋含量之间呈显著正相关,相关系数达到0.246;铁含量与粗蛋白含量呈显著的正相关关系,相关系数是0.262;铜、钙、钠和钾含量与粗蛋白含量、湿面筋和沉降值之间存在正相关,但不显著,其中钠与沉降值之间为负相关。表明施锌或铁对提高小麦粗蛋白和湿面筋有显著效应,其余矿质元素有促进作用但不明显。 利用RAPD分子标记技术对川育23、41058、川育20及其父母本进行分析,力图从分子水平找到小麦矿质元素含量之间的差异性,琼脂糖电泳结果表明不同的小麦品种(系)间扩增出了差异条带。 以上研究结果,将对筛选“微量营养强化型”小麦新材料,选育“微量营养强化型”小麦新品种奠定基础。 62 different wheat cultivars was digested with HNO3 in a tightly closed vessel heated under micro-wave,then contents of zinc,iron,copper,calcium,sodium and potassium were determined by inductively coupled plasma-atomic emission spectroscopy(ICP-AES).The main indexes of wheat quality such as total protein、wet glu and sedimentation volume were detected by Infratec 1255 Food & Feed Analyzer at the same time.The obtained results showed that variation for all of the mineral elements concentrations among different cultivars were observed .In 2006, the amplitude variation of the iron content was 18.55-58.19 ug/g,the average value was 30.83ug/g,and 39.64ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the zinc content was 5.70-25.8 ug/g,the average value was 15.13ug/g,and 20.10ug/g between the highest-content cultivar and the lowest one.In 2008, the amplitude variation of the iron content was 16.68-52.25 ug/g,the average value was 30.10ug/g,and 35.58ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the zinc content was 12.29-33.47 ug/g,the average value was 21.11ug/g,and 21.18ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the calcium content was 167.53-348.80ug/g,the average value was 248.59ug/g,and 192.59ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the copper content was 2.32-5.83 ug/g,the average value was 2.98ug/g,and 3.61ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the potassium content was 1822.71-4414.91 ug/g,the average value was 2617.87ug/g,and 2634.72ug/g between the highest-content cultivar and the lowest one; the amplitude variation of the sodium content was 10.25-39.82 ug/g,the average value was 23.05ug/g,and 29.57ug/g between the highest-content cultivar and the lowest one. Analysis was made on the annual variation of mineral elements content in different Wheat cultivars ,the result shows:there is no obvious difference of iron ,copper ,sodium、calcium and potassium concentrations in wheat cultivars, suggesting the absorption of the iron, copper, sodium、calcium and potassium by wheat are relatively steady ,but zinc concentrations change obviously ,maybe influenced heavily by environment . The correlation between mineral elements 、mineral elements and total protein、mineral elements and sedimentation volume as well as mineral elements and wet glut were analysed in this paper, the result showed that there was significant positive correlation between zinc content and total protein (the correlation coefficient is 0.317), positive correlation between zinc content and wet glu (the correlation coefficient is 0.246), positive correlation between iron content and total protein (the correlation coefficient is 0.262). there was positive but not obvious correlation between the contents of copper, calcium, sodium or potassium and total protein, wet glut or sedimentation volume,among which was negative correlation between sodium and sedimentation volume.It was indicated zinc or iron fertilization has prominent effects in improving the total protein in wheat, the rest mineral elements have Non- obvious facilitation. The study then forecasted the genetic difference of different wheat by the molecular marker of RAPD in order to find differences in molecular level. Chuanyu23、41058、chuanyu20 as well as their male and female parents were analysed by RAPD markers,Agarose gel electrophoresis of DNA revealed the appearance of differential bands . The above-mentioned results of this study establish the foundation to screening the new materials of wheat of " strengthening type of micro- nutrition ", and to breeding the new wheat cultivars of" strengthening type of micro- nutrition ".
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本研究应用微波消解ICP-AES 法对62 个小麦品种及3 个地区土壤的锌铁硒含量进行了分析测定,发现不同小麦品种中微量元素含量差异很大,姊妹系间也存在差异。含铁量最高与最低的小麦品种铁含量相差29.68mg/kg。含锌量最高与最低的小麦品种锌含量相差46.70 mg/kg。含硒量最高与最低的小麦品种硒含量相差0.056 mg/kg。对不同地点的小麦及土壤中锌铁硒含量进行方差分析,发现双流和西昌两地种植小麦的铁含量和硒含量均有显著差异,西昌和荣县种植的锌含量有显著差异。在3 个地点中双流种植小麦硒含量最高,西昌种植小麦的铁和锌含量最高。 通过对小麦微量元素含量与土壤中微量元素含量进行了相关性分析,结果表明:小麦中的锌铁含量与土壤中的锌铁含量呈显著正相关,土壤中铁与锌含量呈极显著正相关,小麦中铁与锌含量也呈极显著正相关。随着土壤微量元素锌铁的提高,小麦中的锌铁元素含量同时提高,而且小麦对两种元素的吸收互相促进。土壤中的硒含量与锌铁含量呈负相关。小麦中硒含量也与锌铁含量也呈负相关。说明锌和铁与硒互相拮抗。小麦硒含量与土壤硒含量呈正相关,但不显著。表明土壤硒含量可以影响小麦硒含量,但不是决定因素,小麦硒含量与小麦自身因素有关。 对姊妹系G290(高硒含量)和G289(低硒含量)进行抗重金属胁迫和抗旱性实验发现,高硒品种G290的抗逆性优于低硒品种G289。 利用RAPD 技术对7 个姊妹系进行遗传差异分析发现,高硒材料G290出现了特异条带,分别标为1、2、3、4,其他姊妹系品种中未发现特异条带,回收4 条特异条带并连接转化,得到目的片段1、2、3 的重组子,进行测序。NCBI 中结果显示没有找到植物中的同源序列,说明特异序列可能是未发现的基因片段,推测可能与小麦硒含量有关,有待进一步研究。 以上研究结果,对小麦营养研究及功能性小麦的筛选和栽培具有指导作用。 In this study, we determinated the contents of zinc, iron, selenium in 62 wheat cultivars and soil samples of three regions by method of microwave digestion/ ICPAES,found that there was great difference of zinc, iron, selenium contents in different wheat cultivars as well as different sister lines. Iron content difference was 29.68 mg/kg between the highest-iron-content cultivar and the lowest one, and zinc content difference was 46.70 mg/kg , selenium content difference was 0.056 mg/kg. Anova analysis was made on contents of zinc, iron, selenium in wheat and soil samples of different locations, significant differences of Fe and Se contents were found between wheat in Shuangliu and Xichang, significant difference of Zn content was found between wheat in Xichang and Rongxian. Se content in wheat of Shuangliu was highest, Fe and Zn contents in wheat of Xichang were highest. Relativity analysis was made on three trace elements in Wheat and in soil, the result showed that there was significant positive correlation of zinc, iron content between in Wheat and in soil, as well as between Fe and Zn both in wheat and in soil. With the improving of Zn, Fe contents in soil, contents of Zn and Fe in wheat increased and absorption of Zn and Fe in wheat will mutual promote. Negative correlation of Se and Zn contents was found in wheat and soil, but not significant, that meant the antagonism of Se and Zn. Positive correlation of Se content in wheat and soil was found. High selenium content G290 and low selenium content G289 in sister lines were selected for heavy metal stress and drought resistance experiments, the result showed that the resistance of high-selenium-content cultivar was better than low selenium one. Analysis on genetic difference was made by RAPD, and specific bands were selected, marked 1,2,3,4, no more specific bands were found in other sister lines.4 bands were recovered, ligated to T-vector and transformed E.coli. Three recombinant plasmids were obtained and sequenced. NCBI Blast showed there was no homology with other plants. It implied that these fragments probably be new genes and maybe were related to selenium in wheat. It needs further research. This paper would be useful for the study of wheat nutrition as well as selection and cultivation of functional wheat.
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By characterizing fresh and used Mo/HMCM-22 catalysts with ICP-AES, XRD, NH3-TPD technique, UV - Vis DRS and UV Raman spectroscopy, the reactivity of Mo species for methane partial oxidation into formaldehyde were directly studied with a new point of view. By comparing the fresh and used catalysts, it was found that the tetrahedral Mo species bonding chemically to the support surface were practically unchanged after the reaction, while the polymolybdate octahedral Mo species, which had a rather weak interaction with the MCM-22 zeolite, leached out during the reaction, especially when the Mo loading was high. Correspondingly, it was found from the time-on-stream reaction data that the HCHO yield remained unchanged, while COx decreased with the reaction time during the reaction. By combining the characterization results and the reaction data, it can be drawn that the isolated tetrahedral molybdenum oxo-species (T-d) is responsible for HCHO formation, while the octahedral polyoxomolybdate species (O-h) will lead to the total oxidation of methane.
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结合国内外的研究进展,综述了环境介质中硒的各种检测方法。其中重点介绍了比较常用的测定方法,如原子吸收光谱法(AAS)、原子荧光光谱法(AFS)和电感耦合等离子体原子发射光谱法(ICP-AES)等,并展望了硒在检测方法上的发展趋势。
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Arabinogalactan derivatives conjugated with gad olinium-diethylenetriaminepentaacetic acid (Gd-DTPA) by ethylenediamine (Gd-DTPA-CMAG-A(2)) or hexylamine (Gd-DTPA-CMAG-A(6)) have been synthesized and characterized by means of Fourier transform infrared spectra (FTIR), C-13 nuclear magnetic resonance (C-13 NMR), size exclusion chromatography (SEC), and inductively coupled plasma atomic emission spectrometry (ICP-AES).
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The nano-scale luminescent complex of Terbium(III)-trimesic acid (TMA)-1,10-phenanthroline(phen) was successfully synthesized by co-precipitation method in this paper. The chemical formula of the synthesized complex was speculated to be Tb(TMA)(phen)(0.0125)center dot 5H(2)O by elemental analysis, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Fourier-transform infrared spectroscopy (FTIR). XRD pattern of Tb(TMA)(phen)(0.0125)center dot 5H(2)O indicated that it was a new crystalline complex since the diffraction angle, diffraction intensity and the distance of crystal plane were all different from those of the two ligands. TG curve proved that the synthesized nano-scale luminescent complex was stable in the range from ambient temperature to 464 degrees C in air. TEM images showed that the complex was spherical shape with an average size of 40 nm.
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用真空电弧熔炼合成了稀土基AB2 型合金.真空电弧合成的稀土基AB2 型合金不具有Laves Phase 的单相结构,而是由多相组成.用XRD、SEM和XPS 对多次充/放电循环后电极合金结构、形貌进行了分析,用ICP-AES 分析电介质溶液中电极合金组成元素的含量,探索了稀土基AB2 型合金作为金属氢化物电极的衰变机理.实验结果表明:腐蚀是稀土基AB2 型合金氢化物电极合金结构变化和电化学性能衰变的主要原因.
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Macromolecular conjugates of two kinds of natural polysaccharides, that from Panax quinquefolium linn (PQPS) and Ganoderma applanatum pat (GAPS), with gadolinium-diethylenetriaminepenta-acetic acid (Gd-DTPA) have been synthesized and characterized by means of FTIR, elementary analysis and ICP-AES. Their stability was investigated by competition study with Ca2+, EDTA (ethylenediaminetetraacetic acid) and DTPA. Polysaccharide-bound complexes exhibit T-1 relaxivities of 1.5-1.7 times that of Gd-DTPA in D2O at 25degreesC and 9.4T. MR imaging of Sprague-Dawley (SD) rats showed remarkable enhancement in rat liver and kidney after i.v. injection of these two complexes: liver parenchyma 60.9+/-5.6%, 57.8+/-7.4% at 65-85 min; kidney 144.9+/-14.5%, 199.9+/-25.4% at 10-30 min for PQPS-GdDTPA, GAPS-Gd-DTPA at gadolinium dose of 0.083 and 0.082 mmol/kg, respectively. Our preliminary in vivo and in vitro study indicates that the two kinds of polysaccharide-bound complexes are potential tissue-specific contrast agents for MRI.
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Arabinogalactan-Gd-DTPA was synthesized by the reaction of diethylenetriaminepenta-acetic acid (DTPA) bisanhydride with polysaccharide in dry DMSO and characterized by FTIR, elemental analysis and ICP-AES. Its stability was investigated by competition with Ca2+, EDTA, DTPA. The t(1)-relaxivity is 8.06 mmol(-1) . L . s(-1) in D2O, 8.48 mmol(-1) . L . s(-1) in 0.725 mmol . L-1 BSA, respectively. t(1)-weighted MR imaging of rat kidney and liver showed a remarkable enhancement post injection of Arabinogalactan-Gd-DTPA. The results indicate that the arabinogalactan-Gd-DTPA is a potential contrast agent for MRI.
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碳电极表面的修饰在电化学和材料科学中很重要 .最近 ,通过层与层电子间的相互作用来自组装修饰玻碳电极已引起人们的关注 [1] .运用这种方法可将一些功能团修饰到电极表面 ,赋予电极一些新的功能 [2 ] .过渡金属取代的多金属氧酸盐不仅在配位环境 ,而且在催化活性方面都类似于金属卟啉和其它大环配体金属配合物 [3] .将其修饰到玻碳电极表面已有文献报道 [4 ] .由于修饰电极的厚度可控、成分可调及具有良好的电催化活性 ,在生物传感器和电子器件等方面具有潜在的应用前景 .取代型夹心型多金属氧酸盐具有大摩尔质量和高电荷密度 ,表现出优秀的磁性和催化活性 [5] ,将成为玻碳电极表面的修饰材料 .我们首次制备了四铁取代的夹心型钨砷酸盐 Na12 [Fe4 ( H2 O) 2 ( As2 W15O56 ) 2 ]·41 H2 O,通过元素分析 ,IR,UV和 NMR对其进行了表征 ,并通过自组装将其修饰到玻碳电极表面形成多层膜 .此修饰电极对 NO- 2 和 H2 O2 具有电催化活性 ,可望成为检测 NO- 2 和 H2 O2 浓度的探针 .1 实验部分1 .1 仪器和试剂 ICP- AES等离子体发射光谱仪 ...
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合成了阿拉伯半乳聚糖修饰的 DTPA钆配合物 ,用红外光谱、元素分析、 ICP-AES等手段进行了表征 ,用竞争性方法研究了其在水溶液中的稳定性 ,测试了其在水中及 BSA溶液中的弛豫性能 ,并进行了体内成像实验 .结果表明 ,其弛豫效率是目前临床所用造影剂 Gd-DTPA的 1 .5~ 2 .0倍 ,对肝脏和肾脏 MRI信号具有良好的增强效果 ,是比较好的潜在磁共振成像造影剂
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用电感耦合等离子体原子发射光谱法 (ICP AES)测定了 11种东北大豆中大量、小量和微量元素。比较了两种湿法消解方法 ,HNO3 HClO4,HNO3 H2 SO4和干灰化法对分析结果的影响。由于大豆含有较多的油脂 ,用混合酸消解时费时较长且需加入较多的酸 ,从而可能产生较高的背景空白 ,因此对大豆样品的前处理采用干灰法较为合适。大豆中钾和磷是大量元素 ,本工作还研究了钾和磷对其他元素测定的影响。结果表明 ,大豆中钾和磷对其他微量元素的测定没有影响。结果还表明 ,这 11种大豆中的各微量元素的含量没有显著性差异