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1.
刘春峰 《中国无机分析化学》2013,3(Z1):29-30
建立了离子色谱法测定镍钴锰氢氧化物中硫酸根含量的方法。试样以盐酸溶解,挥发除去过量盐酸,经阳离子树脂柱去除金属离子,离子色谱法测定其中硫酸根离子的含量。方法操作简便快速,检出限低,样品测定具有较好的精密度,加标回收率为97%~103%。 相似文献
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元素分析仪法是测定有机元素含量的现代分析技术,一次进样可以同时测定化合物中的C、H、N等元素的含量,在元素含量分析中发挥了重要作用,但该方法对卤族元素无法测定.氧瓶燃烧分解样品后用电位滴定法或称(容)量法测定有机卤素的含量,是有机卤素分析的经典方法.国家标准测定聚氯乙烯样品中的氯含量采用氧瓶燃烧分解电位滴定法[1].电位滴定法一次只能测定样品中一种卤离子,若多种离子同时存在会产生干扰,影响测定结果,且需要配制多种试剂,费时费力.有机样品或聚合物经氧瓶燃烧法分解后采用离子色谱法一次进样可以同时测定多种元素的含量而互不干扰[2],分析速度和灵敏度都优于传统方法.许多有机化合物或聚合物都含有卤素,离子色谱对卤素离子测定的灵敏度很高,氧瓶燃烧离子色谱法弥补了元素分析仪法的不足,是有机化合物或聚合物卤素含量分析较理想的方法.本实验以间氯苯甲酸元素分析标准样品为对照品,测定了氯化聚乙烯中的氯含量,取得满意结果. 相似文献
3.
蔬菜中金属元素测定方法研究 总被引:1,自引:0,他引:1
采用微波消解处理样品,应用离子色谱UV-Vis检测和火焰原子吸收法分别测定了蔬菜样品中的金属元素Fe、Cu、Zn、Ni、Ca、Mn和Mg的含量。结果显示,离子色谱UV-Vis检测法测定结果准确,方便快捷。 相似文献
4.
《化学研究与应用》2015,(11)
由于铅、锌两元素均具有两性性质,铅锌硼玻璃样品中大量的铅离子和锌离子的存在会影响其B2O3含量的分析结果。本文通过实验验证,提出准确测定铅锌硼玻璃中B2O3含量的主要思路:在石墨坩埚中用氢氧化钾将玻璃样品熔融后用盐酸脱出,所得溶液逐步通过硫酸盐沉淀、碳酸盐沉淀和氢氧化物沉淀的方法去除大多数的铅锌离子,随后用0.1 mol·L-1EDTA(乙二胺四乙酸二钠)溶液络合的方法去除残余铅锌离子的存在对B2O3含量测定的影响,最后用酸碱滴定法测定样品中B2O3的含量。通过硼硅酸盐玻璃标准物质和铅锌硼玻璃样品对该方法进行B2O3含量测定的验证试验结果显示,该方法具有较好的准确性。 相似文献
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几种样品中溴与碘的离子色谱安培法测定 总被引:3,自引:0,他引:3
1 引言 许多样品通常要求测定溴和碘的含量,往往含量甚微,电导检测的离子色谱法达不到要求。本文研究了离子色谱安培法连续测定溴和碘的可行性,拟定了一个快速、简便,无干扰的、可同时测定各种样品中痕量溴和碘的方法。本法以艾斯卡半熔,抗坏血酸为还原剂,使样品中的碘全部转变成适合于离子色谱安培法检测 相似文献
8.
对不同地区不同深度的土壤进行前期预处理,在最佳试验条件下,应用离子色谱法测定土壤浸提液中硫酸根和硝酸根的含量,测定的相对标准偏差分别为1.9%和3.0%,加标回收率SO42-90.0%~100.0%、NO3-93.0%~101.0%.样品预处理操作简单,方法灵敏度和准确性高,结果稳定性好,检出限低,能满足土壤环境样品检验的要求. 相似文献
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10.
萤石中氟化钙的测定,多是通过测定钙换算成样品中氟化钙含量。这些测定方法操作繁琐,准确度低。近年来有人试图用氟离子选择性电极测定氟矿中的氟含量,只是应用上的报导还不多。本文研究了热解-电位滴定及酸碱滴定测定萤石中氟化钙的适宜条件,并提出了简单快速、切实可行的分析方法。 相似文献
11.
研究了腐植酸(HA)存在下冰相体系中γ-六氯环己烷(γ-HCH)的光转化规律.结果表明,HA浓度对γ-HCH的光转化率呈现低浓度促进而高浓度抑制的现象;盐离子浓度、NO_2~-及NO_3~-对γ-HCH的光转化率均有促进作用;低浓度Fe~(3+)对γ-HCH的光转化率有促进作用,当Fe~(3+)的浓度增大到50μmol/L时,呈现抑制效应;γ-HCH在不同p H值条件下光转化速率的大小顺序为碱性中性酸性.冰相中HA通过产生单线态氧(~1O_2)、羟基自由基(·OH)及三重激发态(HA*)加速γ-HCH的光转化.HA存在下γ-HCH的光转化产物主要是五氯环己烯、邻二氯苯和对二氯苯、一氯苯,光转化过程中~1O_2通过消耗中间产物间接加速了γ-HCH的光转化过程. 相似文献
12.
The simultaneous determination of major impurities present in Antarctic snow and ice at ng g? (ppb) concentrations by ion chromatography is described. Calibration data are presented for ammonium, sodium, potassium, chloride, nitrate and sulphate ions. Special attention is paid to the different ways of removing field contamination from ice and snow cores and suitable equipment is described. The results provide evidence against the validity of published sets of concentration data for nitrogen-containing compounds (NO?3 and NH+4 in Antarctic snow, and demonstrate a crucial contamination problem in the determination of ammonium ions. 相似文献
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从采自青藏高原阿汝和古里雅冰川的两支冰芯中选取31个样品,分别用三种仪器对比分析K^+、Na^+、Ca^2+、Mg^2+四种水溶金属离子,寻求最佳分析方案。分析结果对比发现,电感耦合等离子体发射光谱(ICP-OES)法在K+测量中存在困难,而离子色谱(IC)法和电感耦合等离子体质谱(ICP-MS)法均能够满足要求,且分析结果具有高度的一致性,四种离子的相关系数(R2)均在0.97以上,且并未出现ICP-MS法比IC法测量值明显偏高的现象。因此,除IC法外,ICP-MS法也是检测青藏高原雪冰样品中水溶金属离子的有效手段,其测定速度更快,且可以同时进行微、痕量元素检测,适用于大批量冰芯样品的快速分析。 相似文献
14.
M. Severi S. Becagli E. Castellano A. Morganti R. Traversi R. Udisti 《Microchemical Journal》2009,92(1):15-20
The aim of this study was to use ion chromatographic methods to measure trace species under clean conditions in Antarctic snow samples. Both anionic and cationic contents of the snow samples were measured using preconcentration columns for both the ion chromatographic systems due to the low concentrations typical of Antarctic snow and ice samples. Samples were collected from a snow-pit dug in Talos Dome (East Antarctica) during the 2003-2004 Italian Antarctic Campaign to perform a preliminary survey of the site chosen for deep drilling in the framework of the TALos Dome ICE core (TALDICE) international project. Stratigraphic dating was attempted for the entire snow-pit, covering about 30 years, in order to achieve climatic information from the chemical profiles of the measured species. In particular, ions coming mainly from biogenic sources were investigated as potential markers for historical reconstruction of parameters expressing atmospheric and oceanic circulation, such as Southern Oscillation Index (SOI). For the studied period, a good correlation between biogenic species and SOI and sea-ice extent in the Ross Sea sector was observed, suggesting that these ions, as recorded in Talos Dome, can be used as markers for the reconstruction of the oceanic and atmospheric conditions in the past. 相似文献
15.
讨论了1 ,2 ,3不对称取代咪唑啉盐各种离子的生成途径以及取代基对裂解方式的影响并分析了该类化合物的主要裂解方式。在所有实验中均有 m/z = 127( I+ ) 的离子峰和有机正离子 A 峰存在,表明化合物1 和2 均为有机正离子和碘离子形成的盐。化合物1 和2 的质谱有相似的裂解方式:有机正离子发生失掉氮原子上的一个取代基而保留咪唑啉环产生 D, E, F 离子的裂解方式。更重要的是咪唑啉环有相同的裂解方式: C2 N3 键和 C5 N1 键同时断裂产生 G 离子碎片,以及 C2 N3 键和 C4 C5 键同时断裂产生 H 离子碎片。由于化合物1 和2 环上所连接的取代基不同而导致了其质谱裂解方式和程度的差异。化合物2 的有机正离子 A部分较稳定,质谱中表现为基峰,其 E, F 离子峰很弱;化合物1 的有机正离子 A 稳定性差,其相对丰度很小,其 E, F 离子峰较强。化合物1c ,1d ,1e 的质谱中出现了比 A 离子少三个单位的 C 离子峰,这是一种较特殊的裂解方式。 相似文献
16.
Clean conditions for the determination of ultra-low levels of mercury in ice and snow samples 总被引:1,自引:0,他引:1
Laboratory facilities and methods are presented for the determination of ultra-low levels of mercury (Hg) in ice and snow samples originating from polar ice caps or temperate regions. Special emphasis will be given to the presentation of the clean laboratory and the cleaning procedures. The laboratory is pressurized with air filtered through high efficiency particle filters. This first filtration is not enough to get rid of contamination by Hg in air. Experiments are conducted in a clean bench, especially built for Hg analysis, equipped with both particle filter and activated charcoal filter. It allows to obtain very low levels of atmospheric Hg contamination. Ultrapure water is produced for cleaning all the plastic containers that will be used for ice and snow samples and also for the dilution of the standards. Hg content in laboratory water is about 0.08+/-0.02 pg/g. A Teflon system has been developed for the determination of Hg in ice and snow samples based on Hg(II) reduction to Hg(0) with a SnCl2/HNO3 solution followed by the measurement of gaseous Hg(0) with a Hg analyzer GARDIS 1A+ based on the Cold Vapor Atomic Absorption Spectroscopy method. Blank determination is discussed. 相似文献
17.
A spectrophotometric method for the determination of ionic surfactants with Bromophenol Blue (BPB) based on incorporation into a precipitated chitosan was studied. Cationic surfactants (CS+), such as a quaternary ammonium ion containing a long-chain alkyl group, associate with BPB2- buffered at about pH 9 to form the ion associate (CS+)2 x BPB2-. CS+ associates with anionic surfactants (AS-). In the presence of a definite amount of CS+, an increase in the amount of AS- leads to a decrease in the amount of excess CS+, and therefore to a decrease in the amount of the ion associate of CS+ with BPB2-. The addition of a chitosan dissolved in acetic acid to a solution containing these ion associates leads immediately to precipitation of the chitosan and the incorporation of the ion associates (CS+)2 x BPB2- or CS+ x AS- into the precipitated chitosan. After centrifuging, ionic surfactants can be determined by the following two methods: (1) the absorbance of the supernatant solution is measured at 590 nm. (2) After the supernatant solution is separated, the precipitate is dissolved in an acetic acid solution and the absorbance is measured at 625 nm. Because the color of the precipitate is judged by the naked eye, this can be applied to the visual method. This is a simple and rapid method for the determination of a 10(-6) M order of ionic surfactants. 相似文献
18.
Ponciano CR Martinez R Farenzena LS Iza P da Silveira EF Homem MG Naves de Brito A Wien K 《Journal of the American Society for Mass Spectrometry》2006,17(8):1120-1128
Condensed CO and CO2 are bombarded by approximately 65 MeV 252Cf fission fragments and the desorbed ions are analyzed by time-of-flight mass spectrometry as a function of target temperature, in the ranges 25-33 K and 75-91 K, respectively. Absolute desorption yields are measured up to complete ice sublimation. The mass spectra of both ice targets reveal the emission of: (1) low mass ions, produced by direct Coulomb interaction of the highly charged projectiles and delta-electrons with CO and CO2, and (2) pronounced series of cluster ions. The basic ice cluster structures (CO)n and (CO2)n are present in the emitted cluster series such as (CO)nCO+, (CO2)nCO2+, or (CO2)nCO3-. In the case of CO ice, however, the intense production of the series Cn+, Cn-, and (CO)mCn+ shows that Cn is the main cluster structure, consequence of a higher concentration of free carbon atoms in the nuclear track plasma of CO ice than in that of CO2 ice. Ion cluster abundance is observed to decrease exponentially with cluster mass. The decay constant is k(n) congruent with 0.13, about the same for series based on (CO)n and (CO2)n, but a factor 3.3 higher for the Cn series. The Cn clusters are formed by gas-phase condensation, but the (CO)n and (CO2)n clusters are produced by fracturing of the highly excited solid around the nuclear track. A dramatic reduction of the ion desorption yield is observed near T = 29 K for CO and near T = 85 K for CO2, when fast sublimation occurs and ice thickness vanishes. Close to sublimation temperature, the decay constant of the (CO)2Cn+ series increases due to a decreasing formation probability of large Cn clusters. 相似文献
19.
C. P. Ferrari A. L. Moreau C. F. Boutron 《Analytical and bioanalytical chemistry》2000,366(5):433-437
Laboratory facilities and methods are presented for the determination of ultra-low levels of mercury (Hg) in ice and snow samples originating from polar ice caps or temperate regions. Special emphasis will be given to the presentation of the clean laboratory and the cleaning procedures. The laboratory is pressurized with air filtered through high efficiency particle filters. This first filtration is not enough to get rid of contamination by Hg in air. Experiments are conducted in a clean bench, especially built for Hg analysis, equipped with both particle filter and activated charcoal filter. It allows to obtain very low levels of atmospheric Hg contamination. Ultrapure water is produced for cleaning all the plastic containers that will be used for ice and snow samples and also for the dilution of the standards. Hg content in laboratory water is about ¶0.08 ± 0.02 pg/g. A Teflon system has been developed for the determination of Hg in ice and snow samples based on Hg(II) reduction to Hg(0) with a SnCl2/HNO3 solution followed by the measurement of gaseous Hg(0) with a Hg analyzer GARDIS 1A+ based on the Cold Vapor Atomic Absorption Spectroscopy method. Blank determination is discussed. 相似文献
20.
DX-300离子色谱测定山地冰川雪冰中的有机酸与无机酸阴离子 总被引:9,自引:0,他引:9
利用AS4A SC分离柱 ,AG4A SC保护柱 ,ASRS Ⅱ抑制器 ,TAC 2阴离子富集柱和ATC 1阴离子捕集柱 ,以四硼酸钠 (Na2 B4O7)为淋洗液试剂 ,2 5mmol/LH2 SO4为化学抑制的再生液 ,采用梯度淋洗方式 ,对中国天山乌鲁木齐河源一号冰川雪冰中的生物有机酸和无机酸阴离子进行了测试分析。 2mL雪冰融水样品可在 16min内通过一次进样检测出氟离子、乙酸根离子、甲酸根离子、丙酮酸根离子、一氯乙酸根离子、氯离子、亚硝酸根离子、溴离子、硝酸根离子、磷酸根离子、硫酸根离子和草酸根离子共 10多种有机酸和无机酸阴离子。 相似文献