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31.
It is the first time that boron is determined in the presence of a little methanol by discoloring spectrophotometry in this paper. A russety product can be formed by the reaction between glycine (Gly) and sodium 1,2-naphthoquinone-4-sulfonate (NQS) in alkaline solution. When boron is added to the solution, the system will be discolored, and the addition of a little methanol will improve the discoloration. Beer's law is obeyed in the range of boron concentrations of 0.86-43.24 μg ml−1 at the maximal discoloring wavelength of 382 nm. The equation of linear regression is A = −0.07581-86.79186C (mol l−1), with a linearly correlation coefficient of 0.9979. The detection limit is 0.80 μg ml−1 and R.S.D. is 4.2%. The method is successfully applied to the determination of boron in pharmaceutical and biological samples. The average recoveries are in the range of 98.2-104.1%. Analytical results obtained with this novel method are satisfactory. 相似文献
32.
Monperrus M Tessier E Veschambre S Amouroux D Donard O 《Analytical and bioanalytical chemistry》2005,381(4):854-862
A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography–inductively coupled plasma mass spectrometer (GC–ICP–MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10–60 pg L–1 were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method—the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. 相似文献
33.
C.?Buron C.?Filiatre F.?Membrey A.?FoissyEmail author J.?F.?Argillier 《Colloid and polymer science》2004,282(5):446-453
The interaction between sodium dodecyl sulphate (SDS) and gelatin was studied at pH 4.5 and 6.5 where the gelatin is positively charged (i.e.p. 8). At pH 4.5 a SDS/gelatin concentration range was found where gelatin precipitates. At pH 6.5 the SDS-gelatin complex remains soluble although three SDS concentration domains were distinguished where the SDS-gelatin complex had very different affinities for the solvent. Below C1 the complex was highly surface active but other measurements (viscosity, potentiometry, protons uptake) did not reveal any particular consequence of binding. Between C1 and C2 the molecular size decreased (viscosity lowering) upon charge neutralization and collapse about small SDS aggregates (17 SDS molecules per gelatin molecule). Above C2 a cooperative binding mechanism lead to the formation of SDS aggregates; the complex stretched out and turned strongly hydrophilic (the viscosity increases, low surface activity). At saturation one gelatin molecule bound about 200 SDS molecules. Above the overlap concentration (about 3 wt%) SDS aggregates formed between several gelatin molecules, the viscosity increased continuously with SDS concentration and the binding ratio was lower than in dilute gelatin solutions. A very good correspondence was found between the different analytical data including turbidity, viscosity, surface tension, protons uptake and direct potentiometric SDS binding measurements. 相似文献
34.
重氮树脂与十二烷基硫酸钠相互作用研究罗杨磊曹维孝(北京大学化学与分子工程学院北京100871)关键词重氮树脂,十二烷基硫酸钠,负性PS版随着化学与生命科学领域的发展,大分子与小分子在溶液的相互作用越来越受到关注.表面活性剂因其具有自组装能力,... 相似文献
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36.
离子选择电极—流动注射分析法动力学测定葡萄糖存在下的果糖 总被引:3,自引:0,他引:3
本文将离子电极与流动注射分析相结合,利用30℃下,在强碱性介质中,果糖和葡萄糖与2,4-二硝基酚钠反应速度明显差异,动力学测定了葡萄糖存在下果糖的含量。自制了2,4-二硝基酚电极作为动力学电位测定用的工作电极。本法测定果糖的范围为0.02~1.00mol/L,其RSD为4.0%~4.9%,RE为1.0~5.0%;当C葡/C果≤3倍时,葡萄糖的干扰不超过5%;本法也曾成功地用于果葡萄浆测定,其RSD 相似文献
37.
高效离子排斥色谱法测定饮料中的糖精钠 总被引:3,自引:0,他引:3
提出了一种用高效离子排斥色谱法测定饮料中糖精钠的新方法。以IonPac ICE-AS 6柱为分离柱,0.10 mmol/LH2SO4+甲醇(9+1)为淋洗液,202nm波长下紫外检测。在1-100mg/L范围内,糖精钠的含量与峰面积呈 良好线性关系。检出限为0.60ng,灵敏度优于以往采用离子交换色谱-电导检测法的结果。在实验条件下,饮料 中常见有机酸以及其它人工合成甜味剂等均不产生干扰。方法用于饮料中糖精钠的测定,加标回收率为98%~ 105%。此外还比较了电导检测、紫外检测和经化学抑制系统后紫外检测等三种检测方式对测定灵敏度的影响。 相似文献
38.
Controlled potential coulometric (CPC) studies were carried out for developing a method to determine gallium at milligram levels, in the mixed supporting electrolyte medium (4 M NaClO4 + 0.5 M NaSCN), employing stirring mercury as a working electrode. Investigations for optimization of working electrode potentials, quantity of charge, level of background current and electrolysis time for achieving quantitative reduction of Ga(III) to Ga and its oxidation back to Ga(III), were undertaken. Effect of gallium content and interference of zinc in of gallium determination were also studied. The developed methodology was employed for the determination of gallium in pure Ga as well as in synthetic U + Ga mixture solutions. Accuracy and precision values of better than 0.5% were obtained at 1-2 mg levels. 相似文献
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40.
Behzad Zeynizadeh 《中国化学会会志》2005,52(3):525-530
α,β‐Unsaturated aldehydes and ketones were reduced readily and exclusively to their corresponding allylic alcohols with NaBH4 and catalytic amounts of titanyl acetylacetonate at room temperature. Reduction reactions were carried out in CH3CN or THF. This reducing system was also efficient for the reduction of α‐diketones and acyloins to their corresponding vicinal diols in CH3CN. 相似文献