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Elemental analysis of iron pentacarbonyl by inductively coupled plasma mass spectrometry 电感耦合等离子体质谱法分析五羰基铁元素
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.1.014
M. Steshin, A. M. Potapov, A. D. Bulanov, Yu. S. Belozerov, A. Suchkov
A technique for the quantitative elemental analysis of iron pentacarbonyl by high-resolution mass spectrometry with inductively coupled plasma has been developed. Samples of Fe(CO) 5 were transferred to a nitrate solution for the analysis. To account for the matrix effects analysis of iron pentacarbonyl fractions showed that the impurities of B, Ni and Ti were concentrated in the light fractions, and the impurities of Cr, Co, Cd, Mo and W in the heavy ones. The detection limits of iron in pentacarbonyl for widespread impurities such as Mg, Al, P, Cr, Ni were 10 –6 –10 –5 wt. %, and for less common impurities of Bi, Cd, Co, Pt, Re, Tl, W, U - 10 -8 ÷ 10 -7 wt. % respectively.
建立了电感耦合等离子体高分辨率质谱法定量分析五羰基铁元素的方法。Fe(CO) 5的样品被转移到硝酸盐溶液中进行分析。对五羰基铁馏分的基质效应分析表明,B、Ni和Ti杂质集中在轻馏分中,Cr、Co、Cd、Mo和W杂质集中在重馏分中。五羰基中铁对广泛存在的杂质如Mg、Al、P、Cr、Ni的检出限为10 - 6 ~ 10 - 5 wt. %,对Bi、Cd、Co、Pt、Re、Tl、W、U的检出限分别为10 -8 ~ 10 -7 wt. %。
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引用次数: 0
The application of X-ray fluorescence analysis to research the chemical compositions of tea and coffee samples 应用x射线荧光分析技术研究茶叶和咖啡样品的化学成分
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.1.015
А. Revenko, D. S. Sharykina
The results of food analysis are the main sources of information about their respective quality. X-ray fluorescence analysis (XRF) makes a significant contribution to the study of the problems related to food. Tea is one of the main drinks consumed by the population of the Earth. The complex chemical composition of tea depends on many factors, including soil composition, growing conditions, tea variety
食品分析结果是食品质量信息的主要来源。x射线荧光分析(XRF)对食品相关问题的研究做出了重要贡献。茶是地球上人口消费的主要饮料之一。茶叶复杂的化学成分取决于许多因素,包括土壤成分、生长条件、茶叶品种
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引用次数: 6
Separition of steroid hormones by microemulsion electrokinetic chromatography involving ionic liquids 离子液体微乳电动色谱法分离类固醇激素
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.001
L. Kartsova, E. Bessonova, D. Moskvichev
as an “oil” in the microemulsion for the separation of steroid hormones by MEEKC. The factors such as ILs concentration, nature and pH of the background electrolyte, and the ratio of the components of the microemulsion, that influence the efficiency and separation selectivity of analytes were found. Suitable conditions for the complete separation of a model mixture of steroid hormones: cortisol, cortisone, 11-deoxycortisol, 11-deoxycorticosterone, corticosterone were obtained. The analytical characteristics of methods (optimized conditions) for the determination of steroids by micellar and microemulsion electrokinetic chromatography were compared. It was investigated that the addition of 15 mM 2-hydroxypropyl-β-cyclodextrin increases the separation selectivity and reduces the analysis time. The application of the on-line concentration methods made it possible to reduce the detection limits of analytes to 50 ng / ml. The mode for electrophoretic determination of steroid hormones in biological fluids (urine, blood serum) by MEEKC with the use of ionic liquids has been proposed using the previously obtained results.
作为微乳液中的“油”,用于MEEKC分离类固醇激素。发现了影响分析物分离效率和分离选择性的因素有ILs浓度、背景电解质的性质和pH、微乳液组分的比例等。获得了完全分离类固醇激素模型混合物的合适条件:皮质醇、可的松、11-去氧皮质醇、11-去氧皮质酮、皮质酮。比较了胶束电色谱法和微乳液电色谱法测定类固醇的分析特点(优化条件)。研究了15 mM 2-羟丙基-β-环糊精的加入提高了分离选择性,缩短了分析时间。在线浓度法的应用使分析物的检出限降至50 ng / ml成为可能。利用离子液体的MEEKC电泳测定生物液体(尿、血清)中类固醇激素的模式已被提出。
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引用次数: 2
Control of palm oil content in the mixtures with milk fat by the differential scanning calorimetry (DSC) 差示扫描量热法(DSC)控制乳脂混合物中棕榈油的含量
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.1.010
O. Rudakov, I. Saranov, K. Polansky
1Воронежский государственный технический университет, Российская Федерация, 394006, г. Воронеж, ул. 20-летия Октября, д. 84 2Воронежский государственный университет инженерных технологий, Российская Федерация, 394036, Российская Федерация, г. Воронеж, пр. Революции, д. 19 3Воронежский Филиал Российского экономического университета им. Г.В. Плеханова, Российская Федерация, 394000, Российская Федерация, г. Воронеж, ул. Карла Маркса, д. 67а
1沃罗涅日国立技术大学,俄罗斯联邦,394006沃罗涅日市10月20日,D。84 2沃罗涅日国立工程技术大学,俄罗斯联邦,394036,俄罗斯联邦沃罗涅日海峡革命,D。19俄罗斯经济大学沃罗涅日分校G.V.Plekhanova,俄罗斯联邦,394000,俄罗斯联邦沃罗涅日市卡尔·马克思67a
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引用次数: 5
Modern analyzers for the determination of nitrogen by the Kjeldahl method 凯氏定氮法测定氮的现代分析仪
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.002
E. Zauer, A. B. Ershov
by the Kjeldahl method are systematized: digesters, distillers, and titrators produced by such well-known companies as Buchi (Switzerland), C. Gerhardt, Behr Labor-Technik GmbH and FoodALYT GmbH (Germany), Foss Tecator (Denmark, Sweden), VELP Scientifica (Italy), J.P.Selecta (Spain), Hanon Instruments (China), OOO VPK Sibagropribor and OOO Vilitek (Russia). The data on the characteristics of the analyzers is also provided and includes the number and volume of test tubes (flasks), the time of mineralization, distillation and analysis, mass (volume) of the sample, and the lower limit of nitrogen detection.
由Buchi(瑞士)、C. Gerhardt、Behr l- technik GmbH和FoodALYT GmbH(德国)、Foss Tecator(丹麦、瑞典)、VELP scientific(意大利)、J.P.Selecta(西班牙)、Hanon Instruments(中国)、OOO VPK Sibagropribor和OOO Vilitek(俄罗斯)等知名公司生产的消解器、蒸馏器和滴定器。还提供了有关分析仪特性的数据,包括试管(烧瓶)的数量和体积,矿化时间,蒸馏和分析,样品的质量(体积)以及氮检测的下限。
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引用次数: 1
Comparative characterization of quantitative gas chromatographic analysis capabilities using basic and modified external standard methods 使用基本和改进的外部标准方法的定量气相色谱分析能力的比较特性
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.007
I. Zenkevich, Natalia A. Devleshova, Yulia V. Krivolapova, D. Moskvichev, Lyubov G. Rubicheva, Nikolai Yu. Tyuftyakov
The known mode of chromatographic quantification by the method of external standard is based on the comparison of average absolute peak areas of analyte(s) for target samp les ( S x ) and additionally prepared external standards ( S stand ). This method is characteri zed by the valuable “sensitivity” of the results in relation to the repeatability of the measured peak areas. In the modified method of external standard, the equal amounts of additional standard are added to the equal amounts of samples; the peak ratios ( S x / S add.stand ) and ( S stand / S add.stand ) are used in the subsequent data processing. This modified external standard method is not described in the contemporary scien tific and teaching literature on gas chromatography. Thus, for the illustration of its advan tages, the results of target analyte quantification in different solvents using basic and modified methods are compa red in the cur rent study. All measurements were carried out by the senior students of the Institute for Chemistry of St. Petersburg State University (Russia) during their practical exercises in gas chromatography. It was shown that the modified external standard method compared with its basic ver sion provided better repeatability of determinations, better precision (lesser systema tic errors) and reduced the overall time expenses due to the lesser quantity of serial ana lyses and the absence of the necessity to reveal and exclude the outliers.
已知的外标法色谱定量方法是将目标样品(sx)的分析物(s)的平均绝对峰面积与另外制备的外标(s stand)进行比较。该方法的特点是与测量峰面积的可重复性有关的结果的有价值的“灵敏度”。外标法是在等量的样品中加入等量的附加标准品;在随后的数据处理中使用峰值比(S x / S add.stand)和(S stand / S add.stand)。这种改进的外标法在当代气相色谱的科学和教学文献中没有描述。因此,为了说明其优势,本研究比较了基本方法和改进方法在不同溶剂中对目标分析物的定量结果。所有的测量都是由俄罗斯圣彼得堡国立大学化学研究所的高年级学生在气相色谱的实践练习中进行的。结果表明,改进后的外标法与基本法相比,具有更好的重复性和精密度(更小的系统误差),由于序列分析的数量较少,不需要发现和排除异常值,从而减少了总体时间花费。
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引用次数: 1
Essential oils: the review of the methods for determining the authenticity and detecting adulteration 精油:鉴别和掺假检测方法综述
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/analitika.2019.23.4.010
I. V. Lapko, Yu. B. Aksenova, O. Kuznecova, S. V. Vasilevskij, A. Aksenov, V. F. Taranchenko, A. M. Antohin, A. A. Ihalajnen
Эфирные масла являются продуктами природного происхождения, которые находят самое разнообразное применение в различных областях промышленности. Высокая стоимость, трудоемкость производства и широкое использование приводят к тому, что в продаже наряду с качественными эфирными маслами часто встречают фальсифицированные. Применение поддельных масел повышает их опасность для человека, в связи с чем установление подлинности эфирных масел имеет большое значение. В обзоре проведен анализ опубликованных работ и нормативных документов, посвященных вопросам определения подлинности и выявления фальсификации эфирных масел. Рассмотрен компонентный состав эфирных масел, его вариабельность в зависимости от места произрастания эфиромасличного растения и технологии выделения масла. Обсуждены основные способы фальсификации эфирных масел и спектр используемых для этого приемов, необходимость применения соответствующих методов исследования, позволяющих контролировать подлинность продукции. Проведен анализ литературы и нормативной базы, регламентирующей качество эфирных масел, существующих методов определения их подлинности, указывают достоинства и недостатки. Особое внимание уделено методу масс-спектрометрии изотопных отношений, как наиболее перспективному, вследствие высокой точности и возможности применения для исследования практически любого типа масла. Приведены основные теоретические положения исследования стабильных изотопов и их фракционирования, принципиальные особенности методов измерения. Подтверждено широкое использование метода масс-спектрометрии изотопных отношений на практике конкретными примерами с демонстрацией новых возможностей данного метода, связанных с использованием изотопного профилирования и комбинированных методов изотопного анализа. Отмечена важность для определения подлинности масел информации об изотопном составе их компонентов, который является индикатором любых искусственных процессов, происходящих с эфирным маслом в результате фальсификации. Ключевые слова: эфирные масла, компонентный состав, фальсификация, подлинность, методы, хроматография, спектроскопия, изотопная масс-спектрометрия
精油是自然产生的,在不同的工业领域可以找到最多样化的应用。高成本、劳动密集度和广泛使用意味着,在销售中,除了高质量的乙醚油,人们经常看到伪造的。使用假润滑油增加了人类的危险,因此确定乙醚油的真实性至关重要。审查分析了发表的论文和有关鉴定和鉴定精油伪造问题的监管文件。乙醚油的成分,其多样性取决于乙醚植物的生长地点和油的分泌技术。讨论了伪造乙醚油的主要方法和使用的光谱,需要使用适当的研究方法来控制产品的真实性。对控制乙油质量的文学和监管框架进行了分析,现有的鉴定方法显示了优点和缺点。由于高精准性和研究几乎任何类型的油的可行性,质谱测定同位素的方法是最有前途的。以下是稳定同位素研究及其分馏的基本理论条款,测量方法的基本特征。在实践中广泛使用了同位素关系质谱仪的例子,说明了与同位素剖析和综合同位素分析方法有关的新可能性。重要的是要确定其成分的同位素成分的真实性,这是任何人造黄油因伪造而发生的任何人工过程的指标。关键词:精油、成分、伪造、鉴定、方法、色谱、光谱学、同位素质谱学
{"title":"Essential oils: the review of the methods for determining the authenticity and detecting adulteration","authors":"I. V. Lapko, Yu. B. Aksenova, O. Kuznecova, S. V. Vasilevskij, A. Aksenov, V. F. Taranchenko, A. M. Antohin, A. A. Ihalajnen","doi":"10.15826/analitika.2019.23.4.010","DOIUrl":"https://doi.org/10.15826/analitika.2019.23.4.010","url":null,"abstract":"Эфирные масла являются продуктами природного происхождения, которые находят самое разнообразное применение в различных областях промышленности. Высокая стоимость, трудоемкость производства и широкое использование приводят к тому, что в продаже наряду с качественными эфирными маслами часто встречают фальсифицированные. Применение поддельных масел повышает их опасность для человека, в связи с чем установление подлинности эфирных масел имеет большое значение. В обзоре проведен анализ опубликованных работ и нормативных документов, посвященных вопросам определения подлинности и выявления фальсификации эфирных масел. Рассмотрен компонентный состав эфирных масел, его вариабельность в зависимости от места произрастания эфиромасличного растения и технологии выделения масла. Обсуждены основные способы фальсификации эфирных масел и спектр используемых для этого приемов, необходимость применения соответствующих методов исследования, позволяющих контролировать подлинность продукции. Проведен анализ литературы и нормативной базы, регламентирующей качество эфирных масел, существующих методов определения их подлинности, указывают достоинства и недостатки. Особое внимание уделено методу масс-спектрометрии изотопных отношений, как наиболее перспективному, вследствие высокой точности и возможности применения для исследования практически любого типа масла. Приведены основные теоретические положения исследования стабильных изотопов и их фракционирования, принципиальные особенности методов измерения. Подтверждено широкое использование метода масс-спектрометрии изотопных отношений на практике конкретными примерами с демонстрацией новых возможностей данного метода, связанных с использованием изотопного профилирования и комбинированных методов изотопного анализа. Отмечена важность для определения подлинности масел информации об изотопном составе их компонентов, который является индикатором любых искусственных процессов, происходящих с эфирным маслом в результате фальсификации. Ключевые слова: эфирные масла, компонентный состав, фальсификация, подлинность, методы, хроматография, спектроскопия, изотопная масс-спектрометрия","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"19 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2019-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67251990","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
The method of screening samples for diamonds 筛选钻石样品的方法
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.1.013
B. I. Kitov
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引用次数: 1
Solid-phase spectrophotometric determination of hydrogen peroxide 固相分光光度法测定过氧化氢
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.010
N. Gavrilenko, N. V. Saranchina, D. A. Fedan, M. Gavrilenko
A combined solid-phase spectrophotometric iodometric method for the determination of hydrogen peroxide using a methacrylate polymer was proposed. The method was based on the oxidation reaction of iodide ion with hydrogen peroxide in the hydrochloric acid with the release of free iodine. The iodine was extracted from the solution by a polymethacrylate matrix, and its concentration was measured at the absorbance of 365 nm. The amount of iodine extracted by the polymethacrylate matrix was proportional to the concentration of hydrogen peroxide in the solution. The effect of interfering ions was also investigated. The optimal phase contact time was 5 minutes. The effect of adding the hydrochloric acid to the analyzed solution on the analytical signal of the polymethacrylate matrix after its contact with hydrogen peroxide solution was studied. It was shown that the maximum signal was obtained in the range of acid concentrations in the solution of (3–5)∙10 –3 M. The optimal concentration of potassium iodide in the analyzed solution for the redox reaction was 0.06%. At this concentration, the widest range of detectable concentrations was achieved with the smallest limit of detection for hydrogen peroxide. The developed procedure ensured the determination in the range of (15–130)∙10 -5 % of hydrogen peroxide with the detection limit of 5 × 10 -5 %. The results of the determination of hydrogen peroxide were given for the proposed method in samples of disinfectants and bleaching agents. The proposed method for hydrogen peroxide determination is more preferable in comparison to the iodometric method [1] as it provides the increased sensitivity, simplicity and rapid analysis, the absence of losses of released iodine due to its solid-phase extraction into the methacrylate polymer and can be conducted using the standard spectrophotometric equipment.
提出了用甲基丙烯酸酯聚合物联合固相分光光度碘量测定过氧化氢的方法。该方法是基于碘离子与过氧化氢在盐酸中氧化反应,释放游离碘。用聚甲基丙烯酸酯基质提取碘,在365 nm吸光度下测定碘的浓度。聚甲基丙烯酸酯基质提取碘的量与溶液中过氧化氢的浓度成正比。研究了干扰离子的影响。最佳相接触时间为5分钟。研究了在分析溶液中加入盐酸对聚甲基丙烯酸酯基质与过氧化氢溶液接触后分析信号的影响。结果表明,在(3-5)∙10 -3 m的酸浓度范围内获得最大信号,分析溶液中碘化钾的最佳浓度为0.06%。在此浓度下,可检测浓度的范围最广,过氧化氢的检测限最小。所建立的方法保证了过氧化氢在(15-130)∙10 - 5%范围内的检测,检出限为5 × 10 - 5%。给出了该方法在消毒剂和漂白剂样品中过氧化氢含量的测定结果。与碘量法[1]相比,本文提出的过氧化氢测定方法更可取,因为它提供了更高的灵敏度,简单和快速的分析,并且由于其固相萃取到甲基丙烯酸酯聚合物中而没有释放碘的损失,并且可以使用标准分光光度法设备进行测定。
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引用次数: 0
Multielement analysis of tea by X-ray fluorescence spectrometry with full external reflection 全外反射x射线荧光光谱法分析茶叶中的多元素
Q4 Chemistry Pub Date : 2019-01-01 DOI: 10.15826/ANALITIKA.2019.23.2.009
A. Maltsev, D. S. Sharykina, E. Chuparina, G. Pashkova, A. Revenko
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引用次数: 1
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Analitika i Kontrol
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