Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.3.005
M. Chervyakovskaya, S. Votyakov, V. Chervyakovskiy
A technique of analyzing the isotopic composition of Lu and Hf and for determining the Lu/Hf and Hf/Hf isotopic ratios in zircons is presented using a Neptune Plus (Thermo Scientific) mass spectrometer with inductively coupled plasma with an NWR 213 (ESI) laser ablation attachment. On the example of Mud Tank, GJ-1, 91500, Plesovice and Temora-2 standard zircon samples, the uncertainty of a single measurement of the 176Hf/177Hf ratio has been obtained in the range of 0.002-0.008% in the form of 2σ (with a crater diameter of 50 μm; when it decreased to 25 μm the measurement uncertainty of the 176Hf/177Hf ratio increased by 1.5-2 times). Under the optimum parameters of the NexION 300S with NWR213 with the aim of increasing the locality of the sequential study of U/Pb and Lu/Hf isotope systems, a comparative characteristic of the application of two approaches has been obtained: in adjacent grain areas (approach 1) and in one crater (approach 2). The metrological characteristics of analyzing the isotopic composition of Lu and Hf and for determining the Lu/Hf and Hf/Hf isotopic ratios in zircons have been determined. To establish the application limits of the developed technique, the factor planning of the experiment has been developed. It was established that with a Lu/Hf ratio of 1/50 or more, the technique is not recommended to be applied due to the incorrect allowance of the isobaric effect. The procedures for measuring and calculating the Lu/Hf isotopic ratios of the isotope system in zircon have been tested on zircon grains (samples NP-46 and NP-47) of the Neplyuevsky pluton (South Urals). The data obtained was in satisfactory agreement with the data of the A. P. Karpinsky Russian Geological Research Institute (VSEGEI).
{"title":"Study of Lu/Hf isotopic composition of zircons using a Neptune Plus multicollector inductively coupled plasma mass spectrometer with an NWR 213 laser ablation attachment","authors":"M. Chervyakovskaya, S. Votyakov, V. Chervyakovskiy","doi":"10.15826/analitika.2021.25.3.005","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.3.005","url":null,"abstract":"A technique of analyzing the isotopic composition of Lu and Hf and for determining the Lu/Hf and Hf/Hf isotopic ratios in zircons is presented using a Neptune Plus (Thermo Scientific) mass spectrometer with inductively coupled plasma with an NWR 213 (ESI) laser ablation attachment. On the example of Mud Tank, GJ-1, 91500, Plesovice and Temora-2 standard zircon samples, the uncertainty of a single measurement of the 176Hf/177Hf ratio has been obtained in the range of 0.002-0.008% in the form of 2σ (with a crater diameter of 50 μm; when it decreased to 25 μm the measurement uncertainty of the 176Hf/177Hf ratio increased by 1.5-2 times). Under the optimum parameters of the NexION 300S with NWR213 with the aim of increasing the locality of the sequential study of U/Pb and Lu/Hf isotope systems, a comparative characteristic of the application of two approaches has been obtained: in adjacent grain areas (approach 1) and in one crater (approach 2). The metrological characteristics of analyzing the isotopic composition of Lu and Hf and for determining the Lu/Hf and Hf/Hf isotopic ratios in zircons have been determined. To establish the application limits of the developed technique, the factor planning of the experiment has been developed. It was established that with a Lu/Hf ratio of 1/50 or more, the technique is not recommended to be applied due to the incorrect allowance of the isobaric effect. The procedures for measuring and calculating the Lu/Hf isotopic ratios of the isotope system in zircon have been tested on zircon grains (samples NP-46 and NP-47) of the Neplyuevsky pluton (South Urals). The data obtained was in satisfactory agreement with the data of the A. P. Karpinsky Russian Geological Research Institute (VSEGEI).","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253221","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.4.002
V. А. Labusov, A.V. Behterev, V. G. Garanin
Multichannel analyzers of emission spectra (MAES) are operated as part of more than six hundred systems for atomic emission spectral analysis at enterprises in Russia, the CIS countries, and others. Until recently, MAES analyzers used only BLPP-369M1 photodetector arrays, whose performance is sufficient for integral atomic emission spectrometry applications using bright sources of spectral excitation based, for example, on an arc or spark electric discharge. To solve problems where high temporal spatial resolution and high sensitivity are required, high-speed MAES analyzers have been developed based on two new photodetector arrays—BLPP-2000 and BLPP-4000. A number of optical spectrometers based on these arrays have been developed and put into production by the VMK-Optoelektronika company: Atomic emission spectrometers: Grand Globula and Ekspress arc and spark spectrometers for the direct analysis of powders by evaporation from the channel of a graphite electrode and for the analysis of metals; Grand-Potok arc spectrometers for the rapid analysis of powders by the spill-injection method; Grand-Ekspert and Favorit argon-spark vacuum spectrometers for the rapid analysis of metals and alloys; Grand-SVCh microwave-induced nitrogen plasma spectrometers and Grand-ISP inductively-coupled argon plasma spectrometers for the analysis of liquids; Kolibri-SVCh microwave-induced air plasma spectrometers and Pavlin flame atomic emission spectrometers for the determination of alkaline and alkaline earth elements in solutions. Grand-AAS high-resolution continuous-source electrothermal atomic absorption spectrometers for the simultaneous determination of elements in liquids.
{"title":"Spectrometers with MAES analyzers based on new photodetector arrays","authors":"V. А. Labusov, A.V. Behterev, V. G. Garanin","doi":"10.15826/analitika.2021.25.4.002","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.4.002","url":null,"abstract":"Multichannel analyzers of emission spectra (MAES) are operated as part of more than six hundred systems for atomic emission spectral analysis at enterprises in Russia, the CIS countries, and others. Until recently, MAES analyzers used only BLPP-369M1 photodetector arrays, whose performance is sufficient for integral atomic emission spectrometry applications using bright sources of spectral excitation based, for example, on an arc or spark electric discharge. To solve problems where high temporal spatial resolution and high sensitivity are required, high-speed MAES analyzers have been developed based on two new photodetector arrays—BLPP-2000 and BLPP-4000. A number of optical spectrometers based on these arrays have been developed and put into production by the VMK-Optoelektronika company: Atomic emission spectrometers: Grand Globula and Ekspress arc and spark spectrometers for the direct analysis of powders by evaporation from the channel of a graphite electrode and for the analysis of metals; Grand-Potok arc spectrometers for the rapid analysis of powders by the spill-injection method; Grand-Ekspert and Favorit argon-spark vacuum spectrometers for the rapid analysis of metals and alloys; Grand-SVCh microwave-induced nitrogen plasma spectrometers and Grand-ISP inductively-coupled argon plasma spectrometers for the analysis of liquids; Kolibri-SVCh microwave-induced air plasma spectrometers and Pavlin flame atomic emission spectrometers for the determination of alkaline and alkaline earth elements in solutions. Grand-AAS high-resolution continuous-source electrothermal atomic absorption spectrometers for the simultaneous determination of elements in liquids.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253548","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.4.009
A. A. Dzyuba, S. Dodonov, V. А. Labusov
The analytical characteristics of the new Grand-2000 high-resolution spectrometer with BLPP-4000 photodetectors were evaluated. The device was tested as part of the Grand-Potok complex, which consists of a spectrometer and an electric arc facility and is designed to analyze powder samples continuously brought into the plasma atomizer (free-burning arc in air). The characteristics of the new spectrometer were compared with those of the Grand spectrometer, which is widely employed in analytical laboratories. It is shown that the use of the Grand-2000 spectrometer to determine the concentration of elements in geological and industrial powder samples does not lead to an obvious improvement in the results. The threefold increase in the spectral resolution of the new spectrometer reduces spectral influences from interfering elements, but the relative systematic error both decreases and increases for different samples. This may indicate the influence of unaccounted-for factors, for example, non-optimal spectra processing algorithms for this device. The results obtained suggest good prospects for the use of the Grand-2000 spectrometer to determine the concentration of elements in samples with a complex spectrum, but they also indicate the need for further studies to determine the optimal parameters for processing spectra. In addition, the Grand-2000 spectrometer can be used to supplement and refine the existing database of the wavelengths of spectral lines.
{"title":"Analytical capabilities of the Grand-2000 high-resolution spectrometer","authors":"A. A. Dzyuba, S. Dodonov, V. А. Labusov","doi":"10.15826/analitika.2021.25.4.009","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.4.009","url":null,"abstract":"The analytical characteristics of the new Grand-2000 high-resolution spectrometer with BLPP-4000 photodetectors were evaluated. The device was tested as part of the Grand-Potok complex, which consists of a spectrometer and an electric arc facility and is designed to analyze powder samples continuously brought into the plasma atomizer (free-burning arc in air). The characteristics of the new spectrometer were compared with those of the Grand spectrometer, which is widely employed in analytical laboratories. It is shown that the use of the Grand-2000 spectrometer to determine the concentration of elements in geological and industrial powder samples does not lead to an obvious improvement in the results. The threefold increase in the spectral resolution of the new spectrometer reduces spectral influences from interfering elements, but the relative systematic error both decreases and increases for different samples. This may indicate the influence of unaccounted-for factors, for example, non-optimal spectra processing algorithms for this device. The results obtained suggest good prospects for the use of the Grand-2000 spectrometer to determine the concentration of elements in samples with a complex spectrum, but they also indicate the need for further studies to determine the optimal parameters for processing spectra. In addition, the Grand-2000 spectrometer can be used to supplement and refine the existing database of the wavelengths of spectral lines.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67254071","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.2.002
V. Krylov, R. Mosyagin
The flotation-assisted liquid-liquid microextraction method of mono-, di -, and trichloroacetic acids (CAAs) has been developed. Methyl tert-butyl ether (MTBE) was used as an extractant. The emulsification was performed by the ultrasonic irradiation. The microextraction procedure was carried out in a 27 ml special tube. It was equipped with the capillaries for sampling the extract and an air outlet. A salting-out additive (Na2SO4) was used to reduce the solubility of MTBE in water and to increase the extraction efficiency of CAAs. The air passage through the emulsion of the extractant was carried out using the eight-channel capillary bubbler. The organic matrix replacement was applied for ion chromatographic determination of CAAs with the conductivity detection. Current study showed the advantages of the flotation-assisted demulsification over the centrifugal one. The concentration factors of chlorinated acetic acids were 2-3 times higher. The detection limits of CAAs in water were reduced to (5·10-4 - 4·10-3 mg/l). The extraction time was reduced by more than three times. The trueness of the determination of HUC impurities was confirmed by the addition method. The statistical insignificance of the systematic error in comparison with the random error was shown. The developed method of preconcentration in combination with ion chromatography made it possible to determine the concentrations of CAAs 40-1250 times lower than the normalized SanPiN and WHO. This allowed conducting a highly sensitive determination of CAAs in water long before the onset of the critical ecological state.
{"title":"Microextraction flotamicroextraction flotation concentration and determination of chloroacetic acids in watertion concentration and determination of chloroacetic acids in water","authors":"V. Krylov, R. Mosyagin","doi":"10.15826/analitika.2021.25.2.002","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.2.002","url":null,"abstract":"The flotation-assisted liquid-liquid microextraction method of mono-, di -, and trichloroacetic acids (CAAs) has been developed. Methyl tert-butyl ether (MTBE) was used as an extractant. The emulsification was performed by the ultrasonic irradiation. The microextraction procedure was carried out in a 27 ml special tube. It was equipped with the capillaries for sampling the extract and an air outlet. A salting-out additive (Na2SO4) was used to reduce the solubility of MTBE in water and to increase the extraction efficiency of CAAs. The air passage through the emulsion of the extractant was carried out using the eight-channel capillary bubbler. The organic matrix replacement was applied for ion chromatographic determination of CAAs with the conductivity detection. Current study showed the advantages of the flotation-assisted demulsification over the centrifugal one. The concentration factors of chlorinated acetic acids were 2-3 times higher. The detection limits of CAAs in water were reduced to (5·10-4 - 4·10-3 mg/l). The extraction time was reduced by more than three times. The trueness of the determination of HUC impurities was confirmed by the addition method. The statistical insignificance of the systematic error in comparison with the random error was shown. The developed method of preconcentration in combination with ion chromatography made it possible to determine the concentrations of CAAs 40-1250 times lower than the normalized SanPiN and WHO. This allowed conducting a highly sensitive determination of CAAs in water long before the onset of the critical ecological state.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67252998","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.2.001
N. Anikina, N. Gnilomedova, S. Cherviak, A. V. Vesiutova, M. V. Ermihina
The problem of wine color adulteration is relevant all over the world, and, therefore, establishing or refuting the fact of the colorant presence is an integral part of the techno-chemical control. There are many methods for determining artificial colorants (AC) in the alcoholic beverages with various levels of sensitivity and selectivity of detection as well as the promptness in generating the results and the cost of studying one sample. Current work is devoted to the development of a rapid test for detecting the artificial colorants in wines. It is based on the method of the International Organization of Vine and Wine, the principle of which is to fixate the acidic artificial colorants on a specially prepared woolen thread when boiling the sample of wine. The modification of analytical procedure included the reduction of the test sample aliquot, the number of operations and the examination time without compromising the reliability of the conclusion. In order to imitate the color of red wines, Azorubine (E122), Allura Red AC (E129) and Indigo Carmine (E132) food colorants were used. The objects of the research were: model systems based on wine, white and red wines, counterfeit wines provided by the controlling authorities, and concentrated grape must. It was shown that in the genuine wines, depending on the color saturation of the test sample caused by natural anthocyanins, the woolen thread was discoloring from light to dark beige; its color was enhancing from pale pink to deep ruby with the increase in the content of AC in wine. The sensitivity of the proposed method made it possible to determine the presence of AC at the rate of 0.1-0.2 mg/dm3 in wines. The method did not require expensive equipment and could be used in the laboratories of winemaking industry or by the controlling authorities for establishing the fact of adulteration of alcoholic and juice products.
葡萄酒颜色掺假问题在世界范围内都是相关的，因此，确定或驳斥着色剂存在的事实是技术化学控制的一个组成部分。酒精饮料中人工着色剂的检测方法有很多，它们的检测灵敏度和选择性各不相同，而且产生结果的快速性和一个样品的研究成本也各不相同。目前的工作是致力于开发一种快速检测葡萄酒中人工色素的方法。它是根据国际葡萄和葡萄酒组织的方法，其原理是在煮沸葡萄酒样品时，将酸性人工着色剂固定在特制的毛线上。分析程序的修改包括在不影响结论可靠性的前提下减少测试样品的等分、操作次数和检查时间。为了模拟红酒的颜色，采用了偶氮rubine (E122)， Allura red AC (E129)和Indigo Carmine (E132)食用色素。研究的对象是:基于葡萄酒，白葡萄酒和红葡萄酒的模型系统，由控制当局提供的假冒葡萄酒和浓缩葡萄必须。结果表明，在正品葡萄酒中，根据天然花青素引起的样品颜色饱和度的不同，毛线会从浅米色变色到深米色;随着葡萄酒中AC含量的增加，其颜色由浅粉红色增强为深红宝石色。该方法的灵敏度使测定葡萄酒中AC的存在以0.1-0.2 mg/dm3的速率成为可能。该方法不需要昂贵的设备，可用于酿酒工业实验室或由管制当局确定酒精和果汁产品掺假的事实。
{"title":"Rapid test for detecting artificial colorants in wine products","authors":"N. Anikina, N. Gnilomedova, S. Cherviak, A. V. Vesiutova, M. V. Ermihina","doi":"10.15826/analitika.2021.25.2.001","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.2.001","url":null,"abstract":"The problem of wine color adulteration is relevant all over the world, and, therefore, establishing or refuting the fact of the colorant presence is an integral part of the techno-chemical control. There are many methods for determining artificial colorants (AC) in the alcoholic beverages with various levels of sensitivity and selectivity of detection as well as the promptness in generating the results and the cost of studying one sample. Current work is devoted to the development of a rapid test for detecting the artificial colorants in wines. It is based on the method of the International Organization of Vine and Wine, the principle of which is to fixate the acidic artificial colorants on a specially prepared woolen thread when boiling the sample of wine. The modification of analytical procedure included the reduction of the test sample aliquot, the number of operations and the examination time without compromising the reliability of the conclusion. In order to imitate the color of red wines, Azorubine (E122), Allura Red AC (E129) and Indigo Carmine (E132) food colorants were used. The objects of the research were: model systems based on wine, white and red wines, counterfeit wines provided by the controlling authorities, and concentrated grape must. It was shown that in the genuine wines, depending on the color saturation of the test sample caused by natural anthocyanins, the woolen thread was discoloring from light to dark beige; its color was enhancing from pale pink to deep ruby with the increase in the content of AC in wine. The sensitivity of the proposed method made it possible to determine the presence of AC at the rate of 0.1-0.2 mg/dm3 in wines. The method did not require expensive equipment and could be used in the laboratories of winemaking industry or by the controlling authorities for establishing the fact of adulteration of alcoholic and juice products.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253326","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.2.008
E. Koshel, A. Arkhipenko, V. B. Baranovskaya
The requirements for the composition of initial oxides for the lutetium orthosilicate crystals are quite stringent: the content of the basic substance Lu2O3 is 99.999 wt%. Critical are coloring impurities: Fe, Ni, Cr, Co, Cu, V, Mn, the content of each should be no more than 0.0005 - 0.0010 wt%, Pr, Nd, Sm, Er, Tb, Yb no more than 0.0005 wt% for each one. It is also necessary to control the content of Al, As, Bi, Cd, Mg, Mo, Pb, Sb, Si, Sn, Ti, Zn, Y, La, Ce, Sc, Eu, Gd, Dy, Ho, Tm. To determine the impurity composition of lutetium oxide, one of the promising methods of analysis is direct arc atomic emission spectroscopy (DC Arc). The advantages of this method are the determination of the chemical composition without sample dissolution, a wide range of concentrations (10-6 - 10-1% wt%), a large number of determined elements. To realize the potential analytical capabilities of the method, the experimental conditions were studied: the interelectrode distance, the shape and size of graphite electrodes, the ratio of Lu2O3 to the spectral buffer, the type of carriers and operating modes of the generator. For most elements, the limits of determination are n ∙ 10-6 - n ∙ 10-4 wt%, that is significantly lower than in the current methods of DC Arc. The trueness of results is controlled by ICP-MS. The complex application of new approaches and modern capabilities of spectral equipment made it possible to develop a method with improved metrological characteristics.
{"title":"Lutetium oxide analysis by direct arc atomic emission spectrometry","authors":"E. Koshel, A. Arkhipenko, V. B. Baranovskaya","doi":"10.15826/analitika.2021.25.2.008","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.2.008","url":null,"abstract":"The requirements for the composition of initial oxides for the lutetium orthosilicate crystals are quite stringent: the content of the basic substance Lu2O3 is 99.999 wt%. Critical are coloring impurities: Fe, Ni, Cr, Co, Cu, V, Mn, the content of each should be no more than 0.0005 - 0.0010 wt%, Pr, Nd, Sm, Er, Tb, Yb no more than 0.0005 wt% for each one. It is also necessary to control the content of Al, As, Bi, Cd, Mg, Mo, Pb, Sb, Si, Sn, Ti, Zn, Y, La, Ce, Sc, Eu, Gd, Dy, Ho, Tm. To determine the impurity composition of lutetium oxide, one of the promising methods of analysis is direct arc atomic emission spectroscopy (DC Arc). The advantages of this method are the determination of the chemical composition without sample dissolution, a wide range of concentrations (10-6 - 10-1% wt%), a large number of determined elements. To realize the potential analytical capabilities of the method, the experimental conditions were studied: the interelectrode distance, the shape and size of graphite electrodes, the ratio of Lu2O3 to the spectral buffer, the type of carriers and operating modes of the generator. For most elements, the limits of determination are n ∙ 10-6 - n ∙ 10-4 wt%, that is significantly lower than in the current methods of DC Arc. The trueness of results is controlled by ICP-MS. The complex application of new approaches and modern capabilities of spectral equipment made it possible to develop a method with improved metrological characteristics.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253394","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.3.001
L. Angelova, N. Genova, S. Stoyanova, O. Surleva, I.-H. Nekov, D. Ilieva, A. Surleva
This comparative study was aimed at estimating analytical behavior of methods for determination of plant available potassium applied to Bulgarian arable soils and to reveal the relationship between the amount of extractable K. Twenty-four samples from two traditional agricultural regions in Bulgaria were studied. Soil potassium was extracted by NH4OAc/HOAc pH 4.5 (AA), diluted double acid (Mehlich 1), CaCl2, BaCl2 and a modified acetate/lactate method (ALM) and determined by Flame AES. The factors influencing the methods accuracy were identified and uncertainty was estimated. The expanded uncertainty was (in mg K2O (100 g dry soil)-1): 0.10 (ALM), 0.64 (Mehlich 1), 0.17 (CaCl2) and 1.1 (AA). The study revealed that the factor which mainly influence the uncertainty of the applied analytical methods for plant available potassium in soil was the calibration of Flame AES determination. The obtained results showed that extractable potassium lowered in the following order . Soil potassium extracted by ALM procedure correlated with AA, BaCl2-K, CaCl2 –K and Mehlich 1 - K at 0.05 level of significance. ALM extracted between 1.2 to 5.8 times more soil K than other methods did. The obtained results provided a base for further study on correlation between extractable K and soil fertility indices for particular soil types and climatic regions in Bulgaria.
{"title":"Comparative study of soil test methods for determination of plant available potassium in Bulgarian arable soils","authors":"L. Angelova, N. Genova, S. Stoyanova, O. Surleva, I.-H. Nekov, D. Ilieva, A. Surleva","doi":"10.15826/analitika.2021.25.3.001","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.3.001","url":null,"abstract":"This comparative study was aimed at estimating analytical behavior of methods for determination of plant available potassium applied to Bulgarian arable soils and to reveal the relationship between the amount of extractable K. Twenty-four samples from two traditional agricultural regions in Bulgaria were studied. Soil potassium was extracted by NH4OAc/HOAc pH 4.5 (AA), diluted double acid (Mehlich 1), CaCl2, BaCl2 and a modified acetate/lactate method (ALM) and determined by Flame AES. The factors influencing the methods accuracy were identified and uncertainty was estimated. The expanded uncertainty was (in mg K2O (100 g dry soil)-1): 0.10 (ALM), 0.64 (Mehlich 1), 0.17 (CaCl2) and 1.1 (AA). The study revealed that the factor which mainly influence the uncertainty of the applied analytical methods for plant available potassium in soil was the calibration of Flame AES determination. The obtained results showed that extractable potassium lowered in the following order . Soil potassium extracted by ALM procedure correlated with AA, BaCl2-K, CaCl2 –K and Mehlich 1 - K at 0.05 level of significance. ALM extracted between 1.2 to 5.8 times more soil K than other methods did. The obtained results provided a base for further study on correlation between extractable K and soil fertility indices for particular soil types and climatic regions in Bulgaria.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253437","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.4.003
I. Zarubin, A. Putmakov, E. Lukina, D. O. Selunin, I. D. Burumov
At the Novosibirsk Chemical Concentrates Plant, the determination of alkali metals and calcium in the range of 0.1–100 mg/l is carried out using atomic emission spectra excited in an air-acetylene flame and recorded in the range of 390–860 nm. When these elements are analyzed simultaneously in a wide range of concentrations, the accumulation time of the analytical signal (exposure) is determined by the minimum concentration of calcium. However, at this exposure, the highly sensitive lines of sodium and potassium do not provide the analysis in the entire concentration range, since at large values, the analytical signal goes into saturation. Other analytical lines of potassium and sodium in the above-mentioned operating spectral range have three to four orders of magnitude lower sensitivity. As a result, there may be a gap in the range of detectable concentrations. This paper provides a way to eliminate this gap. To evaluate the degree of correction of the recorded signal, the relative intensities of the spectral lines of potassium and sodium excited in an air-acetylene flame are calculated. Then, based on the calculation results, an optimal echelette diffraction grating with a blaze angle of 300 nm is selected, and a combination of filters is installed to equalize the recorded radiation. As a result, for sodium and potassium, for which the determination is carried out along two analytical lines, the calibration dependences have an overlap that includes at least two concentration values.
{"title":"Extending the working range for the flame photometric determination of alkali metals and calcium using the PAVLIN spectrometer","authors":"I. Zarubin, A. Putmakov, E. Lukina, D. O. Selunin, I. D. Burumov","doi":"10.15826/analitika.2021.25.4.003","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.4.003","url":null,"abstract":"At the Novosibirsk Chemical Concentrates Plant, the determination of alkali metals and calcium in the range of 0.1–100 mg/l is carried out using atomic emission spectra excited in an air-acetylene flame and recorded in the range of 390–860 nm. When these elements are analyzed simultaneously in a wide range of concentrations, the accumulation time of the analytical signal (exposure) is determined by the minimum concentration of calcium. However, at this exposure, the highly sensitive lines of sodium and potassium do not provide the analysis in the entire concentration range, since at large values, the analytical signal goes into saturation. Other analytical lines of potassium and sodium in the above-mentioned operating spectral range have three to four orders of magnitude lower sensitivity. As a result, there may be a gap in the range of detectable concentrations. This paper provides a way to eliminate this gap. To evaluate the degree of correction of the recorded signal, the relative intensities of the spectral lines of potassium and sodium excited in an air-acetylene flame are calculated. Then, based on the calculation results, an optimal echelette diffraction grating with a blaze angle of 300 nm is selected, and a combination of filters is installed to equalize the recorded radiation. As a result, for sodium and potassium, for which the determination is carried out along two analytical lines, the calibration dependences have an overlap that includes at least two concentration values.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253753","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.4.005
V. B. Baranovskaya, M. Medvedevskikh, Y. Karpov
Analytical chemistry and its three segments: fundamental science, chemical analysis and analytical control are associated with the determination of the chemical composition, which must be performed with the required accuracy. Inaccurate or erroneous results of chemical analysis can lead to negative and sometimes tragic consequences. The accuracy of the results is an integral part and a consequence of a whole range of measures to assure the quality of chemical analysis. Current article discusses the main elements of the quality system of chemical analysis and the current trends in solving urgent problems in this area. The first stage of the analytical process requires a clear understanding and documentation of the requirements on the part of the customer. A particular attention is paid to the contribution to the analysis uncertainty of the sampling. The principle of choosing an analytical method is considered, which is based on the type of sample, matrix, measured value etc. Approaches to the validation or certification of the methods and / or their verifications are generalized. It is shown that the basis for the validation of chemical analysis methods is the assessment of uncertainty. It is noted that this is not only a formalized procedure, but also methodologically competent support of the research process of developing an analysis method in terms of cleaning the analytical signal, ways to identify and eliminate sources of its distortion, and the choice of approaches to constructing the calibration dependencies and standard samples. Attention is drawn to the problem of the current state of education in analytical chemistry.
{"title":"Current quality issues in chemical analysis","authors":"V. B. Baranovskaya, M. Medvedevskikh, Y. Karpov","doi":"10.15826/analitika.2021.25.4.005","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.4.005","url":null,"abstract":"Analytical chemistry and its three segments: fundamental science, chemical analysis and analytical control are associated with the determination of the chemical composition, which must be performed with the required accuracy. Inaccurate or erroneous results of chemical analysis can lead to negative and sometimes tragic consequences. The accuracy of the results is an integral part and a consequence of a whole range of measures to assure the quality of chemical analysis. Current article discusses the main elements of the quality system of chemical analysis and the current trends in solving urgent problems in this area. The first stage of the analytical process requires a clear understanding and documentation of the requirements on the part of the customer. A particular attention is paid to the contribution to the analysis uncertainty of the sampling. The principle of choosing an analytical method is considered, which is based on the type of sample, matrix, measured value etc. Approaches to the validation or certification of the methods and / or their verifications are generalized. It is shown that the basis for the validation of chemical analysis methods is the assessment of uncertainty. It is noted that this is not only a formalized procedure, but also methodologically competent support of the research process of developing an analysis method in terms of cleaning the analytical signal, ways to identify and eliminate sources of its distortion, and the choice of approaches to constructing the calibration dependencies and standard samples. Attention is drawn to the problem of the current state of education in analytical chemistry.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253532","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}
Pub Date : 2021-01-01DOI: 10.15826/analitika.2021.25.4.001
A.V. Behterev, V. А. Labusov, A. Putmakov
On August 20 of this year, the VMK-Optoelektronika company – a leading Russian developer and manufacturer of spectral analytical equipment – celebrated its 30th anniversary. The company was founded by the team of developers that initially worked in the Spektr temporary inter-institutional collaboration group created in 1988 by the Chairman of the Presidium of the Siberian Branch of the Academy of Sciences Academician V.A. Koptyug to develop multichannel analyzers of optical spectra based on domestic photodiode arrays and operate them at the academic institutes of the Siberian Branch. Over the past period, the company has developed and produced multichannel analyzers of emission spectra (MAES) based on photodetector array assemblies to equip existing spectral instruments in analytical laboratories and create new ones; a wide range of spectrum sources; high-resolution high-aperture spectral devices; atomic emission spectrometers for the analysis of powders, metals, and liquids. Currently, enterprises in Russia and the CIS countries operate: - more than 600 spectral systems for atomic emission analysis developed on the basis of existing spectral devices by replacing photographic plates and photomultipliers with MAES analyzers; many of these systems also include Sharovaya Molniya and Vezuvii electric-arc and spark-discharge generators, Globula and Kristall spectroanalytical instruments, Potok electric-arc facilities for atomic emission analysis of powder samples by the spill-injection method, and other devices; - about 100 atomic emission spectrometers entirely consisting of devices developed by the company. The company has a leading position in the development of scintillation atomic emission spectral analysis of geological powder samples and simultaneous multielement electrothermal atomic absorption analysis of liquids.
{"title":"VMK-Optoelektronika company is 30 years old!","authors":"A.V. Behterev, V. А. Labusov, A. Putmakov","doi":"10.15826/analitika.2021.25.4.001","DOIUrl":"https://doi.org/10.15826/analitika.2021.25.4.001","url":null,"abstract":"On August 20 of this year, the VMK-Optoelektronika company – a leading Russian developer and manufacturer of spectral analytical equipment – celebrated its 30th anniversary. The company was founded by the team of developers that initially worked in the Spektr temporary inter-institutional collaboration group created in 1988 by the Chairman of the Presidium of the Siberian Branch of the Academy of Sciences Academician V.A. Koptyug to develop multichannel analyzers of optical spectra based on domestic photodiode arrays and operate them at the academic institutes of the Siberian Branch. Over the past period, the company has developed and produced multichannel analyzers of emission spectra (MAES) based on photodetector array assemblies to equip existing spectral instruments in analytical laboratories and create new ones; a wide range of spectrum sources; high-resolution high-aperture spectral devices; atomic emission spectrometers for the analysis of powders, metals, and liquids. Currently, enterprises in Russia and the CIS countries operate: - more than 600 spectral systems for atomic emission analysis developed on the basis of existing spectral devices by replacing photographic plates and photomultipliers with MAES analyzers; many of these systems also include Sharovaya Molniya and Vezuvii electric-arc and spark-discharge generators, Globula and Kristall spectroanalytical instruments, Potok electric-arc facilities for atomic emission analysis of powder samples by the spill-injection method, and other devices; - about 100 atomic emission spectrometers entirely consisting of devices developed by the company. The company has a leading position in the development of scintillation atomic emission spectral analysis of geological powder samples and simultaneous multielement electrothermal atomic absorption analysis of liquids.","PeriodicalId":37743,"journal":{"name":"Analitika i Kontrol","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67253948","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}
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