42 research outputs found
Variations in sea surface roughness induced by the 2004 Sumatra-Andaman tsunami
Observations of tsunamis away from shore are critically important for improving early warning systems and understanding of tsunami generation and propagation. Tsunamis are difficult to detect and measure in the open ocean because the wave amplitude there is much smaller than it is close to shore. Currently, tsunami observations in deep water rely on measurements of variations in the sea surface height or bottom pressure. Here we demonstrate that there exists a different observable, specifically, ocean surface roughness, which can be used to reveal tsunamis away from shore. The first detailed measurements of the tsunami effect on sea surface height and radar backscattering strength in the open ocean were obtained from satellite altimeters during passage of the 2004 Sumatra-Andaman tsunami. Through statistical analyses of satellite altimeter observations, we show that the Sumatra-Andaman tsunami effected distinct, detectable changes in sea surface roughness. The magnitude and spatial structure of the observed variations in radar backscattering strength are consistent with hydrodynamic models predicting variations in the near-surface wind across the tsunami wave front. Tsunami-induced changes in sea surface roughness can be potentially used for early tsunami detection by orbiting microwave radars and radiometers, which have broad surface coverage across the satellite ground track
Determination of gold and palladium in rocks and ores by atomic absorption spectrometry using two-stage probe atomization
© 2017, Pleiades Publishing, Ltd.The efficiency of two-stage probe atomization for the determination of gold and palladium in geological samples by electrothermal atomic absorption spectrometry is studied. The effects of temperature–time program and the position of the probe in an atomizer on the fractionation of sample components and the magnitude of the analytical signal are studied. It is demonstrated that gold and palladium can be quantitatively determined by atomic absorption spectrometry in rocks and ores, using a two-stage probe atomization with the limits of detection for gold and palladium 0.01 and 0.04 g/t, respectively
PrF3Van Vleck paramagnet as a promising material for the nuclear dynamic polarization of 3He
We suggest using insulating Van Vleck paramagnet PrF3 as a solid substrate for the dynamic polarization of 3He nuclei at high magnetic fields. The exploring of solid effect for this purpose assumes the knowledge of the optimal conditions for transfer of polarization from the Pr3+ electron shell in PrF3 to 141Pr nuclear spins as well as the existence of effective channel for magnetization transfer from 141Pr nuclear spins to nuclear spins of liquid 3He (so-called magnetic coupling phenomenon). To study solid effect in PrF 3 the magnetic field dependencies of the Stark energy levels of 3H4 ground state multiple were calculated for high magnetic fields up to 40 T using the set of crystal-field parameters obtained early from magnetization measurements and exchange charges model. Also the results of searching for a direct magnetic coupling between nuclei of the liquid 3He and 141Pr nuclei in the system "PrF3 powder - liquid 3He" by pulse NMR method are represented. Also the surface effects in the PrF3 crystal were studied by SQUID and optical microscopy measurements. Other aspects of the nuclear polarization transfer are discussed. © 2006 IOP Publishing Ltd
SAMPLE TRASFORMATION AT TWO-STAGE PROBE ATOMIZATION IN GRAPHITE FURNACE FOR ATOMIC ABSORPTION SPECTROMETRY
The surface of the U-shaped tungsten probe for a graphite furnace atomic absorption analysis with two-stage probe atomization was studied using scanning electron microscopy. The aim of the work was investigation of morphology of the sample after vapor phase transfer from the tube furnace to the tungsten probe and additional thermal treatment on the probe. It is shown for the sample having complex matrix (the slurry of milled up to 80 µm gold ore) that a polycrystalline layer of agglomerated particles of size less than 1 µm is formed on the surface of the probe after primary vaporization. After additional pyrolysis on the probe at the furnace temperature1500°Cthe deposit is modified into an amorphous film and drops of reduced metals with diameter up to 1 µm. In the case of simple matrix (water solution of palladium nitrate) a solid film with clots and flakes of 50 – 100 nm micro drops of palladium is deposited on the probe. The two stage treatment leads to the simplification of chemical and phase composition of the deposit and its localization on the probe tip within2 mm. This caused substantial improvement of analytical signal associated with atomization of the deposit from the probe inserted into the graphite furnace.Keywords: atomic absorption analysis, two-stage probe atomization, graphite furnace, ore, suspension, electron microscopy.(Russian)DOI:http://dx.doi.org/10.15826/analitika.2015.19.1.008Y.А. Zakharov, D.S. Irisov1, R.R. Haibullin, I.B. Chistyakov2Kazan (Volga region) Federal University, Kazan`, Russian Federation1LLC «Atzond», Kazan`, Russian Federation2LLC «Interlab», Moscow, Russian Federatio
Sample transformation at two-stage probe atomization in graphite furnace for atomic absorption spectrometry
С помощью растровой сканирующей электронной микроскопии исследована поверхность вольфрамового U-образного зонда, применяемого для двухстадийной зондовой атомизации проб в графитовой печи при атомно-абсорбционном анализе. Цель - проследить изменение состояния пробы после ее термической перегонки из печи на зонд и дополнительной термообработки на зонде. Показано, что в ходе первичной атомизации многокомпонентной по матричному составу пробы (суспензии размолотой до 80 мкм золотосодержащей руды), получается конденсатное отложение в виде слоя слипшихся поликристаллических частиц размером не более 1 мкм. После стадии пиролиза на зонде при температуре печи 1500⁰С это отложение превращается в оплавленную пленку с каплями восстановленных металлов диаметром до 1 мкм. В случае однокомпонентной по матричному составу пробы (водного раствора нитрата палладия) на зонде откладывается монолитная пленка со сгустками и хлопьями из микрокапель палладия размером 50-100 нм. В результате такого фракционирования химический состав пробы упрощается, а так же компактно локализуется на кончике зонда в пределах 2 мм. Это положительно сказывается на аналитическом сигнале, регистрируемом при вторичной атомизации конденсата с зонда, погружаемого в графитовую печь.The surface of the U-shaped tungsten probe for a graphite furnace atomic absorption analysis with two-stage probe atomization was studied using scanning electron microscopy. The aim of the work was investigation of morphology of the sample after vapor phase transfer from the tube furnace to the tungsten probe and additional thermal treatment on the probe. It is shown for the sample having multicomponent matrix (the slurry of milled up to 80 µm gold ore) that a polycrystalline layer of agglomerated particles of size less than 1 µm is formed on the surface of the probe after primary vaporization. After additional pyrolysis on the probe at the furnace temperature 1500 °C the deposit is modified into an amorphous film and drops of reduced metals with diameter up to 1 µm. In the case of single component matrix (water solution of palladium nitrate) a solid film with clots and flakes of 50-100 nm micro drops of palladium is deposited on the probe. The two stage treatment leads to the simplification of the sample deposit and its localization on the probe tip within 2 mm. This caused substantial improvement of analytical signal associated with atomization of the deposit from the probe inserted into the graphite furnace
Assessment of Resistance and Bioremediation Ability of Lactobacillus Strains to Lead and Cadmium
© 2017 Anna V. Kirillova et al.Cadmium (Cd) and lead (Pb) are heavy metals, important environmental pollutants, and potent toxicants to organism. Lactic acid bacteria (LAB) have been reported to remove Cd and Pb from solutions and therefore represent a useful tool for decontamination of food and beverages from heavy metals. Heavy metal ion binding by LAB was reported as metabolism-independent surface process. In this work ten Lactobacillus strains were investigated with respect to hydrophobicity, Lewis acid-base, and electrostatic properties of their outer cell surface in order to characterize their Cd and Pb removal capacity. Seven L. plantarum and L. fermentum strains were shown to remove Cd from culture medium. The metabolism-dependent accumulation mechanism of Cd removal was proposed based on extended character of Cd binding and lack of correlation between any of the surface characteristics and Cd removal. The results of this study should be considered when selecting probiotic strains for people at risk of Cd exposure
ПРЯМОЕ ОПРЕДЕЛЕНИЕ ЗОЛОТА В СУСПЕНЗИЯХ СТАНДАРТНЫХ ОБРАЗЦОВ ГОРНЫХ ПОРОД И РУДЫ МЕТОДОМ ЭЛЕКТРОТЕРМИЧЕСКОЙ АТОМНО-АБСОРБЦИОННОЙ СПЕКТРОМЕТРИИ ВЫСОКОГО РАЗРЕШЕНИЯ Ю.А. Захаров, Д.С. Ирисов, Р.В. Окунев, Р.Х. Мусин, Р.Р. Хайбуллин
High resolution continuum source atomic absorption spectrometer ContrAA-700 with graphite furnace is used for direct gold determination in rocks and ores on the level 10-6-10-3 % mas. Russian standard reference materials of gold containing ore СЗР-4 (2.13 ± 0.05 g/ton), black slates of Sykhoy Log СЛг-1 (2.50 ± 0.03 g/ton) and СЧС-1 (0.10 ± 0.02 g/ton) in mass 1 mg was inserted into the furnace in the suspension form prepared on the mix of concentrated HNO3 and HCl (1:3) with following sevenfold dilution by water. It was revealed that spectral lines of gold have dense fine structured spectral interferences of different molecules of the matrix. Absorption resonance line Au 242.8 nm is overlapped by left wing of very intensive SiO band. Twice as less sensitive line Au 267.6 nm is in a narrow gap between the molecular components. Strong matrix depression of the analytical signal and intensive background at usual one-stage atomization do the analysis impossible if gold concentration less 2 g/ton. Application of the additional accessory Atzond-1 for two-stage probe atomization provides ability for automatic dozing of the suspensions and reduces the matrix interference. Due to fractionation of the sample vapors on the tungsten probe the line Au 267.6 nm, in difference from resonance line Au 242.8 nm, is completely freed from the spectral overlapping and provides lower quantitative limit of gold determination 0.05 g/ton (Sr =30 %; n = 5; Р= 0.95).Keywords: atomic absorption spectrometry, graphite atomizer, double-stage probe atomization, gold, silver, rocks, ores, black slate, suspension (Russian)DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.004 Y.А. Zakharov, D.S. Irisov1, R.V. Okunev, R.Kh. Musin, R.R. HaibullinKazan (Volga region) Federal University, Kazan, Russian Federation1LLC «Atzond», Kazan, Russian FederationREFERENCES 1. Busev A.I., Ivanov V.M. Analiticheskaia khimiia zolota [Analytical chemistry of gold]. Moscow, Nauka, 1973. 263 p. (in Russian). 2. Vasilyeva I.E., Pozhidaev Yu.N., Vlasova N.N., Voronkov M.G., Philipchenko Yu.A. [Sorption-atomic-emission determination of gold, platinum and palladium in rocks and ores using sorbent PSTM-3Т]. Analitika i kontrol' [Analytics and control], 2010, vol. 14, no. 1, pp. 16-24. (in Russian). 3. Judelevich I.G., Starceva E.A. Atomno-absorbtsionnoe opredelenie blagorodnykh metallov [Atomic absorption determination of noble metals]. Novosibirsk, Nauka, 1981. 159 p. (in Russian). 4. Balaram V., Mathur R., Satyanarayanan M., Sawant S. S., Roy P., Subramanyam K. S. V., Kamala C. T., Anjaiah K. V., Ramesh S. L., Dasaram B. A Rapid Method for the Determination of Gold in Rocks, Ores and Other Geological Materials by F-AAS and GF-AAS After Separation and Preconcentration by DIBK Extraction for Prospecting Studies. MAPAN-Journal of Metrology Society of India, 2012, vol. 27, no. 2, pp. 87-95. doi: 10.1007/s12647-012-0012-2 5. Reddi G. S., Rao C. R. M. Analytical techniques for the determination of precious metals in geological and related materials. Analyst, 1999, vol. 124, pp. 1531-1540. 6. Shvetsov V. A. Probirnyi analiz pri razvedke zolotorudnykh mestorozhdenii. Diss. dokt. him. nauk. [The assay analysis at investigation of gold fields. Dr. chem. sci. diss.]. Irkutsk, 2006. 259 p. (in Russian). 7. Vasilyeva I.E., Shabanova E.V., Busko A.E., Kunaev A.B. [Estimation of Au- and Ag- particle sizes in geological samples using high time-resolved scintillation atomic emission analysis]. Analitika i kontrol' [Analytics and control], 2010, vol. 14, no. 4, pp. 201-213. (in Russian). 8. Konyshev V.O. [Experience of sampling error evaluation and development of methodology to explore a deposit with bonanza gold distribution]. Otechestvennaia geologiia [Domestic geology], 2004, no. 6, pp. 22-34. 9. Resano M., Aramendı´a M., Garcia-Ruiz E. and Belarra M. A. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of Au in samples of various natures. J. Anal. At. Spectrom., 2005, vol. 20, pp. 479-481. 10. Zakharov Y.А., Okunev R.V., Hasanova S.I., Irisov D.S., Haibullin R.R. [Atomic absorption determination of gold and silver in rocks and ores using double-stage probe atomization in the graphite furnace]. Analitika i kontrol' [Analytics and control], 2013, vol. 17, no. 4, pp. 414-422 (in Russian). 11. Welz B., Becker-Ross H., Florek S., Heitmann U. High-Resolution Continuum Source AAS: The Better Way to Do Atomic Absorption Spectrometry. Weinheim, WILLEY-VCH, Verlag GmbHCo. KGaA, 2005. 295 p. 12. Gunduz S., Akman S. Determination of lead in rice grains by solid sampling HR-CS GFAAS. Food Chemistry, 2013, vol. 141, pp. 2634-2638. 13. Boschetti W., Borges A.R., DuarteA.T., Dessuy M.B., Vale M.G.R., de Andrade J.B. and Welz B. Simultaneous determination of Mo and Ni in wine and soil amendments by HR-CS GF AAS. Anal. Methods, 2014, vol. 6, pp. 4247-4256. 14. Castilho I.N., Pereira E.R., Welz B., Shaltout A.A., Caraseka E. and Martens I.B.G. Determination of selenium in soil samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis. Anal. Methods, 2014, vol. 6, pp. 2870-2875. 15. Castilho I.N., Welz B., Vale M.G., de Andrade J.B., Smichowski P., Shaltout A.A., Colares L., Carasek E. Comparison of three different sample preparation procedures for the determination of traffic-related elements in airborne particulate matter collected on glass fiber filters. Talanta, 2012, vol. 88, pp. 689–695. 16. Resano M., Mozas E., Crespo C., Briceсo J., del Campo Menoyoa J. and Belarra M. A. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry to monitor the biodistribution of gold nanoparticles in mice tissue after intravenous administration. J. Anal. At. Spectrom., 2010, vol. 25. pp. 1864-1873. 17. Zakharov Y.A., Haibullin R.R., Irisov D. S., Sadykov M. F., Gainutdinov A. R. [Hardware-software complex for atomic absorption spectrometry with multistage probe atomization]. Naychnoe priborostroenie [Scientific instrumentation], 2013, vol. 23, no 4, pp. 104-111. 18. Federal state budgetary institution of science A.P. Vinogradov Institute of Geochemistry SB RAS. Available at: http://www.igc.irk.ru/Innovation/Standarts-obr/Catalog-2013.pdf (accessed 01 July 2014). 19. Pupyshev A.A. Atomno-absorbtsionnyi spectral`nyi analiz [Atomic absorption spectral analysis]. Moscow, Technosphera Publ., 2009. 782 с. (in Russian). 20. López-Garcia I., Campillo N., Arnau-Jerez I., Hernández-Córdoba M. Slurry sampling for the determination of silver and gold in soils and sediments using electrothermal atomic absorption spectrometry. Spectrochim. Acta, 2003, vol. 58B, pp. 1715-1721. 21. Kurilko S. S., Put'makov A. N., Labusov V. A., Borovikov V. M., Seliunin D. O. Materialy XIII Mezhdunarodnogo simpoziuma «Primenenie analizatorov MAJeS v promyshlennosti» [Proc. 13th Int. Symp. "The use of MAES analyzers in the industry"]. Novosibirsk, 2013, pp. 40-50 (in Russian). 22. Katskov D.A., Khanye G.E. Simultaneous Multi-Element Electrothermal Atomic Absorption Determination Using a Low Resolution CCD Spectrometer and Continuum Light Source: The Concept and Methodology. S. Afr. J. Chem., 2010, vol. 63, pp. 45-57. 23. Gibson J., Katskov D.A. Simultaneous Determination of Metals in Coal with Low-Resolution Continuum Source Atomic Absorption Spectrometer and Filter Furnace Atomizer. S. Afr. J. Chem,. 2011, vol. 64, pp. 79-87. 24. Katskov D.A., Sadagov Yu.M. Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry. Spectrochim. Acta, 2011, vol. 66B, pp. 451-460. 25. Kurfürst U. Solid Sample Analysis: Direct and Slurry Sampling Using GF-AAS and ETV-ICP. Berlin: Springer, 1998. 423 р. 26. Slurry sampling for direct analysis of solid materials by electrothermal atomic absorption spectrometry (ETAAS). A literature review from 1990 to 2000 / M.J. Cal-Prieto et [al.] // Talanta. 2002. V. 56. P. 1-51. 27. Zakharov Y.A., Kokorina O.B., Gil'mutdinov A.K. [Concentrating of determined elements on the probe in electrothermal atomizer]. Zhurnal prikladnoi spektroskopii [Journal of Applied Spectroscopy], 2005, vol. 72, no. 2, pp. 256-259 (in Russian).Атомно-абсорбционный спектрометр высокого разрешения ContrAA-700 с графитовой печью применен для прямого определения золота в горных породах и рудах на уровне 10-6-10-3 % мас.В печь вводили навески 1 мг стандартных образцов золотосодержащей руды СЗР-4 (2.13 ± 0.05 г/т), черных сланцев Сухого Лога СЛг-1 (2.5 ± 0.3 г/т) и СЧС-1 (0.10 ± 0.02 г/т) в виде суспензий, приготовленных на смеси концентрированных HNO3 и HCl (1 : 3) с последующим семикратным разбавлением водой. Выявлено наличие плотного окружения спектральных линий золота тонко структурированнымиполосами поглощения разнообразных молекул матрицы. Резонансная линия поглощения Au 242.8 нм перекрыта левым крылом очень интенсивной полосы SiO. В два раза менее чувствительная линия Au 267.6 нм находится в узком промежутке между спектральными молекулярными компонентами. Из-за сильного подавления аналитического сигнала и интенсивного неселективного поглощения определение с использованием одностадийной атомизации крайне затруднено и может осуществляться при концентрации золота не менее 2 г/т. Использование приставки АТЗОНД-1 для осуществления двухстадийной зондовой атомизации позволило автоматически дозировать суспензии и снизить матричные помехи. За счет фракционирования паров пробы на вольфрамовом зонде линия Au 267.6 нм, в отличие от резонансной линии Au 242.8 нм, освобождается от спектральных наложений и обеспечивает более низкий предел количественного определения золота 0.05 г/т (Sr =30 %; n = 5; Р = 0.95).Ключевые слова: атомно-абсорбционная спектрометрия, графитовый атомизатор, суспензия, золото, горная порода, черный сланец, двухстадийная зондовая атомизация DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.004 ЛИТЕРАТУРА1. Бусев А.И., Иванов В.М. Аналитическая химия золота. М.: Наука, 1973. 263 с.2. Сорбционно-атомно-эмиссионное определение золота, платины и палладия в горных породах и рудах с использованием сорбента ПСТМ-З / И.Е. Васильева [и др.] // Аналитика и контроль. 2010. Т. 14, № 1. С. 16-24.3. Юделевич И.Г., Старцева Е.А. Атомно-абсорбционное определение благородных металлов. Новосибирск: Наука, 1981. 159 с.4. ARapid Method for the Determination of Gold in Rocks, Ores and Other Geological Materials by F-AAS and GF-AAS After Separation and Preconcentration by DIBK Extraction for Prospecting Studies / V. Balaram [et al.] // MAPAN-Journal of Metrology Society of India. 2012. V. 27, № 2. P. 87-95.5. Reddi G.S., Rao C.R.M. Analytical techniques for the determination of precious metals in geological and related materials // Analyst. 1999. V. 124. P. 1531-1540.6. Швецов В.А. Пробирный анализ при разведке золоторудных месторождений: дис. … д-ра хим. наук. Иркутск, 2006. 259 с.7. Методика определения содержания золота и серебра в геологических образцах с использованием сцинтилляционного атомно-эмиссионного анализа с высоким временным разрешением/ И.Е. Васильева [и др.] // Аналитика и контроль. 2010. Т. 14, № 4. С. 201-213.8. Конышев В.О. Опыт оценки погрешностей опробования и совершенствование методологии разведки месторождения с бонанцевым распределением золота // Отечественная геология, 2004. № 6. С. 22-34.9. Solid sampling-graphite furnace atomic absorption spectrometry for the direct determination of Au in samples of various natures / M. Resano [et al.] // J. Anal. At. Spectrom. 2005. V. 20. 479-481.10. Атомно-абсорбционное определение золота и серебра в породах и рудах с помощью двухстадийной зондовой атомизации в графитовой печи / Ю.А. Захаров [и др.] // Аналитика и контроль. 2013. Т. 17, № 4. С. 414-422.11. Welz B., Becker-Ross H., Florek S., Heitmann U. High-Resolution Continuum Source AAS: The Better Way to Do Atomic Absorption Spectrometry. Weinheim, WILLEY-VCH, Verlag GmbHCo. KGaA. 2005. 295 p.12. Gunduz S., Akman S. Determination of lead in rice grains by solid sampling HR-CS GFAAS // Food Chemistry. 2013. V. 141. P. 2634-2638.13. Simultaneous determination of Mo and Ni in wine and soil amendments by HR-CS GF AAS / W. Boschetti [et al.] // Anal. Methods. 2014. V. 6. P. 4247-4256.14. Determination of selenium in soil samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis / I.N.B. Castilho [et al.] // Anal. Methods. 2014. V. 6. P. 2870-2875.15. Comparison of three different sample preparation procedures for the determination of traffic-related elements in airborne particulate matter collected on glass fiber filters / I.N.B. Castilho [et al.] // Talanta. 2012. V. 88. P. 689-695.16. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry to monitor the biodistribution of gold nanoparticles in mice tissue after intravenous administration / M. Resano [et al.] // J. Anal. At. Spectrom. 2010. V. 25. P. 1864-1873.17. Аппаратно-программный комплекс для атомно-абсорбционной спектрометрии с многостадийной зондовой атомизацией / Ю.А. Захаров [и др.] // Научное приборостроение. 2013. Т. 23. №4. C. 104-111.18. Сайт Института геохимии им. А.П. Виноградова СО РАН [Электронный ресурс]: http://www.igc.irk.ru/Innovation/Standarts-obr/Catalog-2013.pdf (дата обращения: 01.07.2014).19. Пупышев А.А. Атомно-абсорбционный спектральный анализ. М.: Техносфера, 2009. 782 с.20. Slurry sampling for the determination of silver and gold in soils and sediments using electrothermal atomic absorption spectrometry / I. Lopez-Garcia [et al.] // Spectrochim. Acta. 2003. V. 58 B. P. 1715-1721.21. Разработка источника атомно-абсорбционного спектра для одновременного многоэлементного анализа / С.С. Курилко и [др.] // Материалы XIII Международного симпозиума «Применение анализаторов МАЭС в промышленности», Новосибирск, 2013. С. 40-50.22. Katskov D.A., Khanye G.E. Simultaneous Multi-Element Electrothermal Atomic Absorption Determination Using a Low Resolution CCD Spectrometer and Continuum Light Source: The Concept and Methodology // S. Afr. J. Chem. 2010. V. 63. P. 45-57.23. Gibson J., Katskov D.A. Simultaneous Determination of Metals in Coal with Low-Resolution Continuum Source Atomic Absorption Spectrometer and Filter Furnace Atomizer // S. Afr. J. Chem. 2011. V. 64. P. 79-87.24. Katskov D.A., Sadagov Yu.M. Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry// Spectrochim. Acta. 2011. V. 66B. P. 451-460.25. Kurfürst U. Solid Sample Analysis: Direct and Slurry Sampling Using GF-AAS and ETV-ICP. Berlin: Springer, 1998. 423 р.26. Slurry sampling for direct analysis of solid materials by electrothermal atomic absorption spectrometry (ETAAS). A literature review from 1990 to 2000 / M.J. Cal-Prieto et [al.] // Talanta. 2002. V. 56. P. 1-51.27. Концентрирование определяемых элементов на зонде в электротермическом атомизаторе / Ю.А. Захаров [и др.] // Журн. прикл. спектр. 2005. Т. 72, № 2. С. 256–259
ПРЯМОЕ АТОМНО-АБСОРБЦИОННОЕ ОПРЕДЕЛЕНИЕ СВИНЦА И КАДМИЯ В ПИТЬЕВЫХ МОЛОЧНЫХ ПРОДУКТАХ С ПОМОЩЬЮ ДВУХСТАДИЙНОЙ ЗОНДОВОЙ АТОМИЗАЦИИ В ГРАФИТОВОЙ ПЕЧИ
The method of the direct atomic absorption determination of Pb and Cd in milk, cream and powder baby formula using the accessory ATZOND-1 for commercial graphite furnace is offered. The limits of detection have been improved in comparison with methods of traditional one-stage atomization and they are equal: in the liquid foods (in µg/l) for Pb – 0.5, Cd – 0.04; in the powder baby formula (in µg/kg) for Pb – 1.7 , Cd – 0.14. Preliminary mineralization of the probes is excepted and duration of the analysis is shortened. For maximum permissible inRussiaconcentrations: of lead 50 µg/kg RSD 3 %; of cadmium 20 µg/kg RSD 12%.Keywords: direct atomic absorbtion analysis, graphite atomizer, double-stage probe atomization, milk, milk foods(Russian)DOI: http://dx.doi.org/10.15826/analitika.2013.17.3.002Y.А. Zakharov, О.B. Kokorina, D.S. Irisov1, R.R. Haibullin1, S.I. Hasanova Kazan (Volga region) Federal University, Kazan, Russian Federation1LLC «Atzond», Kazan, Russian Federation Описан способ прямого атомно-абсорбционного анализа цельного молока, сливок и порошковой молочной смеси для детского питания на содержание свинца и кадмия с использованием приставки АТЗОНД-1. Пределы обнаружения улучшены по сравнению с методикой, использующей традиционную одностадийную атомизацию, и составляют в жидких продуктах (в мкг/л) для Pb – 0.5, для Cd – 0.04, а в порошковых смесях (в мкг/кг) соответственно 1.7 и 0.14. Сокращена длительность анализа за счет исключения предварительной минерализации проб. Для концентраций на уровне действующих в России ПДК свинца 50 мкг/кг Sr 3 %, кадмия 20 мкг/кг Sr 12 %.Ключевые слова: прямой атомно-абсорбционный анализ, графитовый атомизатор, двухстадийная зондовая атомизация, молоко, молочные продукты DOI: http://dx.doi.org/10.15826/analitika.2013.17.3.002 Литература1. Методика выполнения измерения массовой концентрации цинка, кадмия, меди, свинца в пробах молока атомно-абсорбционным методом с электротермической атомизацией на атомно-абсорбционном спектрометре "МГА –915". Свид-во № 224.04.05.001/2002. Шифр М 04-25-2001.2. ГОСТ 30178-96 Сырье и продукты пищевые. Атомно-абсорбционный метод определения токсичных элементов.3. Методика выполнения измерений массовой доли свинца и кадмия в пищевых продуктах и продовольственном сырье методом электротермической атомно-абсорбционной спектрометрии. Методические указания МУК 4.1.986-00 (утв. Главным государственным санитарным врачом РФ 13.10.2000).4. [Электронный ресурс]: http://publications.jrc.ec.europa.eu/repository/bitstream/111111111/25471/1/jrc68255%20imep33%20final.pdf / IMEP-33: Total cadmium and lead in baby food. Interlaboratory Comparison Report. European Commission Joint Research Centre Institute for Reference Materials and Measurements, December 2011 (дата обращения: 25.07.2013).5. [Электронный ресурс]: http://irmm.jrc.ec.europa.eu/interlaboratory_comparisons/Documents/EUR%2025177%20EN%20-%20IMEP-113.pdf / IMEP-113: Total cadmium and lead in baby food. Interlaboratory Comparison Report. European Commission Joint Research Centre Institute for Reference Materials and Measurements, December 2011 (дата обращения: 25.07.2013).6. Прямой атомно-абсорбционный анализ почв с помощью приставки Атзонд-1 для двухстадийной зондовой атомизации в графитовой печи / Ю.А. Захаров и [др.] // Аналитика и контроль. 2013. Т. 17, № 2. С. 159-169.7. Прямое определение марганца, меди, свинца и ртути в биопробах методом зеемановской атомно-абсорбционной спектрометрии с высокочастотной модуляцией поляризации / А.А. Ганеев и [др.] // Ж. аналит. химии. 1999. Т. 54. С. 69-77.8. Прямое определение элементов в пробах сложного состава методом зеемановской атомно-абсорбционной спектрометрии с высокочастотной модуляцией поляризации / А.А. Ганеев и [др.] // Заводская лаборатория. Диагностика материалов. 1999. Т. 65. С. 14-23.9. Прямое атомно-абсорбционное определение содержания Ni и V в нефти / Н.Б. Иваненко и [др.] // Ж. прикл. химии. 2006. Т. 79. С. 1562-1565.10. Application of Zeeman Graphite Furnace Atomic Absorption Spectrometry with High-Frequency Modulation Polarization for the Direct Determination of Aluminum, Beryllium, Cadmium, Chromium, Mercury, Manganese, Nickel, Lead, and Thallium in Human Blood / N.B. Ivanenko et [al.] // Arch. Environ. Contam. Toxicol. 2012. V. 63 P. 299-308.11. Казимиров В.И., Зорин А.Д., Занозина В.Ф. Определение Cu, Sb, Pb методом атомно-абсорбционной спектроскопии с непламенной атомизацией при исследовании компонентов продуктов выстрела // Вестник ННГУ. Серия Химия. 2004. № 1. С. 225-233.12. Спектрометр атомно-абсорбционный МГА-915, МГА-915М, МГА-915МД. Руководство по эксплуатации. Санкт-Петербург. 2011 г.13. Захаров Ю.А., Кокорина О.Б., Гильмутдинов А.Х. Электротермическая атомизация веществ с фракционной конденсацией определяемого элемента на зонде // Ж. прикл. спектр. 2005. Т. 72, № 1. С. 124-128.
The study of the system "van Vleck paramagnet PrF3-Helium- 3"
Present paper is the result of experimental investigations of the system "Van Vleck paramagnet PrF3 - liquid 3He", where earlier cross-relaxation effect between liquid 3He nuclei and 141Pr nuclei was discovered. We report on 141Pr spin kinetics in Van Vleck paramagnet crystal powders PrF3 with different paramagnet impurities. All experiments have been made by pulse NMR methods at temperature 1.5 K. © 2009 IOP Publishing Ltd