WO2008007998A1 - X-ray fluorescence analyser for determining a sulphur content in liquid hydrocarbons - Google Patents
X-ray fluorescence analyser for determining a sulphur content in liquid hydrocarbons Download PDFInfo
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- WO2008007998A1 WO2008007998A1 PCT/RU2007/000220 RU2007000220W WO2008007998A1 WO 2008007998 A1 WO2008007998 A1 WO 2008007998A1 RU 2007000220 W RU2007000220 W RU 2007000220W WO 2008007998 A1 WO2008007998 A1 WO 2008007998A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
- G01N33/287—Sulfur content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/307—Accessories, mechanical or electrical features cuvettes-sample holders
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/637—Specific applications or type of materials liquid
Definitions
- the utility model relates to the field of X-ray fluorescence analysis and can be used to determine the concentration of sulfur in oil, oil products and other liquid hydrocarbons.
- a device for determining the concentration of sulfur in liquid hydrocarbons containing a cuvette in which the analyzed liquid hydrocarbon; at the bottom of the cuvette a window is made, covered with a film transparent to x-ray radiation; under the cuvette are an X-ray tube and a X-ray fluorescence detector emanating from the analyte, which is connected to a spectral analyzer, the output of which is connected to the processor device, see http://www.practicingoilanalysis.com.
- an X-ray fluorescence analyzer of sulfur content in liquid hydrocarbons including an x-ray source, a cuvette for placing an analyte, equipped with a window made in the bottom of the cuvette; the window is closed with an X-ray transparent film; there is also a detector of x-ray fluorescence radiation emanating from the analyte after its exposure to x-rays; the detector and the x-ray source are placed under the cell; the detector output is connected to the input of a spectral analyzer, the output of which is connected to the input of an electronic computing device, the output of which is connected to the input of the information display unit, JP2000065764 A.
- Known X-ray fluorescence analyzer of sulfur content in liquid hydrocarbons including a cuvette for placement of the analyte, in the side wall of which there is a window closed by a film transparent to x-ray radiation, an x-ray source located on the side of the cell from the side of the window; X-ray fluorescence detector emitting from the analyte, located opposite to the radiation source on the other side of the cuvette, electronic computing device and information display unit, RU 94023383 Al.
- the device the information of which is given in the description of RU 94023383 Al, is adopted as a prototype of this utility model.
- X-ray radiation decays sharply in a liquid.
- the X-ray fluorescence detector senses this radiation only from a thin layer of liquid adjacent to it ( ⁇ lmm). Therefore, with the opposite arrangement of the x-ray source and the X-ray fluorescence detector, the latter should be excited in the entire volume of the liquid. This necessitates the use of very powerful sources of x-ray radiation, which requires appropriate reinforced means of protection against this radiation.
- the present utility model is based on solving the problem of reducing the power of an x-ray source of an x-ray fluorescence emitter and, accordingly, simplifying the design of the device as a whole.
- this problem is solved due to the fact that in the X-ray fluorescence analyzer the sulfur content in liquid hydrocarbons, including a cuvette for placing the analyte, in the side wall of which there is a window closed by an X-ray transparent film, an x-ray source located on the side of the cuvette with side of the window, a detector of x-ray fluorescence emanating from the analyte, a spectral analyzer of the detector output signal, electronically calculates
- the device and the information display unit, the X-ray source and the X-ray fluorescence detector emanating from the analyte are located on one side relative to the cell.
- the applicant has not identified sources containing information on technical solutions identical to this utility model, which allows us to conclude that it meets the “new” (N) criterion.
- the required power of the x-ray source is significantly reduced, since the x-ray fluorescence radiation is not excited in the entire volume of liquid hydrocarbon, but only in a thin layer of liquid adjacent to the X-ray source and the X-ray fluorescence detector.
- the X-ray fluorescence analyzer of the sulfur content in liquid hydrocarbons includes a source of 1 x-ray radiation, in a specific example, an X-ray tube type BX-7.
- a source of 1 x-ray radiation in a specific example, an X-ray tube type BX-7.
- the cell 2 is the analyte 3, in particular gasoline.
- the cuvette 2 has a window closed by a film 4 transparent to x-ray radiation.
- Detector 5 is, in this example, a SI-12 type gas proportional counter.
- Spectrum analyzer 6 is a differential amplitude discriminator.
- the electronic computing device 7 is an SRI processor 188-5, the output of which is connected to the input of the information display unit 8.
- Block 8 in this example is a sign-integrated liquid crystal module WMC1604M with a thermal printer “KP-KTM-01”.
- the output of the detector 5 is connected to the input of the spectral analyzer 6, the output of which is connected to the input of the electronic computing device 7, the output of which is connected to the input of the information display unit 8.
- the cell window 2, closed by a film 4, is made in the side wall of the cell.
- the X-ray source 1 and the X-ray fluorescence detector 5 emanating from the analyte 3 are located on the side of the cell 2 from the side of the window closed by the film 4. Under the cell 2 there is a pallet 9.
- the device operates as follows. X-ray radiation emanating from source 1 penetrates through the film 4, which closes the window in the side wall of the cell 2, which contains the analyzed fluid. In the interaction of x-rays with liquid atoms, a secondary, so-called, x-ray fluorescence radiation occurs, the spectral composition of which is determined by the chemical composition of the analyzed liquid.
- X-ray fluorescence radiation from a liquid layer 3 adjacent to the film 4 passes through the film 4 and enters the X-ray detector 5.
- the detector captures the x-ray quanta that fall into it in the form of pulses of an electrical signal whose amplitude is proportional to the energy of the quanta.
- the signal from the detector enters the spectral analyzer 6, which "cuts out” from the amplitude spectrum the interval corresponding to the energy of the sulfur line.
- the digital signal from the spectral analyzer enters the electronic computing device 7, which controls the installation and determines the mass fraction of sulfur in the analyzed liquids.
- the analysis results are sent to the information display unit S. In case of violation of the integrity of the film 4, the analyzed liquid will fall into the tray 9.
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Abstract
Description
Рентгенофлуоресцентный анализатор содержания серы в жидких углеводородах X-ray fluorescence analyzer of sulfur content in liquid hydrocarbons
Область техникиTechnical field
Полезная модель относится к области рентгенофлуоресцентного анализа и может быть использована для определения концентрации серы в нефти, нефтепродуктах и других жидких углеводородах.The utility model relates to the field of X-ray fluorescence analysis and can be used to determine the concentration of sulfur in oil, oil products and other liquid hydrocarbons.
Предшествующий уровень техникиState of the art
Известно устройство для определения концентрации серы в жидких углеводородах, содержащее кювету, в которой размещается анализируемый жидкий углеводород; в дне кюветы выполнено окно, закрытое пленкой, прозрачной для рентгеновского излучения; под кюветой расположены рентгеновская трубка и детектор рентгенофлуоресцентного излучения, исходящего от анализируемого вещества, который соединен со спектральным анализатором, выход которого связан с процессорным устройством, см. http://www.practicingoilanalysis.com.A device for determining the concentration of sulfur in liquid hydrocarbons, containing a cuvette in which the analyzed liquid hydrocarbon; at the bottom of the cuvette a window is made, covered with a film transparent to x-ray radiation; under the cuvette are an X-ray tube and a X-ray fluorescence detector emanating from the analyte, which is connected to a spectral analyzer, the output of which is connected to the processor device, see http://www.practicingoilanalysis.com.
Известен также рентгенофлуоресцентный анализатор содержания серы в жидких углеводородах, включающий источник рентгеновского излучения, кювету для размещения анализируемого вещества, снабженную окном, выполненным в дне кюветы; окно закрыто прозрачной для рентгеновского излучения пленкой; также имеется детектор рентгенофлуоресцентного излучения, исходящего от анализируемого вещества после его облучения рентгеновскими лучами; детектор и источник рентгеновского излучения размещены под кюветой; выход детектора соединен со входом спектрального анализатора, выход которого соединен со входом электронно- вычислительного устройства, выход которого соединен со входом блока отображения информации, JP2000065764 А.Also known is an X-ray fluorescence analyzer of sulfur content in liquid hydrocarbons, including an x-ray source, a cuvette for placing an analyte, equipped with a window made in the bottom of the cuvette; the window is closed with an X-ray transparent film; there is also a detector of x-ray fluorescence radiation emanating from the analyte after its exposure to x-rays; the detector and the x-ray source are placed under the cell; the detector output is connected to the input of a spectral analyzer, the output of which is connected to the input of an electronic computing device, the output of which is connected to the input of the information display unit, JP2000065764 A.
Данное техническое решение, практически, имеет такую же конструкцию, что и описанный выше аналог. В случае нарушения целостности пленки, анализируемое вещество попадает на источник рентгеновского излучения и детектор, что приводит к выходу их из строя. Поэтому их отделяют от кюветы дополнительной защитной полупрозрачной пленкой.This technical solution, in practice, has the same design as the analogue described above. In the event of a violation of the integrity of the film, the analyte enters the x-ray source and detector, which leads to their failure. Therefore, they are separated from the cell by an additional protective translucent film.
Это вызывает экспоненциальное увеличение поглощения рентгенофлуоресцентного излучения, что резко снижает чувствительность анализатора; кроме того, поскольку защитная пленка вносит дополнительные помехи в работу анализатора, главным образом, из-за ее загрязнения в процессе эксплуатации, а также и из-за неравномерности ее толщины и плотности, существенно снижается точность результатов анализа.This causes an exponential increase in the absorption of x-ray fluorescence radiation, which dramatically reduces the sensitivity of the analyzer; in addition, since the protective film introduces additional interference into the operation of the analyzer, mainly due to its contamination during operation, as well as due to the unevenness of its thickness and density, the accuracy of the analysis results is significantly reduced.
Известен рентгенофлуоресцентный анализатор содержания серы в жидких углеводородах, включающий кювету для размещения анализируемого вещества, в боковой стенке которой выполнено окно, закрытое прозрачной для рентгеновского излучения пленкой, источник рентгеновского излучения, расположенный сбоку от кюветы со стороны окна; детектор рентгенофлуоресцентного излучения, исходящего от анализируемого вещества, расположенный оппозитно источнику излучения с другой стороны кюветы, электронно-вычислительное устройство и блок отображения информации, RU 94023383 Al.Known X-ray fluorescence analyzer of sulfur content in liquid hydrocarbons, including a cuvette for placement of the analyte, in the side wall of which there is a window closed by a film transparent to x-ray radiation, an x-ray source located on the side of the cell from the side of the window; X-ray fluorescence detector emitting from the analyte, located opposite to the radiation source on the other side of the cuvette, electronic computing device and information display unit, RU 94023383 Al.
Устройство, информация о котором приведена в описании к RU 94023383 Al, принято в качестве прототипа настоящей полезной модели.The device, the information of which is given in the description of RU 94023383 Al, is adopted as a prototype of this utility model.
Рентгеновское излучение резко затухает в жидкости. В то же время детектор рентгенофлуоресцентного излучения воспринимает это излучение лишь от смежного с ним тонкого слоя жидкости (<lмм). Поэтому при оппозитном расположении источника рентгеновского излучения и детектора рентгенофлуоресцентного излучения последнее должно возбуждаться во всем объеме жидкости. Это обусловливает необходимость использования весьма мощных источников рентгеновского излучения, что требует соответствующих усиленных средств защиты от этого излучения.X-ray radiation decays sharply in a liquid. At the same time, the X-ray fluorescence detector senses this radiation only from a thin layer of liquid adjacent to it (<lmm). Therefore, with the opposite arrangement of the x-ray source and the X-ray fluorescence detector, the latter should be excited in the entire volume of the liquid. This necessitates the use of very powerful sources of x-ray radiation, which requires appropriate reinforced means of protection against this radiation.
Раскрытие изобретения В основу настоящей полезной модели положено решение задачи снижения мощности источника рентгеновского излучения рентгенофлуоресцентного излучателя и, соответственно, упрощения конструкции устройства в целом.Disclosure of invention The present utility model is based on solving the problem of reducing the power of an x-ray source of an x-ray fluorescence emitter and, accordingly, simplifying the design of the device as a whole.
Согласно полезной модели эта задача решается за счет того, что в рентгенофлуоресцентном анализаторе содержания серы в жидких углеводородах, включающем кювету для размещения анализируемого вещества, в боковой стенке которой выполнено окно, закрытое прозрачной для рентгеновского излучения пленкой, источник рентгеновского излучения, расположенный сбоку от кюветы со стороны окна, детектор рентгенофлуоресцентного излучения, исходящего от анализируемого вещества, спектральный анализатор выходного сигнала детектора, электронно- вычислительное устройство и блок отображения информации, источник рентгеновского излучения и детектор рентгенофлуоресцентного излучения, исходящего от анализируемого вещества, расположены с одной стороны относительно кюветы. Заявителем не выявлены источники, содержащие информацию о технических решениях, идентичных настоящей полезной модели, что позволяет сделать вывод о ее соответствии критерию «нoвизнa» (N).According to a utility model, this problem is solved due to the fact that in the X-ray fluorescence analyzer the sulfur content in liquid hydrocarbons, including a cuvette for placing the analyte, in the side wall of which there is a window closed by an X-ray transparent film, an x-ray source located on the side of the cuvette with side of the window, a detector of x-ray fluorescence emanating from the analyte, a spectral analyzer of the detector output signal, electronically calculates The device and the information display unit, the X-ray source and the X-ray fluorescence detector emanating from the analyte are located on one side relative to the cell. The applicant has not identified sources containing information on technical solutions identical to this utility model, which allows us to conclude that it meets the “new” (N) criterion.
Благодаря реализации отличительных признаков полезной модели существенно снижается потребная мощность источника рентгеновского излучения, поскольку рентгенофлуоресцентное излучение возбуждается не во всем объеме жидкого углеводорода, а только в тонком слое жидкости, прилежащем к источнику рентгеновского излучения и детектору рентгенофлуоресцентного излучения.Due to the implementation of the distinguishing features of the utility model, the required power of the x-ray source is significantly reduced, since the x-ray fluorescence radiation is not excited in the entire volume of liquid hydrocarbon, but only in a thin layer of liquid adjacent to the X-ray source and the X-ray fluorescence detector.
Краткое описание чертежейBrief Description of the Drawings
В дальнейшем изобретение поясняется подробным описанием примеров его осуществления со ссылкой на чертеж, на котором представлена схема устройства.The invention is further explained in the detailed description of examples of its implementation with reference to the drawing, which shows a diagram of the device.
Лучший вариант осуществления изобретенияThe best embodiment of the invention
Рентгенофлуоресцентный анализатор содержания серы в жидких углеводородах включает источник 1 рентгеновского излучения, в конкретном примере рентгеновскую трубку прострельного типа БX-7. В кювете 2 находится анализируемое вещество 3, в частности, бензин. Кювета 2 имеет окно, закрытое пленкой 4, прозрачной для рентгеновского излучения. Детектор 5 представляет собой в данном примере газовый пропорциональный счетчик типа СИ- 12. Спектральный анализатор 6 представляет собой дифференциальный амплитудный дискриминатор.The X-ray fluorescence analyzer of the sulfur content in liquid hydrocarbons includes a source of 1 x-ray radiation, in a specific example, an X-ray tube type BX-7. In the cell 2 is the analyte 3, in particular gasoline. The cuvette 2 has a window closed by a film 4 transparent to x-ray radiation. Detector 5 is, in this example, a SI-12 type gas proportional counter. Spectrum analyzer 6 is a differential amplitude discriminator.
Электронно-вычислительное устройство 7 представляет собой процессорное устройство СРИ 188-5, выход которого соединен со входом блока 8 отображения информации. Блок 8 в данном примере представляет собой знакоинтегрирующий жидкокристаллический модуль WMC1604M с термопринтером «Mepкypий KTM-01».The electronic computing device 7 is an SRI processor 188-5, the output of which is connected to the input of the information display unit 8. Block 8 in this example is a sign-integrated liquid crystal module WMC1604M with a thermal printer “KP-KTM-01”.
Выход детектора 5 соединен со входом спектрального анализатора 6, выход которого соединен со входом электронно- вычислительного устройства 7, выход которого соединен со входом блока 8 отображения информации. Окно кюветы 2, закрытое пленкой 4, выполнено в боковой стенке кюветы. Источник 1 рентгеновского излучения и детектор 5 рентгенофлуоресцентного излучения, исходящего от анализируемого вещества 3, расположены сбоку от кюветы 2 со стороны окна, закрытого пленкой 4. Под кюветой 2 расположен поддон 9. Устройство работает следующим образом. Рентгеновское излучение, исходящее из источника 1, проникает через пленку 4, закрывающую окно в боковой стенке кюветы 2, в которой содержится анализируемая жидкость. При взаимодействии рентгеновского излучения с атомами жидкости возникает вторичное, так называемое, рентгенофлуоресцентное излучение, спектральный состав которого определяется химическим составом анализируемой жидкости.The output of the detector 5 is connected to the input of the spectral analyzer 6, the output of which is connected to the input of the electronic computing device 7, the output of which is connected to the input of the information display unit 8. The cell window 2, closed by a film 4, is made in the side wall of the cell. The X-ray source 1 and the X-ray fluorescence detector 5 emanating from the analyte 3 are located on the side of the cell 2 from the side of the window closed by the film 4. Under the cell 2 there is a pallet 9. The device operates as follows. X-ray radiation emanating from source 1 penetrates through the film 4, which closes the window in the side wall of the cell 2, which contains the analyzed fluid. In the interaction of x-rays with liquid atoms, a secondary, so-called, x-ray fluorescence radiation occurs, the spectral composition of which is determined by the chemical composition of the analyzed liquid.
Рентгенофлуоресцентное излучение от слоя жидкости 3, прилегающего к пленке 4, проходит сквозь пленку 4 и попадает в детектор 5 рентгеновского излучения. Детектор фиксирует попадающие в него рентгеновские кванты в виде импульсов электрического сигнала, амплитуда которых пропорциональна энергии квантов. Сигнал с детектора поступает в спектральный анализатор 6, который «выpeзaeт» из амплитудного спектра интервал, соответствующий энергии линии серы. Цифровой сигнал со спектрального анализатора попадает в электронно- вычислительное устройство 7, которое управляет работой установки и определяет массовую долю серы в анализируемой жидкости. Результаты анализа поступают в блок S отображения информации. В случае нарушения целостности пленки 4 анализируемая жидкость попадет в поддон 9. При этом не требуется дополнительная защитная полупрозрачная пленка. Поскольку в заявленном устройстве рентгенофлуоресцентное излучение возбуждается лишь в тонком слое прилегающем к пленке 4, значительно уменьшается требуемая мощность источника рентгеновского излучения и, соответственно, габариты, материалоемкость и стоимость устройства в целом.X-ray fluorescence radiation from a liquid layer 3 adjacent to the film 4 passes through the film 4 and enters the X-ray detector 5. The detector captures the x-ray quanta that fall into it in the form of pulses of an electrical signal whose amplitude is proportional to the energy of the quanta. The signal from the detector enters the spectral analyzer 6, which "cuts out" from the amplitude spectrum the interval corresponding to the energy of the sulfur line. The digital signal from the spectral analyzer enters the electronic computing device 7, which controls the installation and determines the mass fraction of sulfur in the analyzed liquids. The analysis results are sent to the information display unit S. In case of violation of the integrity of the film 4, the analyzed liquid will fall into the tray 9. In this case, no additional protective translucent film is required. Since in the inventive device x-ray fluorescence radiation is excited only in a thin layer adjacent to the film 4, the required power of the x-ray source and, accordingly, the dimensions, material consumption and cost of the device as a whole are significantly reduced.
Промышленная применимостьIndustrial applicability
Для реализации полезной модели использовано известное оборудование и материалы, что позволяет сделать вывод о ее соответствии критерию промышленная применимость)) (IA). To implement the utility model, well-known equipment and materials were used, which allows us to conclude that it meets the criterion of industrial applicability)) (IA).
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| RU2006126766 | 2006-07-14 | ||
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2011002983A1 (en) | 2009-07-02 | 2011-01-06 | Dow Global Technologies Inc. | Tpo compositions, articles, and methods of making the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU94023383A (en) * | 1994-06-20 | 1996-08-27 | Фирма "ИКА" | Method for measuring sulfur content in crude oil |
| US5712891A (en) * | 1995-11-15 | 1998-01-27 | Compagnie Generale Des Matieres Nucleaires | Apparatus for the analysis of a solution by X-ray fluorescence |
| RU2106627C1 (en) * | 1996-07-22 | 1998-03-10 | Андрей Федорович Александров | Device for monitoring parameters of suspended particles |
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2007
- 2007-04-28 WO PCT/RU2007/000220 patent/WO2008007998A1/en not_active Ceased
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU94023383A (en) * | 1994-06-20 | 1996-08-27 | Фирма "ИКА" | Method for measuring sulfur content in crude oil |
| US5712891A (en) * | 1995-11-15 | 1998-01-27 | Compagnie Generale Des Matieres Nucleaires | Apparatus for the analysis of a solution by X-ray fluorescence |
| RU2106627C1 (en) * | 1996-07-22 | 1998-03-10 | Андрей Федорович Александров | Device for monitoring parameters of suspended particles |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011002983A1 (en) | 2009-07-02 | 2011-01-06 | Dow Global Technologies Inc. | Tpo compositions, articles, and methods of making the same |
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