WO2014070043A1 - Method for cleaning photoionization detectors and device for the implementation thereof - Google Patents
Method for cleaning photoionization detectors and device for the implementation thereof Download PDFInfo
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- WO2014070043A1 WO2014070043A1 PCT/RU2013/000947 RU2013000947W WO2014070043A1 WO 2014070043 A1 WO2014070043 A1 WO 2014070043A1 RU 2013000947 W RU2013000947 W RU 2013000947W WO 2014070043 A1 WO2014070043 A1 WO 2014070043A1
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- Prior art keywords
- pid
- substance
- cleaning
- aqueous solution
- detector
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000203 mixture Substances 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 25
- 229920000642 polymer Polymers 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 14
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- 239000000017 hydrogel Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000000356 contaminant Substances 0.000 claims description 7
- 238000011109 contamination Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000230 xanthan gum Substances 0.000 claims description 4
- 229920001285 xanthan gum Polymers 0.000 claims description 4
- 235000010493 xanthan gum Nutrition 0.000 claims description 4
- 229940082509 xanthan gum Drugs 0.000 claims description 4
- 229920002313 fluoropolymer Polymers 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000000499 gel Substances 0.000 abstract 2
- 238000001824 photoionisation detection Methods 0.000 abstract 1
- 239000000411 inducer Substances 0.000 description 6
- 239000000428 dust Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
- G01N27/66—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber and measuring current or voltage
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
- G01N2021/151—Gas blown
Definitions
- the invention relates to the field of analytical instrumentation and, in particular, to methods and means of increasing the reliability of gas analytical equipment, including gas analyzers with a photoionization detector (PID).
- PID photoionization detector
- the PID is contaminated, including the windows of a photoionization lamp, electrodes, and other elements of the ionization chamber. This causes both a decrease in PID sensitivity and an increase in noise and drift. It is also known that to eliminate these shortcomings, manufacturers of analytical equipment recommend periodic cleaning of the detector by disassembling it and washing the detector parts in a solvent, as well as by wiping the lamp window with substances that remove impurities, such as acetone or hydrofluoric acid. The disadvantage of this method is the need for disassembly and assembly of the PID, which, when performed regularly, complicates the maintenance procedure, as well as the need to work with harmful hydrofluoric acid, which requires special safety measures.
- the disadvantage of this method is the inability to remove using ozone contaminants containing silicon dioxide, the deposition of which on the surface of the window causes a strong absorption of ionizing radiation emitted by the lamp.
- a known gas-vapor mixture generator in which a polymer hydrogel powder is used - a polymer three-dimensional cross-linked system based on polymers containing an aqueous solution of a substance, for example, ammonia (see utility model patent RU 77440 U1, IPC G01 7 / 14,2008) .
- the known composition used in this generator cannot be used to clean the internal volume of the PID from contamination, and, in particular, to clean the window of the PID lamp from silica deposited on the window in the form of dust and which is the main reason for the decrease in the sensitivity of the PID, and also increasing its noise and drift.
- the objective of the invention was to develop such a method of cleaning the detector, which would carry out cleaning of the detector elements, including silicon dioxide, but would not require disassembly and subsequent assembly of the detector, as well as the development of a composition for a steam-air generator that would produce cleaning the internal volume of the PID, including the window of the lamp from silicon dioxide.
- the proposed device for cleaning the PID from contamination containing a container with hydrofluoric acid, placed in a mixer with fittings for supplying and discharging a gas in which, according to the invention, a container with hydrofluoric acid is made of a polymer material permeable to hydrogen fluoride.
- the hydrofluoric acid container is made of fluoroplastic.
- compositions for a gas-vapor mixture generator containing a gel-forming polymer powder and an aqueous solution of a substance, in which, according to the invention, a compound is used as a substance, the vapors of which clean the internal volume of the PID from contamination, including the window of a photoionization lamp from pollution, including silicon dioxide ..
- an aqueous solution of hydrofluoric acid is used as the aqueous solution of the substance, the vapors of which clean the silicon dioxide window of the PID lamp.
- composition for the generator is a polymer capable of forming a hydrogel at a pH of 1 to 6 is used as a gelling polymer.
- a polymer capable of forming a hydrogel at a pH of 1 to 6 is used as a gelling polymer.
- xanthan gum or hydroxyethyl cellulose are used as the gelling polymer.
- Figure 1 is a schematic diagram of a device for cleaning PID
- Fig. 2 is a schematic diagram of a connection of a gas-vapor mixture generator.
- the device contains a container 1 (see Fig. 1) of a polymeric material permeable to hydrogen fluoride vapors, for example, fluoroplastic, partially filled with hydrofluoric acid 2 and placed in a mixer 3 with fittings 4 and 5 for supplying and discharging gas.
- the fitting 4 is connected to the filter 6 to absorb dust and moisture.
- the nozzle 5 for outputting gas from the mixer 3 is connected to the input 7 of the ionization chamber 8, which is connected to the photoionization lamp 9, the window 10 of which is facing the ionization chamber 8.
- the ionization chamber 8 is equipped with electrodes 11 and 12 connected to a power source and an electrometer (in Fig.
- a flow inducer installed in the gas analyzer can be used as a flow inducer.
- a flow inducer can also be installed at the inlet of the device.
- the device operates as follows.
- a container 1 partially filled with hydrofluoric acid 2 and placed in a mixer 3, equipped with nozzles with fittings 4 and 5 for supplying and discharging gas, is connected to the inlet 7 of the ionization chamber 8.
- a flow inducer 15 is turned on and air preliminarily purified from dust and foreign substances by means of a filter 6 enters the mixer 3, where it is saturated with hydrogen fluoride.
- this stream enters the ionization chamber 8, cleaning its elements and, including the window 10 of the lamp 9 from impurities and, in particular, from S1O2.
- the flow inducer is installed at the inlet of the device, it produces air injection. The rest of the device works similarly.
- the mixer 3, containing the container 1, is disconnected, and the filter 6 is connected directly to the input 7 of the ionization chamber 8, after which the flow rate driver 15 is still working.
- the internal volume of the ionization chamber 8 is purified from HF vapors and products of its interaction with pollutants.
- the preparation of the composition for generating a gas-vapor mixture that purifies the internal volume of the photoionization detector is carried out as follows: the initial substance, a gel-forming polymer in the form of dry powder or granules, is placed in a container, an aqueous solution of the substance is added, the vapors of which purify the internal volume of the PID from contamination. Then the mixture is stirred and left for 5-10 hours. During this time, the granules swell to form a hydrogel, partially filling the internal volume of the container.
- xanthan gum is used as a gelling polymer, as a substance, the vapors of which clean the internal volume of the PID, including the window of a photoionization lamp from silicon dioxide - a 20% aqueous solution of hydrofluoric acid.
- the ratio of the mass of xanthan gum to the mass of a 20% aqueous solution of hydrogen fluoride is 1: 60.
- the container must be made of a material resistant to hydrofluoric acid, such as polyethylene.
- composition for generating a gas-vapor mixture is performed using a gas-vapor mixture generator, schematically shown in Fig. 2.
- the generator contains a tank 1 with the proposed composition 2, a mixer 3 mounted above the tank 1, pipe 4 for supply b
- a filter absorber 6 and a compressor 19 are sequentially installed in the gas channel 18 for supplying gas to the pipe 4 of the mixer 3.
- the generation of the mixture is as follows.
- the air stream created by the compressor 19 and cleaned by the filter 6 from dust, moisture and contaminants is supplied to the mixer 3 mounted on the tank 1, where it is saturated with hydrogen fluoride vapors emitted by the proposed composition.
- a mixture of air and hydrogen fluoride vapors is introduced through the nozzle 5 to the input 7 of the ionization chamber 8 and purifies the internal volume of the latter, including the lamp window, electrodes, is removed from it and enters the absorber 14, where it is absorbed by a sorbent that prevents the release of harmful substances into the air .
- the service life (shelf life) of the developed composition depends on the amount of hydrofluoric acid absorbed by the hydrogel and the flow rate of the mixture.
- composition for generating a gas-vapor mixture Due to the above-mentioned features of the composition for generating a gas-vapor mixture, a technical result is achieved, which consists in cleaning the internal volume of the PID ionization chamber, including the window of the PID lamp from silicon dioxide without disassembling the detector with full restoration of the PID technical characteristics. This ensures the safe operation of personnel and does not release harmful substances.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Toxicology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to methods for cleaning photoionization detectors (PID) to remove dirt and to a device for implementing said method. The technical result of the invention consists in that the window of a PID lamp is cleaned to remove silicon dioxide without the detector being dismantled with the technical characteristics of the detector being restored in full. What is proposed is: a method for cleaning PIDs to remove dirt, wherein a gaseous substance which removes dirt from the surface of PID elements is passed through the internal volume of the detector, in which, in accordance with the invention, this gaseous substance used is hydrogen fluoride. Also proposed is: a device for implementing the method, said device comprising a vessel (1) with hydrofluoric acid (2), said vessel being arranged in a mixer (3) with nozzles (4) and (5) for the supply and discharge of a gas, in which, in accordance with the invention, the vessel (1) containing hydrofluoric acid (2) is formed from a polymeric material which is permeable to hydrogen fluoride vapours. What is proposed is: a composition for producing a vapour-and-gas mix which cleans the internal volume (PID), said composition comprising a powder of a gel forming polymer and an aqueous solution of a substance, in which the aqueous solution of the substance used is a substance with vapours which clean the window of the VUV lamp and the internal volume of the PID to remove dirt. An aqueous solution of hydrogen fluoride can be used as the aqueous solution of the substance. A polymer which is capable of forming a hydrogel at a pH of from 1 to 6 can be used as the gel forming polymer.
Description
СПОСОБ ОЧИСТКИ ФОТОИОНИЗАЦИОННЫХ ДЕТЕКТОРОВ И METHOD FOR CLEANING PHOTOIONIZATION DETECTORS AND
УСТРОЙСТВО ДЛЯ ЕГО ОСУЩЕСТВЛЕНИЯ DEVICE FOR ITS IMPLEMENTATION
Область техники Technical field
Изобретение относится к области аналитического приборостроения и, в частности, к методам и средствам повышения надежности газоаналитической аппаратуры, в том числе газоанализаторов с фотоионизационным детектором (ФИД). The invention relates to the field of analytical instrumentation and, in particular, to methods and means of increasing the reliability of gas analytical equipment, including gas analyzers with a photoionization detector (PID).
Предшествующий уровень техники State of the art
Общеизвестно, что в процессе работы происходит загрязнение ФИД, в том числе окна фотоионизационной лампы, электродов, других элементов ионизационной камеры. Это вызывает как падение чувствительности ФИД, так и увеличение шума и дрейфа. Известно также, что для устранения этих недостатков производители аналитического оборудования рекомендуют производить периодическую очистку детектора путем его разборки и промывки деталей детектора в растворителе, а также с помощью протирки окна лампы веществами, удаляющими загрязнения, например ацетоном или фтористоводородной кислотой. Недостатком этого способа является необходимость разборки и сборки ФИД, что при регулярном выполнении усложняет процедуру обслуживания, а также необходимость работы с вредной для здоровья фтористоводородной кислотой, требующей выполнения специальных мер безопасности. It is well known that in the process of operation, the PID is contaminated, including the windows of a photoionization lamp, electrodes, and other elements of the ionization chamber. This causes both a decrease in PID sensitivity and an increase in noise and drift. It is also known that to eliminate these shortcomings, manufacturers of analytical equipment recommend periodic cleaning of the detector by disassembling it and washing the detector parts in a solvent, as well as by wiping the lamp window with substances that remove impurities, such as acetone or hydrofluoric acid. The disadvantage of this method is the need for disassembly and assembly of the PID, which, when performed regularly, complicates the maintenance procedure, as well as the need to work with harmful hydrofluoric acid, which requires special safety measures.
Известен также способ очистки элементов ФИД от загрязнения, согласно которому детектор не разбирается, а в качестве средства очистки используется газообразный озон, генерируемый фотоионизационной лампой в процессе работы (см., например, патент US6734435). There is also a method of cleaning PID elements from contamination, according to which the detector cannot be disassembled, and gaseous ozone generated by a photoionization lamp during operation is used as a cleaning agent (see, for example, US6734435).
Недостатком известного способа является невозможность удаления с помощью озона загрязнений, содержащих диоксид кремния,
осаждение которых на поверхности окна вызывает сильное поглощение ионизирующего излучения, испускаемого лампой. The disadvantage of this method is the inability to remove using ozone contaminants containing silicon dioxide, the deposition of which on the surface of the window causes a strong absorption of ionizing radiation emitted by the lamp.
Следует отметить, что если речь идет о химических загрязнениях, то можно использовать не жидкость, а ее пары, применяя для этого, например, генераторы газопаровых смесей. It should be noted that when it comes to chemical pollution, it is possible to use not liquid, but its vapors, using, for example, gas-vapor mixture generators.
Известен генератор парогазовой смеси, в составе которого использован порошок полимерного гидрогеля - полимерной трехмерной сшитой системы на основе полимеров, содержащей водный раствор вещества, например, аммиака (см. патент на полезную модель RU 77440 U1 , МПК G01 7/14,2008 г.). A known gas-vapor mixture generator, in which a polymer hydrogel powder is used - a polymer three-dimensional cross-linked system based on polymers containing an aqueous solution of a substance, for example, ammonia (see utility model patent RU 77440 U1, IPC G01 7 / 14,2008) .
Однако известный состав, используемый в этом генераторе, не может быть применен для очистки внутреннего объема ФИД от загрязнений, и, в частности, для очистки окна лампы ФИД от диоксида кремния, оседающего на окне в виде пыли и являющегося основной причиной снижения чувствительности ФИД, а также увеличения его шума и дрейфа. However, the known composition used in this generator cannot be used to clean the internal volume of the PID from contamination, and, in particular, to clean the window of the PID lamp from silica deposited on the window in the form of dust and which is the main reason for the decrease in the sensitivity of the PID, and also increasing its noise and drift.
Раскрытие изобретения Disclosure of invention
Задача изобретения состояла в разработке такого способа очистки детектора, который бы при своем осуществлении производил бы очистку элементов детектора, в том числе от диоксида кремния, но не требовал бы разборки и последующей сборки детектора, а также разработке состава для генератора паровоздушной смеси, который бы производил очистку внутреннего объема ФИД, в том числе окна лампы от диоксида кремния. The objective of the invention was to develop such a method of cleaning the detector, which would carry out cleaning of the detector elements, including silicon dioxide, but would not require disassembly and subsequent assembly of the detector, as well as the development of a composition for a steam-air generator that would produce cleaning the internal volume of the PID, including the window of the lamp from silicon dioxide.
Указанная задача решается тем, что предложен способ очистки ФИД от загрязнений, при котором через внутренний объем детектора пропускают газообразное вещество, удаляющее загрязнения с поверхностей элементов детектора, в котором, согласно изобретению в качестве такого вещества используют фтористый водород. This problem is solved by the fact that a method is proposed for cleaning the PID from contaminants, in which a gaseous substance is passed through the internal volume of the detector, which removes contaminants from the surfaces of the detector elements, in which, according to the invention, hydrogen fluoride is used as such a substance.
Задача решается также тем, что предложено устройство для очистки ФИД от загрязнений, содержащее емкость с фтористоводородной кислотой, помещенную в смеситель со штуцерами
для подвода и вывода газа, в котором согласно изобретению емкость с фтористоводородной кислотой выполнена из полимерного материала, проницаемого для фтористого водорода. The problem is also solved by the fact that the proposed device for cleaning the PID from contamination, containing a container with hydrofluoric acid, placed in a mixer with fittings for supplying and discharging a gas in which, according to the invention, a container with hydrofluoric acid is made of a polymer material permeable to hydrogen fluoride.
В предпочтительном варианте осуществления устройства емкость с фтористоводородной кислотой выполнена из фторопласта. In a preferred embodiment of the device, the hydrofluoric acid container is made of fluoroplastic.
Указанная задача решается тем, что предложен состав для генератора газопаровой смеси, содержащий порошок гелеобразующего полимера и водный раствор вещества, в котором, согласно изобретению, в качестве вещества использовано соединение, пары которого очищают внутреннего объема ФИД от загрязнений, и в том числе окно фотоионизационной лампы от загрязнений, в том числе от диоксида кремния.. This problem is solved by the fact that a composition is proposed for a gas-vapor mixture generator containing a gel-forming polymer powder and an aqueous solution of a substance, in which, according to the invention, a compound is used as a substance, the vapors of which clean the internal volume of the PID from contamination, including the window of a photoionization lamp from pollution, including silicon dioxide ..
В преимущественном варианте состава для генератора в качестве водного раствора вещества использован водный раствор фтористоводородной кислоты, пары которой очищают окно лампы ФИД от диоксида кремния. In an advantageous embodiment of the composition for the generator, an aqueous solution of hydrofluoric acid is used as the aqueous solution of the substance, the vapors of which clean the silicon dioxide window of the PID lamp.
Еще одним отличием состава для генератора является то, что в качестве гелеобразующего полимера использован полимер, способный образовать гидрогель при значении рН от 1 до 6. В предпочтительном варианте состава в качестве гелеобразующего полимера использована ксантановая камедь или гидроксиэтилцеллюлоза. Another difference in the composition for the generator is that a polymer capable of forming a hydrogel at a pH of 1 to 6 is used as a gelling polymer. In a preferred embodiment of the composition, xanthan gum or hydroxyethyl cellulose are used as the gelling polymer.
Благодаря отмеченным выше особенностям осуществления способа, устройства и состава для его осуществления достигается технический результат, который состоит в том, что производится очистка окна лампы ФИД от диоксида кремния без разборки детектора, с полным восстановлением технических характеристик детектора. Due to the above-mentioned features of the method, device and composition for its implementation, a technical result is achieved, which consists in cleaning the window of the PID lamp from silicon dioxide without disassembling the detector, with full restoration of the technical characteristics of the detector.
Описание фигур чертежей Description of the figures of the drawings
Сущность изобретения поясняется чертежами, на которых представлены принципиальные схемы устройства для очистки ФИД, подключенного к ионизационной камере ФИД. The invention is illustrated by drawings, which shows a schematic diagram of a device for cleaning PID connected to the ionization chamber of the PID.
На Рис.1 - принципиальная схема устройства для очистки ФИД;
Рис. 2 - принципиальная схема подключения генератора газопаровой смеси. Figure 1 is a schematic diagram of a device for cleaning PID; Fig. 2 is a schematic diagram of a connection of a gas-vapor mixture generator.
Лучшие варианты осуществления изобретения The best embodiments of the invention
Устройство содержит емкость 1 (см. рис.1) из полимерного материала, проницаемого для паров фтористого водорода, например, из фторопласта, частично заполненную фтористоводородной кислотой 2 и помещенную в смеситель 3 со штуцерами 4 и 5 для подвода и вывода газа. Штуцер 4 соединен с фильтром 6 для поглощения пыли и влаги. Штуцер 5 для вывода газа из смесителя 3 соединен с входом 7 ионизационной камеры 8 , которая соединена с фотоионизационной лампой 9, окно 10 которой обращено в ионизационную камеру 8. Ионизационная камера 8 снабжена электродами 11 и 12, соединенными с источником питания и электрометром (на рис. не показаны), а также штуцером для 13 для выхода газа, соединенным через фильтр 14 для поглощения фтористого водорода с побудителем расхода 15. В качестве побудителя расхода может использоваться побудитель расхода, установленный в газоанализаторе. Побудитель расхода может также устанавливаться на входе в устройство. The device contains a container 1 (see Fig. 1) of a polymeric material permeable to hydrogen fluoride vapors, for example, fluoroplastic, partially filled with hydrofluoric acid 2 and placed in a mixer 3 with fittings 4 and 5 for supplying and discharging gas. The fitting 4 is connected to the filter 6 to absorb dust and moisture. The nozzle 5 for outputting gas from the mixer 3 is connected to the input 7 of the ionization chamber 8, which is connected to the photoionization lamp 9, the window 10 of which is facing the ionization chamber 8. The ionization chamber 8 is equipped with electrodes 11 and 12 connected to a power source and an electrometer (in Fig. (not shown), as well as a nozzle for gas outlet 13 connected through a filter 14 for absorbing hydrogen fluoride with a flow inducer 15. A flow inducer installed in the gas analyzer can be used as a flow inducer. A flow inducer can also be installed at the inlet of the device.
В соответствии с заявленным способом устройство работает следующим образом. In accordance with the claimed method, the device operates as follows.
Для проведения очистки окна 10 и элементов ионизационной камеры 8 от загрязнений к входу 7 ионизационной камеры 8 подключают емкость 1 , частично заполненную фтористоводородной кислотой 2 и помещенную в смеситель 3, снабженный патрубками со штуцерами 4 и 5 для подвода и вывода газа. После этого включают побудитель расхода 15 и воздух, предварительно очищенный от пыли и посторонних веществ с помощью фильтра 6, поступает в смеситель 3, где насыщается фтористым водородом. To clean the window 10 and elements of the ionization chamber 8 from impurities, a container 1, partially filled with hydrofluoric acid 2 and placed in a mixer 3, equipped with nozzles with fittings 4 and 5 for supplying and discharging gas, is connected to the inlet 7 of the ionization chamber 8. After that, a flow inducer 15 is turned on and air preliminarily purified from dust and foreign substances by means of a filter 6 enters the mixer 3, where it is saturated with hydrogen fluoride.
Затем этот поток поступает в ионизационную камеру 8, очищая ее элементы и, в том числе окно 10 лампы 9 от загрязнений и, в частности, от S1O2. Очистка от S1O2 происходит благодаря химической реакции S1O2+4HF = SiF4 +2Н2О. Пары SiF4 и НгО выводятся из ионизационной камеры 8 воздухом. Пары HF и SiF4 поглощаются фильтром 14, что
предотвращает поступление их в окружающую среду и делает процесс очистки безопасным. Then this stream enters the ionization chamber 8, cleaning its elements and, including the window 10 of the lamp 9 from impurities and, in particular, from S1O2. Purification from S1O2 occurs due to the chemical reaction S1O2 + 4HF = SiF 4 + 2H2O. Vapors SiF 4 and HgO are removed from the ionization chamber 8 by air. The HF and SiF 4 pairs are absorbed by the filter 14, which prevents them from entering the environment and makes the cleaning process safe.
Если побудитель расхода устанавливается на входе в устройство, он производит нагнетание воздуха. В остальном устройство работает аналогично. If the flow inducer is installed at the inlet of the device, it produces air injection. The rest of the device works similarly.
После завершения процесса очистки смеситель 3, содержащий емкость 1, отсоединяется, а фильтр 6 подключается непосредственно к входу 7 ионизационной камеры 8, после чего побудитель расхода 15 еще некоторое время работает. За это время внутренний объем ионизационной камеры 8 очищается от паров HF и продуктов его взаимодействия с загрязнителями. After completion of the cleaning process, the mixer 3, containing the container 1, is disconnected, and the filter 6 is connected directly to the input 7 of the ionization chamber 8, after which the flow rate driver 15 is still working. During this time, the internal volume of the ionization chamber 8 is purified from HF vapors and products of its interaction with pollutants.
Приготовление состава для генерирования газопаровой смеси, очищающей внутренний объем фотоионизационного детектора осуществляется следующим образом: исходное вещество гелеобразующий полимер в виде сухого порошка или гранул помещают в емкость, добавляют водный раствор вещества, пары которого очищают внутренней объем ФИД от загрязнений. Затем смесь перемешивают и оставляют на 5-10 часов. За это время происходит набухание гранул с образованием гидрогеля, частично заполняющего внутренний объем емкости. В преимущественном варианте состава в качестве гелеобразующего полимера используют ксантановую камедь, в качестве вещества, пары которого очищают внутренний объем ФИД, в том числе окно фотоионизационной лампы от диоксида кремния - 20% водный раствор фтористоводородной кислоты. В предпочтительном варианте отношение массы ксантановой камеди к массе 20% водного раствора фтористого водорода составляет 1 :60. The preparation of the composition for generating a gas-vapor mixture that purifies the internal volume of the photoionization detector is carried out as follows: the initial substance, a gel-forming polymer in the form of dry powder or granules, is placed in a container, an aqueous solution of the substance is added, the vapors of which purify the internal volume of the PID from contamination. Then the mixture is stirred and left for 5-10 hours. During this time, the granules swell to form a hydrogel, partially filling the internal volume of the container. In an advantageous embodiment of the composition, xanthan gum is used as a gelling polymer, as a substance, the vapors of which clean the internal volume of the PID, including the window of a photoionization lamp from silicon dioxide - a 20% aqueous solution of hydrofluoric acid. In a preferred embodiment, the ratio of the mass of xanthan gum to the mass of a 20% aqueous solution of hydrogen fluoride is 1: 60.
Емкость должна быть выполнена из материала, устойчивого к воздействию фтористоводородной кислоты, например полиэтилена. The container must be made of a material resistant to hydrofluoric acid, such as polyethylene.
Применение состава для генерирования газопаровой смеси производится с помощью генератора газопаровой смеси, схематически представленного на рис. 2. The use of the composition for generating a gas-vapor mixture is performed using a gas-vapor mixture generator, schematically shown in Fig. 2.
Генератор содержит емкость 1 с предложенным составом 2, смеситель 3, установленный над емкостью 1 , патрубок 4 для подвода
б The generator contains a tank 1 with the proposed composition 2, a mixer 3 mounted above the tank 1, pipe 4 for supply b
газа, например, воздуха, и патрубок 5 для вывода газопаровой смеси из смесителя 3. На поверхности гидрогеля находится пластина 16 с отверстиями 17, выполненная из инертного материала, например полиэтилена. Она служит для фиксации состава 2 в емкости 1 при ее использовании и транспортировке. В газовом канале 18 для подвода газа в патрубок 4 смесителя 3 последовательно установлены фильтр- поглотитель 6 и компрессор 19. gas, for example, air, and a pipe 5 for withdrawing the gas-vapor mixture from the mixer 3. On the surface of the hydrogel is a plate 16 with holes 17 made of an inert material, such as polyethylene. It serves to fix the composition 2 in the tank 1 during its use and transportation. In the gas channel 18 for supplying gas to the pipe 4 of the mixer 3, a filter absorber 6 and a compressor 19 are sequentially installed.
Генерация смеси происходит следующим образом. Поток воздуха, создаваемый компрессором 19 и очищенный фильтром 6 от пыли, влаги и загрязнений подается в смеситель 3, установленный на емкости 1 , где насыщается парами фтористого водорода, эмитируемыми предложенным составом. Смесь воздуха и паров фтористого водорода вводится через штуцер 5 на вход 7 ионизационной камеры 8 и производит очистку внутреннего объема последнего, в том числе окна лампы, электродов, выводится из него и поступает в поглотитель 14, где поглощается сорбентом, предотвращающим выброс вредных веществ в воздух. The generation of the mixture is as follows. The air stream created by the compressor 19 and cleaned by the filter 6 from dust, moisture and contaminants is supplied to the mixer 3 mounted on the tank 1, where it is saturated with hydrogen fluoride vapors emitted by the proposed composition. A mixture of air and hydrogen fluoride vapors is introduced through the nozzle 5 to the input 7 of the ionization chamber 8 and purifies the internal volume of the latter, including the lamp window, electrodes, is removed from it and enters the absorber 14, where it is absorbed by a sorbent that prevents the release of harmful substances into the air .
Срок службы (годности) разработанного состава зависит от количества фтористоводородной кислоты, поглощенной гидрогелем, и расхода смеси. The service life (shelf life) of the developed composition depends on the amount of hydrofluoric acid absorbed by the hydrogel and the flow rate of the mixture.
Благодаря отмеченным выше особенностям выполнения состава для генерирования газопаровой смеси обеспечивается достижение технического результата, который состоит в том, что производится очистка внутреннего объема ионизационной камеры ФИД, в том числе окна лампы ФИД от диоксида кремния без разборки детектора с полным восстановлением технических характеристик ФИД. При этом обеспечивается безопасная работа персонала и не происходит выброса вредных веществ. Due to the above-mentioned features of the composition for generating a gas-vapor mixture, a technical result is achieved, which consists in cleaning the internal volume of the PID ionization chamber, including the window of the PID lamp from silicon dioxide without disassembling the detector with full restoration of the PID technical characteristics. This ensures the safe operation of personnel and does not release harmful substances.
При такой очистке полностью восстанавливаются все рабочие характеристики детектора. Важно, что в процессе очистки отсутствует контакт оператора с фтористоводородной кислотой, работа по очистке может производиться без вытяжного шкафа.
With this cleaning, all detector performance is fully restored. It is important that during the cleaning process there is no operator contact with hydrofluoric acid; cleaning work can be done without a fume hood.
Claims
1. Способ очистки фотоионизационных детекторов от загрязнений, при котором через внутренний объем детектора пропускают газообразное вещество, удаляющее загрязнения с поверхностей 1. A method of cleaning photoionization detectors from contaminants, in which a gaseous substance is removed through the internal volume of the detector, which removes contaminants from surfaces
5 элементов фотоионизационного детектора, отличающийся тем, что в качестве газообразного вещества используют пары фтористого водорода. 5 elements of a photoionization detector, characterized in that hydrogen fluoride vapor is used as a gaseous substance.
2. Устройство для очистки фотоионизационных детекторов от загрязнений, содержащее емкость с фтористоводородной кислотой, ю отличающееся тем, что емкость с фтористоводородной кислотой выполнена из проницаемого для паров фтористого водорода полимерного материала и помещена в сосуд, имеющий штуцера для подвода и вывода газа. 2. A device for cleaning photoionization detectors from contaminants, containing a container with hydrofluoric acid, characterized in that the container with hydrofluoric acid is made of a polymer material permeable to hydrogen fluoride and placed in a vessel having a fitting for supplying and discharging gas.
3. Устройство по п.2, отличающееся тем, что емкость с 15 фтористоводородной кислотой выполнена из фторопласта. 3. The device according to claim 2, characterized in that the container with 15 hydrofluoric acid is made of fluoroplastic.
4. Состав для генерирования газопаровой смеси, очищающей внутренний объем фотоионизационного детектора, содержащий порошок гелеобразующего полимера и водный раствор вещества, отличающийся тем, что в качестве вещества, использовано соединение, 4. The composition for generating a gas-vapor mixture, cleaning the internal volume of the photoionization detector, containing a gelling polymer powder and an aqueous solution of a substance, characterized in that the compound used is a substance,
20 пары которого очищают внутренний объем фотоионизационного детектора (ФИД) от загрязнений. 20 pairs of which clean the internal volume of the photoionization detector (PID) from contamination.
5. Состав по п. 4, отличающийся тем, что в качестве водного раствора вещества использован водный раствор фтористоводородной кислоты, пары которого очищают окно лампы ФИД от диоксида кремния. 5. The composition according to p. 4, characterized in that an aqueous solution of hydrofluoric acid is used as the aqueous solution of the substance, the vapor of which cleans the window of the PID lamp from silicon dioxide.
25 6. Состав по п. п. 4 или 5, отличающийся тем, что в качестве гелеобразующего полимера используется полимер, способный образовывать гидрогель при рН от 1 до 6. 25 6. Composition according to claim 4 or 5, characterized in that a polymer capable of forming a hydrogel at a pH of 1 to 6 is used as a gelling polymer.
7. Состав по п. п. 6, отличающийся тем, что в качестве гелеобразующего полимера используется ксантановая камедь или 7. The composition according to p. 6, characterized in that as the gelling polymer is used xanthan gum or
30 гидроксиэтилцеллюлоза
30 hydroxyethyl cellulose
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RU2012146460/05A RU2540388C2 (en) | 2012-11-01 | 2012-11-01 | Device for cleaning of photo-ionisation detectors of fouling |
RU2012146460 | 2012-11-01 | ||
RU2013119865 | 2013-04-30 | ||
RU2013119865/05A RU2530046C1 (en) | 2013-04-30 | 2013-04-30 | Composition for generating gas-vapour mixture |
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RU774478C (en) * | 1979-05-04 | 1993-07-15 | Предприятие П/Я Р-6644 | Method of ionic-chemical etching of silicon dioxide or silicon nitride |
RU2030453C1 (en) * | 1990-07-10 | 1995-03-10 | Ютилов Юрий Михайлович | Composition for cleansing of glass surface and other materials |
US6734435B2 (en) * | 2001-05-29 | 2004-05-11 | Rae Systems, Inc. | Photo-ionization detector and method for continuous operation and real-time self-cleaning |
RU2315287C2 (en) * | 2004-12-09 | 2008-01-20 | ООО Бюро аналитического приборостроения ХРОМДЕТ-ЭКОЛОГИЯ | Method and device for analyzing materials |
RU77440U1 (en) * | 2008-05-26 | 2008-10-20 | Ооо Бюро Аналитического Приборостроения "Хромдет-Экология" | GAS-STEAM MIXTURE GENERATOR |
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RU774478C (en) * | 1979-05-04 | 1993-07-15 | Предприятие П/Я Р-6644 | Method of ionic-chemical etching of silicon dioxide or silicon nitride |
RU2030453C1 (en) * | 1990-07-10 | 1995-03-10 | Ютилов Юрий Михайлович | Composition for cleansing of glass surface and other materials |
US6734435B2 (en) * | 2001-05-29 | 2004-05-11 | Rae Systems, Inc. | Photo-ionization detector and method for continuous operation and real-time self-cleaning |
RU2315287C2 (en) * | 2004-12-09 | 2008-01-20 | ООО Бюро аналитического приборостроения ХРОМДЕТ-ЭКОЛОГИЯ | Method and device for analyzing materials |
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