WO2017162925A1 - Method and arrangement for optimization or calibration a particle detector - Google Patents
Method and arrangement for optimization or calibration a particle detector Download PDFInfo
- Publication number
- WO2017162925A1 WO2017162925A1 PCT/FI2017/050207 FI2017050207W WO2017162925A1 WO 2017162925 A1 WO2017162925 A1 WO 2017162925A1 FI 2017050207 W FI2017050207 W FI 2017050207W WO 2017162925 A1 WO2017162925 A1 WO 2017162925A1
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- WO
- WIPO (PCT)
- Prior art keywords
- arrangement
- particle
- carrier gas
- generator
- nanoparticles
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 100
- 238000005457 optimization Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 32
- 239000012159 carrier gas Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910000809 Alumel Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910001006 Constantan Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910000768 nicrosil Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 238000012795 verification Methods 0.000 abstract description 7
- 239000003570 air Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 239000012080 ambient air Substances 0.000 description 4
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- ORQBXQOJMQIAOY-UHFFFAOYSA-N nobelium Chemical compound [No] ORQBXQOJMQIAOY-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 229910001120 nichrome Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- -1 helium (He) Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000002285 radioactive effect Effects 0.000 description 2
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0095—Manufacture or treatments or nanostructures not provided for in groups B82B3/0009 - B82B3/009
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/065—Investigating concentration of particle suspensions using condensation nuclei counters
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0009—Calibration of the apparatus
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N2015/0038—Investigating nanoparticles
Definitions
- the invention relates to a method and arrangement for optimization or calibration particle detectors, such as ion mobility spectrometers, mass spectrometers, particle counters, such as condensation particle counters and other particle detectors. Especially the invention relates to a field deployable neutral and charged nanoparticle and cluster generator arrangement.
- An object of the invention is to alleviate and eliminate the problems relating to the known prior art. Especially the object of the invention is to provide a simple and easy to use as well as reliable arrangement and method for optimization or calibration particle detectors.
- the invention relates to an arrangement device for optimization or calibration particle detectors according to claim 1.
- the invention relates to a method for verification, optimization or calibration particle detectors according to claim 13.
- a particle detector is verified, optimized or calibrated by heating a generator element to or over a certain temperature so to enable emission of the nanoparticles characteristic for the element material and providing said generated nanoparticles to the particle detector to be verified, optimized or calibrated.
- An arrangement for verification, optimization or calibration advantageously comprises advantageously the particle detector, but at least a particle generator chamber, where the generator element is situated.
- the arrangement comprises an inlet for receiving carrier gas into the particle generator chamber and an outlet configured to be coupled with the particle detector.
- the carrier gas is configured to flow so to gather at least portion of the nanoparticles generated in the particle generator chamber and to deliver the carrier gas together with the generated nanoparticles to the particle detector.
- the generator element used for emitting the nanoparticles is e.g. a resistively heated metal wire (hot wire generator), which is heated to or over a certain temperature so to enabling emission of the nanoparticles from the surface of the generator element and thereby the generation or formation of the nanoparticles into the carrier gas flow in the particle generator chamber.
- a resistively heated metal wire hot wire generator
- other type of element can be used, such as a foil to increase a surface area of the element.
- the arrangement and especially the heated metal wire generator according to the invention can be operated with different carrier gases, such as for example with the ambient air, as well as nitrogen (N 2 ) and noble gases like helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe).
- the arrangement can produce sub 50 nm, and in more advantageously even sub 10 nm and down to sub 1 nm neutral, but also electrically charged particles (positive and negative) without an additional electrical charger.
- the particles can be generated by resistively heating a spring of metal wire, which is placed in the carrier gas stream. Vapor emitted from the hot metal surface forms nanoparticles in the surrounding carrier gas stream.
- the produced particle distribution is very stable and the size range of the distribution can be controlled by controlling the heating power of the wire or flow rate of the gas.
- the particles produced by the generator allow the verification and optimization as well as calibration of the current mass spectrometers and particle counters or other particle detectors in the field operation for example, but is applicable practically in any conditions.
- the particle generator can be used in almost any conditions outside laboratory where sub 50 nm neutral or charged nanoparticles are needed.
- the hot wire based generators are advantageously operated in an inert gas, however in field conditions the availability of bottled inert gas (for example N 2 , Ar, or He) can be complicated. When oxygen is present in the carrier gas it will oxidize the metal wire and the generator might stop working within minutes due to breaking of the metal wire. Therefore, selection of a material that can be used with purified ambient air (presence of 0 2 ) is important. Different wire material can be used, such as nickel (Ni) -chrome (Cr) alloy that allows long term operation in field conditions.
- metal alloys which can be heated in oxygen rich atmosphere, like nicrosil, constantan and alumel, as well as silver (Ag), palladium (Pd), titanium (Ti) are also suitable to generate particles when heated up. Also different lengths and diameters, in addition to heating powers, can be used and thereby control the size distribution of the nanoparticles generated.
- the element may also comprise at least two different chemical compositions for generation of different nanoparticles at the same time.
- a resistively heated NiCr (nickel chromium) wire is used, which can produce the particle of exactly known composition in the air.
- NiCr nickel chromium
- the filtered air is enough, which makes the arrangement of the invention very suitable in the field conditions.
- the producing particles of exactly known composition is crucial demand in the mass spectrometer and particle counter calibrations. This is even emphasized in the field conditions, where the surrounding air includes different impurities.
- the hot-wire based generator of the arrangement according to the invention produces so called "self charged" metal oxide ions without an additional charger, the concentration of small ions is decreased when higher currents are used and more heavier ions are produced. It has been found that high concentration of heavier ions acts as a sink to the metal vapors and prevents nucleation that produces the smallest metal oxide clusters.
- the broader range of ions can be obtained by adding an extra x-ray charger between hot-wire generator and mass spectrometer.
- the arrangement setup equipped with an x-ray source can produce metal oxide clusters and ions from 100Th (amu) to several thousand Thomsons. In atmospheric research this is exactly the mass range of interest.
- a corona charger can be added to the arrangement to additionally increase the number of charged particles significantly.
- the present invention offers advantages over the known prior art.
- the arrangement based on the hot element generator such as the hot wire
- the hot element generator is very small and fast to use e.g. when compared to furnaces, for example.
- the particle size distribution range that the wire based generator can generate is controllable, and the generator can also produce particles starting from 1 nm (or even sub 1 nm), which for example the atomizer cannot do that easily.
- the nanoparticle generator according to the invention can produce particle distribution with both neutral but also charged particles and even without an additional charger, which none of the existing generators can do.
- the chemical purity of produced metal ions and clusters is very high even when the carrier gas is filtered ambient air.
- the ability to generate also charged particles solves the problem of transporting radioactive sources.
- the operation of the current mass spectrometers and particle counters cannot be verified nor optimized in the field without a stable particle source that can operate at field conditions, and that source has been lacking.
- the wire based generator arrangement according to the invention can produce a stable size distribution in the wanted size range, and solves thus the problem of instrument optimization and verification at the measurement site.
- particles of exactly known composition can be produced, even in the field conditions and in conditions where the carrier gas is filtered air, which is crucial e.g. in the mass spectrometer and particle counter calibrations. This is achieved e.g.
- the particle composition can be described with a formula (Cr0 3 )x(Cr0 4 )y K z-
- K potassium
- a fraction of the particles obtain electrical charge during the particle formation process, yielding similar formula for negatively charged particles (Cr0 3 )x(Cr0 4 )y K z-
- the exact molecular composition in the air is (Cr03)x- without any unknown amounts of impurities.
- these well-known particles can be used to calibrate e.g. the mass spectrometer mass axis very accurately, or the size dependent detection efficiency of a condensation particle counter (especially if combined to differential mobility analysis technique).
- the particle detector can be optimized and/or calibrated.
- the particle detector may be configured to perform self optimization and/or calibration when the particles of exactly known composition are fed to said detector, for example either by chosen a suitable composition of a library stored into the memory of the particle detector or by inputting said composition of said particles to the particle detector.
- FIGS 1 -2 illustrate principles of exemplary arrangements for verification, optimization or calibration a particle detector according to an advantageous embodiment of the invention.
- FIGS 1 -2 illustrate principles of exemplary arrangements 100 for verification, optimization or calibration a particle detector 1 10 according to an advantageous embodiment of the invention.
- the arrangement comprises a particle generator chamber 101 and a generator element 102 in said chamber 101 to generate nanoparticles.
- the generator element 102 is advantageously a resistively heated metal wire 102 (e.g. NiCr), which is heated to or over a certain temperature thus emitting the nanoparticles from the surface of the generator element.
- the arrangement also comprises an inlet 103 for receiving carrier gas flow 104, such as filtered air, into the particle generator chamber 101 , as well as an outlet 105 to be coupled to the particle detector 1 10.
- the carrier gas flow 104 is configured to bypass the generator element 102 and to deliver the generated nanoparticles via the outlet 105 to the particle detector 1 10.
- the arrangement advantageously also comprises a power feeding means 106 for feeding electrical power to the resistively heated generator element 102 to raise its temperature to or over a certain temperature.
- An outer power source can be electrically connected to the power feeding means 106, or alternative or in addition to the arrangement may also comprise own power source 107.
- the arrangement advantageously comprises a controller 108 for controlling the power fed to the power feeding means.
- the controller 108 advantageously controls a low voltage high current power supply (exemplary operational range e.g. around 10 volts and 10-30 Amps). By controlling the heating power of the generator element a size range and concentration of the generated nanoparticles can be adjusted.
- the arrangement may also comprise a flow generating means 109 for generating the flow rate of the carrier gas flow in or out or through the particle generator chamber.
- the flow generating means 109 may be a controllable flow generating means 109 and it can be arranged in the connection with inlet or outlet or both.
- the arrangement may also comprise filtering system, for example in connection with the flow generating means 109, to filtering e.g. unwanted particles from the ambient air when the air is used as the carrier gas.
- the arrangement may also comprise a cooling section 1 1 1 arranged after the outlet 105 in the direction of flow 104 in order to cooling down the carrier gas flow before entering into the particle detector 1 10.
- the arrangement may additionally comprise also an x-ray charger 1 13 arranged after the outlet 105 in the direction of flow in order to provide additional charged particles into the flow.
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- General Health & Medical Sciences (AREA)
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Abstract
An arrangement (100) for verification, optimization or calibration a particle detector (110) comprises a particle generator chamber (101) with an element (102) for generating nanoparticles. The arrangement comprises also an inlet (103) for receiving carrier gas and an outlet (104) for delivering said carrier gas together with the generated nanoparticles outside from the particle generator chamber (101) and again to the particle detector (110). The element (102) is advantageously a resistively heated metal wire, which is heated to or over a certain temperature so to enabling emission of the nanoparticles characteristic for the element material.
Description
METHOD AND ARRANGEMENT FOR OPTIMIZATION OR CALIBRATION A PARTICLE DETECTOR
TECHNICAL FIELD OF THE INVENTION The invention relates to a method and arrangement for optimization or calibration particle detectors, such as ion mobility spectrometers, mass spectrometers, particle counters, such as condensation particle counters and other particle detectors. Especially the invention relates to a field deployable neutral and charged nanoparticle and cluster generator arrangement.
BACKGROUND OF THE INVENTION
Utilization e.g. of mass spectrometers and condensation particle counters in atmospheric research has been increasing recently. Very often the particle counters and mass spectrometers are part of instrument setups, which are operated in field conditions without a direct support from the best possible laboratory instrumentation. The data obtained by the mass spectrometers is strongly dependent on the inlet line settings. The settings affect two parameters: the penetration of charged particles through the inlet line, and fragmentation of charged particles in the inlet line. The operation of current state-of-the-art particle counters is dependent on the sample air properties, such as absolute humidity and temperature, which are varying from day to day and from measurement site to site.
Therefore there is a need to verify, optimize or calibrate the operation of the particle detectors even daily due to changing operation or environmental conditions. However a simple and easy to use, as well as reliable particle generator to verify, optimize or calibrate the operation of the described instruments has been lacking. This is the case especially in field conditions and out of a clean laboratory environment. Additionally, generation of charged sub 50 nm and especially sub 10 nm particles typically requires an additional particle charger, often a radioactive source, of which transportation is usually strictly regulated and makes thus the use of them troublesome and also expensive.
SUMMARY OF THE INVENTION
An object of the invention is to alleviate and eliminate the problems relating to the known prior art. Especially the object of the invention is to provide a simple and easy to use as well as reliable arrangement and method for optimization or calibration particle detectors.
The object of the invention can be achieved by the features of independent claims.
The invention relates to an arrangement device for optimization or calibration particle detectors according to claim 1. In addition the invention relates to a method for verification, optimization or calibration particle detectors according to claim 13.
According to an embodiment of the invention a particle detector is verified, optimized or calibrated by heating a generator element to or over a certain temperature so to enable emission of the nanoparticles characteristic for the element material and providing said generated nanoparticles to the particle detector to be verified, optimized or calibrated. An arrangement for verification, optimization or calibration advantageously comprises advantageously the particle detector, but at least a particle generator chamber, where the generator element is situated. In addition the arrangement comprises an inlet for receiving carrier gas into the particle generator chamber and an outlet configured to be coupled with the particle detector. The carrier gas is configured to flow so to gather at least portion of the nanoparticles generated in the particle generator chamber and to deliver the carrier gas together with the generated nanoparticles to the particle detector.
The generator element used for emitting the nanoparticles is e.g. a resistively heated metal wire (hot wire generator), which is heated to or over a certain temperature so to enabling emission of the nanoparticles from the surface of the generator element and thereby the generation or formation of the nanoparticles into the carrier gas flow in the particle generator chamber. Also other type of element can be used, such as a foil to increase a surface area of the element.
The arrangement and especially the heated metal wire generator according to the invention can be operated with different carrier gases, such as for example with the ambient air, as well as nitrogen (N2) and noble gases like helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe). The arrangement can produce sub 50 nm, and in more advantageously even sub 10 nm and down to sub 1 nm neutral, but also electrically charged particles (positive and negative) without an additional electrical charger. As an example the particles can be generated by resistively heating a spring of metal wire, which is placed in the carrier gas stream. Vapor emitted from the hot metal surface forms nanoparticles in the surrounding carrier gas stream. The produced particle distribution is very stable and the size range of the distribution can be controlled by controlling the heating power of the wire or flow rate of the gas. The particles produced by the generator allow the verification and optimization as well as calibration of the current mass spectrometers and particle counters or other particle detectors in the field operation for example, but is applicable practically in any conditions. The particle generator can be used in almost any conditions outside laboratory where sub 50 nm neutral or charged nanoparticles are needed.
The hot wire based generators are advantageously operated in an inert gas, however in field conditions the availability of bottled inert gas (for example N2, Ar, or He) can be complicated. When oxygen is present in the carrier gas it will oxidize the metal wire and the generator might stop working within minutes due to breaking of the metal wire. Therefore, selection of a material that can be used with purified ambient air (presence of 02) is important. Different wire material can be used, such as nickel (Ni) -chrome (Cr) alloy that allows long term operation in field conditions. Other metal alloys, which can be heated in oxygen rich atmosphere, like nicrosil, constantan and alumel, as well as silver (Ag), palladium (Pd), titanium (Ti) are also suitable to generate particles when heated up. Also different lengths and diameters, in addition to heating powers, can be used and thereby control the size distribution of the nanoparticles generated. In addition it is to be noted that the element may also comprise at least two different chemical compositions for generation of different nanoparticles at the same time.
According to an embodiment a resistively heated NiCr (nickel chromium) wire is used, which can produce the particle of exactly known composition in the air. Thus no bottled inert gas is even needed but the filtered air is
enough, which makes the arrangement of the invention very suitable in the field conditions. The producing particles of exactly known composition is crucial demand in the mass spectrometer and particle counter calibrations. This is even emphasized in the field conditions, where the surrounding air includes different impurities.
Even though the hot-wire based generator of the arrangement according to the invention produces so called "self charged" metal oxide ions without an additional charger, the concentration of small ions is decreased when higher currents are used and more heavier ions are produced. It has been found that high concentration of heavier ions acts as a sink to the metal vapors and prevents nucleation that produces the smallest metal oxide clusters. According to an additional embodiment of the invention, if one desires to see simultaneously the smallest metal ions and heavier ions, the broader range of ions can be obtained by adding an extra x-ray charger between hot-wire generator and mass spectrometer. According to an example, the arrangement setup equipped with an x-ray source can produce metal oxide clusters and ions from 100Th (amu) to several thousand Thomsons. In atmospheric research this is exactly the mass range of interest. In addition, according to an example also a corona charger can be added to the arrangement to additionally increase the number of charged particles significantly.
The present invention offers advantages over the known prior art. At first the arrangement based on the hot element generator, such as the hot wire, is very small and fast to use e.g. when compared to furnaces, for example. The particle size distribution range that the wire based generator can generate is controllable, and the generator can also produce particles starting from 1 nm (or even sub 1 nm), which for example the atomizer cannot do that easily. The nanoparticle generator according to the invention can produce particle distribution with both neutral but also charged particles and even without an additional charger, which none of the existing generators can do. In addition the chemical purity of produced metal ions and clusters is very high even when the carrier gas is filtered ambient air.
The ability to generate also charged particles solves the problem of transporting radioactive sources. The operation of the current mass spectrometers and particle counters cannot be verified nor optimized in the field without a stable particle source that can operate at field conditions, and
that source has been lacking. The wire based generator arrangement according to the invention can produce a stable size distribution in the wanted size range, and solves thus the problem of instrument optimization and verification at the measurement site. In particularly it is to be noted that according to the invention particles of exactly known composition can be produced, even in the field conditions and in conditions where the carrier gas is filtered air, which is crucial e.g. in the mass spectrometer and particle counter calibrations. This is achieved e.g. by using a NiCr wire, where the particle composition can be described with a formula (Cr03)x(Cr04)yKz- There might be a little amount of potassium (K) as impurity, and most of the particles are electrically neutral, and also there is a small possibility that there is one more oxygen atom. A fraction of the particles obtain electrical charge during the particle formation process, yielding similar formula for negatively charged particles (Cr03)x(Cr04)yKz- However, according to an embodiment the exact molecular composition in the air is (Cr03)x- without any unknown amounts of impurities. According to the invention these well-known particles can be used to calibrate e.g. the mass spectrometer mass axis very accurately, or the size dependent detection efficiency of a condensation particle counter (especially if combined to differential mobility analysis technique).
When the exact composition of the produced particles is known, the particle detector can be optimized and/or calibrated. According to an example the particle detector may be configured to perform self optimization and/or calibration when the particles of exactly known composition are fed to said detector, for example either by chosen a suitable composition of a library stored into the memory of the particle detector or by inputting said composition of said particles to the particle detector.
The exemplary embodiments presented in this text are not to be interpreted to pose limitations to the applicability of the appended claims. The verb "to comprise" is used in this text as an open limitation that does not exclude the existence of also unrecited features. The features recited in depending claims are mutually freely combinable unless otherwise explicitly stated.
The novel features which are considered as characteristic of the invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together
with additional objects and advantages thereof, will be best understood from the following description of specific example embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
Next the invention will be described in greater detail with reference to exemplary embodiments in accordance with the accompanying drawings, in which:
Figures 1 -2 illustrate principles of exemplary arrangements for verification, optimization or calibration a particle detector according to an advantageous embodiment of the invention.
DETAILED DESCRIPTION
Figures 1 -2 illustrate principles of exemplary arrangements 100 for verification, optimization or calibration a particle detector 1 10 according to an advantageous embodiment of the invention. The arrangement comprises a particle generator chamber 101 and a generator element 102 in said chamber 101 to generate nanoparticles. The generator element 102 is advantageously a resistively heated metal wire 102 (e.g. NiCr), which is heated to or over a certain temperature thus emitting the nanoparticles from the surface of the generator element. The arrangement also comprises an inlet 103 for receiving carrier gas flow 104, such as filtered air, into the particle generator chamber 101 , as well as an outlet 105 to be coupled to the particle detector 1 10. The carrier gas flow 104 is configured to bypass the generator element 102 and to deliver the generated nanoparticles via the outlet 105 to the particle detector 1 10.
The arrangement advantageously also comprises a power feeding means 106 for feeding electrical power to the resistively heated generator element 102 to raise its temperature to or over a certain temperature. An outer power source can be electrically connected to the power feeding means 106, or alternative or in addition to the arrangement may also comprise own power source 107. In addition the arrangement advantageously comprises a
controller 108 for controlling the power fed to the power feeding means. The controller 108 advantageously controls a low voltage high current power supply (exemplary operational range e.g. around 10 volts and 10-30 Amps). By controlling the heating power of the generator element a size range and concentration of the generated nanoparticles can be adjusted.
In addition the arrangement may also comprise a flow generating means 109 for generating the flow rate of the carrier gas flow in or out or through the particle generator chamber. The flow generating means 109 may be a controllable flow generating means 109 and it can be arranged in the connection with inlet or outlet or both. The arrangement may also comprise filtering system, for example in connection with the flow generating means 109, to filtering e.g. unwanted particles from the ambient air when the air is used as the carrier gas.
The arrangement may also comprise a cooling section 1 1 1 arranged after the outlet 105 in the direction of flow 104 in order to cooling down the carrier gas flow before entering into the particle detector 1 10.
In addition, according to an embodiment the arrangement may additionally comprise also an x-ray charger 1 13 arranged after the outlet 105 in the direction of flow in order to provide additional charged particles into the flow. The invention has been explained above with reference to the aforementioned embodiments, and several advantages of the invention have been demonstrated. It is clear that the invention is not only restricted to these embodiments, but comprises all possible embodiments within the spirit and scope of the inventive thought and the following patent claims. In addition it is to be noted that the features recited in dependent claims are mutually freely combinable unless otherwise explicitly stated.
Claims
1. An arrangement for optimization or calibration a particle detector, wherein the arrangement comprises:
- the particle detector to be optimized or calibrated,
- a particle generator chamber for generating nanoparticles,
- an inlet for receiving carrier gas into the particle generator chamber, said carrier gas configured to flow so to gather at least portion of the nanoparticles generated in the particle generator chamber,
- an outlet coupled with the particle detector to be optimized or calibrated and to deliver said carrier gas together with the generated nanoparticles gathered by said carrier gas to the particle detector, wherein the arrangement additionally comprises
- a generator element to be heated to or over a certain temperature so to enabling emission of the nanoparticles characteristic for generator element and the generation of said nanoparticles into the carrier gas flow in the particle generator chamber, wherein said generator element is configured to be heated by feeding electric current through said generator element and thereby heating said generator element resistively.
2. The arrangement of claim 1 , wherein the generator element is a resistively heated element, and wherein said arrangement comprises a power feeding means for feeding electrical power to the resistively heated element to raise its temperature over the predetermined temperature or to a certain temperature.
3. The arrangement of claim 2, wherein the power feeding means is a controllable power feeding means for controlling the heating power of the element and thereby controlling a size range of the generated nanoparticles.
4. The arrangement of any of previous claims, wherein the arrangement comprises a controllable flow generating means for controlling the flow rate of the carrier gas flow in or out or through the particle generator chamber, and thereby controlling a size range of the generated nanoparticles.
5. The arrangement of any of previous claims, wherein the heat of the element, flow rate of the carrier gas flow in or out or through the particle generator chamber and/or the material and size of the element is selectable
or controllable so to enable size distribution of the generated nanoparticles be less than 50 nm, advantageously less than 10 nm and down to 1 nm.
6. The arrangement of any of previous claims, wherein the generator element comprises nickel (Ni), chrome (Cr), silver (Ag), palladium (Pd), molybdenum (Mo), titanium (Ti), nickelchromium alloy, nicrosil alloy, constantan alloy and alumel alloy or the composition of those.
7. The arrangement of any of previous claims, wherein the generator element comprises at least two different chemical compositions for generation of different nanoparticles.
8. The arrangement of any of previous claims, wherein the arrangement comprises a cooling section arranged after the outlet in the direction of flow in order to cooling down the carrier gas flow before entering into the particle detector.
9. The arrangement of any of previous claims, wherein the generator element and/or the carrier gas is/are chosen so to generate neutral or electrically charged particles in the particle generator chamber without an additional electrical charger.
10. The arrangement of any of previous claims, wherein the arrangement additionally comprises an x-ray charger arranged after the outlet in the direction of flow in order to provide additional charged particles into the flow.
1 1. The arrangement of any of previous claims, wherein the particle detector is a mass spectrometer, ion mobility spectrometer, particle counter or a condensation particle counter.
12. The arrangement of any of previous claims, wherein the arrangement is a field deployable arrangement.
13. A method for optimization and/or calibration a particle detector, wherein the method comprises steps of:
- heating a generator element to a certain temperature so to enable emission of the nanoparticles characteristic for the generator element and thereby generating nanoparticles in a particle generator chamber, wherein said generator element is heated by feeding electric current
through said generator element and thereby heating said generator element resistively,
- receiving carrier gas into the particle generator chamber, and providing said carrier gas to flow so to gather at least portion of the generated particles, and
- delivering said carrier gas together with the generated particles gathered by said carrier gas to the particle detector, and
- optimizing and/or calibrating said particle detector by said produced nanoparticles characteristic for the generator element.
14. The method of claim 13, wherein carrier gas comprises: helium (He), neon (Ne), argon (Ar), krypton (Kr), xenon (Xe), nitrogen (N2) or Air or filtered air.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FI20165251A FI20165251A (en) | 2016-03-24 | 2016-03-24 | Process and arrangement for verification, optimization or calibration of a particle detector |
FI20165251 | 2016-03-24 |
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WO2017162925A1 true WO2017162925A1 (en) | 2017-09-28 |
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PCT/FI2017/050207 WO2017162925A1 (en) | 2016-03-24 | 2017-03-24 | Method and arrangement for optimization or calibration a particle detector |
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WO (1) | WO2017162925A1 (en) |
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CN114755290A (en) * | 2022-03-31 | 2022-07-15 | 瑞莱谱(杭州)医疗科技有限公司 | Method and system for automatically tuning an inductively coupled plasma mass spectrometer |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001033377A (en) * | 1999-07-01 | 2001-02-09 | L'air Liquide | Device and method for counting condensation nucleus for electronic specialty gas |
EP1757359A1 (en) * | 2005-08-23 | 2007-02-28 | Samsung Electronics Co., Ltd. | Nano particle generator |
-
2016
- 2016-03-24 FI FI20165251A patent/FI20165251A/en not_active Application Discontinuation
-
2017
- 2017-03-24 WO PCT/FI2017/050207 patent/WO2017162925A1/en active Application Filing
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001033377A (en) * | 1999-07-01 | 2001-02-09 | L'air Liquide | Device and method for counting condensation nucleus for electronic specialty gas |
EP1757359A1 (en) * | 2005-08-23 | 2007-02-28 | Samsung Electronics Co., Ltd. | Nano particle generator |
Non-Patent Citations (3)
Title |
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BOIES, A. M. ET AL.: "Hot-wire synthesis of gold nanoparticles", AEROSOL SCIENCE AND TECHNOLOGY, vol. 45, May 2011 (2011-05-01), pages 654 - 663, XP055426281, Retrieved from the Internet <URL:http://www.tandfonline.com/doi/abs/10.1080/02786826.2010.551145> [retrieved on 20170626] * |
JIANG, J. ET AL.: "Model for nanoparticle charging by diffusion, direct photoionization, and thermionization mechanisms", JOURNAL OF ELECTROSTATICS, vol. 65, no. 4, April 2007 (2007-04-01), AMSTERDAM, NL, pages 209 - 220, XP005736511, [retrieved on 20170627] * |
PEINEKE, C. ET AL.: "Using a glowing wire generator for production of charged, uniformly sized nanoparticles at high concentrations", JOURNAL OF AEROSOL SCIENCE, vol. 37, no. 12, December 2006 (2006-12-01), AMSTERDAM, NL, pages 1651 - 1661, XP028071001, [retrieved on 20170622] * |
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