Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C19/00—Other disintegrating devices or methods
  • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C19/00—Other disintegrating devices or methods
  • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
  • B02C2019/183—Crushing by discharge of high electrical energy

Definitions

• the invention relates to a sample container according to the preamble of claim 1 and an arrangement for
• samples of samples can be used in the analysis of mineral samples.
• the fragmentation of material samples by means of pulsed high-voltage discharges is characterized by a comparatively higher selectivity or selectivity.
• the constituents of a sample can be better separated during the fragmentation or comminution process.
• a particularly selective fragmentation can be achieved if the high voltage breakdown by the Sample-forming solid, along grain boundaries and inhomogeneities in the material of the sample takes place.
• This type of fragmentation is called electrodynamic fragmentation, in which correspondingly high field strengths or voltages are used.
• electro-hydraulic fragmentation the fragmentation or comminution of the samples takes place by means of shock waves, which are generated during high-voltage breakdown in a dielectric fluid surrounding the sample, which is generally water.
• electrodynamic fragmentation requires higher electric field strengths than electrohydraulic fragmentation, but as a rule has better selectivity.
• the accuracy required to analyze samples is typically in parts per million (ppm) or parts per million (ppt) range.
• a sample container and an arrangement for electrohydraulic fragmentation of samples wherein the sample container has two oppositely disposed electrodes and is filled with a suitable liquid, generally water, and arranged in the arrangement for electro-hydraulic fragmentation.
• the electrodes of the sample container are connected in series with two other electrodes, between which there is a gas gap.
• the sample container is charged with voltage pulses via a single-stage capacitor discharge circuit and the gas gap.
• the sample container may be removed from the assembly after fragmentation of samples in the sample container and disposed of after removal of the fragmented samples.
• the sample container according to the invention comprises an insulating body and a first and a second electrode.
• the first and the second electrode each protrude into the sample container and are connected to one another via the insulating body.
• the sample container is with a filled dielectric fluid, wherein the first E- electrode is associated with a Gassammeiraum, which can also be referred to as Gasplenum.
• the first electrode is preferably arranged at the top, while the second electrode is preferably arranged opposite the first electrode opposite the bottom.
• gas typically forms in the interior of the sample container in the form of gas bubbles, the gas bubbles usually accumulating on the upper inner side of the sample container. Due to the electrical fields which occur during fragmentation due to pulsed high-voltage discharges, which also occur at the outer side of the sample container, unwanted sliding discharges along the inner sample container walls or sides and / or high-voltage breakdowns or high-voltage flashovers may occur due to the gas bubbles accumulating there the inner and / or outer sides or walls of the sample container come. This can lead to a shortening of the life of the sample container and to its destruction or to its structural failure.
• the sample container according to the invention has a gas collection chamber in which the gas generated during fragmentation by pulsed high-voltage discharges can collect.
• the Gassammei- space is preferably in a substantially field-free in operation space within the field relief, so that the gas or gas bubbles can cause no sliding discharges or high-voltage breakdowns or high-voltage flashovers. Any gas that is present or released in the fragmentation and collected in the gas collection chamber can be taken out of the sample container according to the invention, just like the fragmented samples, for analysis purposes.
• the sample container advantageously forms an independent element, so that for the fragmentation of each sample or each sample material own sample container can be used.
• the sample container according to the invention can be disposed of.
• the inventive arrangement for the electrodynamic fragmentation of samples comprises a process vessel, a sample container according to the invention and means for connecting the first and the second electrode of the sample container to a high voltage source, in particular a high voltage pulse generator.
• the process container is filled with a dielectric liquid and the sample container is disposed within the process container in the dielectric liquid.
• a dielectric liquid which is in particular water, is located both on the inside of the sample container and on the outside of the sample container.
• the sample container is insulated in its interior and in the outer space surrounding the sample container against surface sliding discharges.
• the arrangement and the sample container can be operated with pulse voltages of up to 300 kV, with which a breakdown (so-called solid-state breakdown) can be achieved by samples with dimensions of up to a few centimeters, which leads to a high selective comminution of the samples.
• a field-shaping body is arranged in the process container, which surrounds the sample container like a coat.
• FIG. 1 shows a cross-section of a partial section of a first exemplary embodiment of an inventive arrangement with a first exemplary embodiment of a sample container according to the invention
• FIG. 2 shows potential lines on the right-hand side of the arrangement illustrated in FIG.
• FIG. 3 a schematic representation of a second exemplary embodiment of an arrangement according to the invention with a second exemplary embodiment of a sample container according to the invention
• FIG. 4 shows field lines in an arrangement according to FIG. 3 without field-shaping body (FIG. 4 a), field lines in a further arrangement according to FIG. 3 without field-shaping body (FIG. 4 b), field lines in an arrangement according to FIG. 3 with field-shaping body (FIG. 4 c) and FIG
• Figure 5 shows a cross section of a partial section of an inventive arrangement, as shown schematically in Figure 3.
• the sample container 2 comprises a first, upper electrode 3 and a second, lower electrode 4.
• the sample container 2 is filled with a dielectric liquid 5, in particular water.
• the upper, first electrode 3 is associated with a gas collection chamber 6, which preferably surrounds the region of the first electrode 3 protruding into the sample container 2 in an annular manner such that the end region 7 of the first electrode 3 is arranged in the dielectric liquid 5.
• the electrical field prevailing during the fragmentation process is very small.
• the first electrode 3 preferably projects further into the sample container 2 than the second electrode 4.
• the end region 7 of the first electrode 3 projecting into the sample container 2 is preferably at least partially conically tapered and preferably has a centrally arranged projection 9.
• the protruding into the sample container 2 end portion 8 of the second electrode 4 is preferably designed spherical segment.
• the sample container 2 has an insulating body 10 which connects the first electrode 3 and the second electrode 4 to each other.
• the insulating body 10 is preferably designed as a hollow cylinder.
• the insulating body 10 is, in particular at its end portions 11, 12, preferably made of flexible material.
• the end regions 11, 12 of the insulating body 10 are in contact with sealing surfaces 13, 14 of the first and second electrodes 3, 4, which preferably expand conically outwards in each case.
• the end portion 12 is guided over the sealing surface 14 of the second electrode 4 and in this case preferably by the conical configuration of the sealing surface 14 to the outside conically widened, so that a clamping connection between the end portion 12 and the sealing surface 14 is formed.
• the clamping rings 15 are provided on their respective inner side with clamping grooves 18, so that sliding down or sliding down of the insulating 10 of a sealing surface 13, 14 of the electrodes 3, 4 during the fragmentation of a sample can be prevented.
• the clamping grooves 18 may also be referred to as retaining grooves or barb grooves. Open areas on the walls or sides and / or the end faces of the sample container 2, which can cause a high electric field elevation and thus a flashover over the surface of the insulating body 10, which would result in destruction of the insulating body 10 and thus of the sample container 2 , can be avoided in this way.
• the wall of the insulating body 10 preferably extends as straight as possible and perpendicular to the potential or electric field lines 19 which occur during operation (see FIG.
• the clamping rings 15 are preferably shaped such that the potential lines 19 and the electric field lines are substantially perpendicular to the wall of the insulating body 10.
• the first electrode 3 is preferably configured in such a way that a first, upper triple point 20, which is located between the first electrode 3, the insulating body 10 and the dielectric liquid 5, is electrically connected. is relieved, so that at the upper triple point 20 substantially no electron emission occurs, which could lead to a flashover over the surface of the insulator 10 and thus to a destruction of the insulator 10.
• the protruding into the sample container 2 end portion 7 of the first electrode 3 is preferably designed to taper conically and in particular centrally provided with the projection 9 (see Figure 2).
• the second electrode 4 is preferably designed such that a second, lower triple point 21, which is arranged between the lower electrode 4, the insulating body 10 and the dielectric liquid 5, is electrically relieved, so that also at the lower triple point 21 in FIG Essentially, no electron emission can occur, which could lead to a flashover over the surface of the insulating body 10.
• the end region 8 of the second electrode 4 is preferably designed in the manner of a spherical segment (see FIG. 2).
• a field-shaping body 47 is further provided between the outer wall of the sample container 2 and the inner wall of the process container 22. The field-shaping body 47 and its function will be described in detail below with reference to FIGS. 3 to 5.
• the gas collecting space 6 assigned to the first electrode 3 serves to collect gas or gas volume arising during the fragmentation process, namely at a distance from the inner surface of the insulating body 10 and thus likewise spaced from the upper triple point 20.
• the fragments can be separated - Rung process prevailing electric fields, in particular the prevailing at the upper triple point 20 e- lectric fields, are not substantially affected by the resulting gas, so that high-voltage flashovers on the wall of the insulating body 10 can be avoided.
• the material of the insulating body 10 comprises or the insulating body 10 is made of PE (polyethylene), which is characterized by a high dielectric strength, preferably of LDPE (low density polyethylene), which is characterized by a high ductility.
• the wall thickness of the insulating body 10 is preferably 1 mm. It can thus be ensured that the insulating body 10 and thus the sample container 2 can withstand the forces occurring during the fragmentation process or that the walls of the insulating body 10 can absorb these forces without damage.
• the simple geometry of the insulating body 10 allows cost-effective production, which is particularly advantageous because the sample container 2 and / or the insulating body 10 can be replaced after each fragmentation of a sample to avoid cross-contamination and / or safety reasons due to possible structural fatigue.
• the sample container 2 is arranged in a process container 22 of the arrangement 1 for fragmentation of samples.
• the lower, second electrode 4 is in this case arranged on a bottom 24 of the process container 22, the bottom 24 preferably having means 25 for receiving the lower, second electrode 4 in the form of a raised portion 25 for receiving a bottom recess 26 of the lower, second electrode 4 , In this way, a lateral slippage of the second, lower electrode 4, which could lead to a sliding down of the insulating body 10 from the sealing surfaces 13 and 14, can be prevented. A sliding down of the insulating body 10 from the sealing surfaces 13, 14 would lead to a destruction of the insulating body 10 and thus of the sample container 2.
• the process container 22 is associated with a high voltage electrode 27 which is in communication with the first electrode 3.
• the high voltage electrode 27 is preferably associated with a high voltage insulator 45, which surrounds this nikringf ⁇ rmig.
• the high-voltage electrode 27 preferably surrounds a fixing body 28 in an annular manner.
• the fixing body 28 may be For example, act to a fixing screw which is screwed into the high voltage electrode 27.
• the first electrode 3 preferably has an outer annular edge 29, which encloses the fixing body 28 in the state contacting the high-voltage electrode 27.
• the fixing body 28 prevents the first electrode 3 from slipping sideways, which could result in the insulating body 10 slipping off the sealing surfaces 13, 14.
• the fixing element 28 can therefore advantageously hold the first electrode 3 in its position.
• the sample container 2 shown in FIG. 1 can therefore also be referred to as the smallest sample capsule.
• an ignition voltage of 80 kV it achieves, for example, a stability of 24 high-voltage pulses.
• FIG. 3 shows a second exemplary embodiment of an inventive arrangement 31 for fragmenting samples with a second exemplary embodiment of a sample container 32 according to the invention, which comprises an insulating body 50.
• a first, upper electrode 33 and a second, lower electrode 34 are arranged in the sample container 32.
• the first electrode 33 and the second electrode 34 are preferably each integrated in a short side of the sample container 32.
• the sample container 32 is filled with a dielectric liquid 35, in particular with water.
• the dielectric liquid 35 at least partially covers an end region 37 of the first electrode 33 designed as a pin, wherein the end region 37 projects into the sample container 32.
• a gas collection chamber 36 provided for collecting and collecting gas bubbles generated during fragmentation.
• Sample material 32 to be fragmented or samples 5 38 to be fragmented are introduced into the sample container 32. After the introduction of the samples 38 into the sample container 32, it is filled with the dielectric liquid 35, in particular avoiding gas inclusions. Thereafter, the first electrode 33 and the second electrode 34, which are discharging
• a contact 43 in which it. in particular may be a resilient contact strip.
• the lower, second electrode 34 preferably represents a ground electrode which is connected to a
• closing electrode 40 is connected, which is formed by the housing 44 of the process container 41.
• the upper connection electrode 39 which is connected to the first, upper electrode 33, is arranged, preferably centrally, in the process container 31 and has an electrode stem.
• connection electrode 39 formed from electrode rod 39.1 and electrode basin 39.2 is preferably formed in one piece.
• the electrode rod 39.1 is preferably annularly surrounded by a high-voltage insulator 45.
• the electrode basin 39.2 has the function of a field relief.
• the gas collection chamber 36 is advantageous Properly disposed in a substantially field-free space within the field relief, so that the gas collected in the gas collection chamber 36 has substantially no effect on the high voltage breakdown generated in the fragmentation.
• the gas collection chamber 36 is preferably arranged inside the electrode basin 39. 2 for this purpose.
• the process container is filled with a dielectric liquid 46, which is preferably water, wherein the sample container 32 arranged in the process container 41 is completely surrounded by the dielectric liquid 46.
• a dielectric liquid 46 which is preferably water
• the dielectric fluids 35 and 46 also other dielectric fluids than water into consideration.
• the first, upper electrode 33 is preferably designed such that a triple point 20, which is located between the first electrode 33, the insulating body 50 and the gas collection chamber 36, is electrically relieved, so that substantially no electron emission occurs at the triple point 20. Such an electron emission could lead to a flashover over the surface of the insulating body 50 and thus to a destruction of the insulating body 50.
• the second, lower electrode 34 is preferably designed such that a triple point 21, which is located between the second electrode 34, the insulating body 50 and the dielectric liquid 35, is electrically relieved so that substantially no electron emission occurs at the triple point 21 ,
• a field shaping body 47 is arranged, which surrounds the sample container 32 like a coat.
• the field-shaping body 47 is thus provided between the inner wall of the housing 44 of the process container 41 and the outer wall of the sample container 32.
• the material of the field forming body 47 or the Feldformungsk ⁇ rper 47 made of plastic, in particular HDPE (high density polyethylene).
• HDPE high density polyethylene
• the field-shaping body 47 can withstand high loads in the form of voltage pulses without being destroyed.
• the field-shaping body 47 widens preferably conically, in order to pass into a section not denoted in detail with a larger inner diameter. By increasing the inner diameter of the field-shaping body upwards, space is created for receiving the high-voltage insulator 45 and the electrode basin 39.2.
• the electrical fields produced during the fragmentation are influenced or controlled in such a way that substantially no impermissibly high electric field strengths, which could lead to destruction of the sample container 32 and / or the process container 41, along the inner or the outer wall of the sample container 32 and the insulator 50 may occur.
• FIG. 4 shows the profile of the electric field lines 48 in a right-hand section of the process container 41 with sample container 32 arranged in the latter.
• FIGS. 4a and 4b do not provide a field-shaping element, the distance between the outer wall of FIG Sample container 32 and the inner wall of the process container 41 is selected to be substantially smaller than in Figure 4b.
• the respective field lines 38 extend over a relatively long distance within the wall of the insulating body 50 or of the sample container 32.
• the field lines 38 are close to one another, which is indicative of an electric field increase.
• a field-shaping body 47 is provided between the outer wall of the sample container 32 and the inner wall of the process container 41. This has the effect that the field lines in comparison with the figures 4a and 4b only about extend short distances through the wall of the insulating body 50 and the sample container 32, further apart and thus less burden on them.
• pulsed, high-current high-voltage discharges are generated between the first electrode 33 and the second electrode 34 by means of the high-voltage pulse generator 42 for fragmenting the samples 38.
• the high voltage pulse generator 42 voltage pulses with a pulse duration of up to a few microseconds at voltage peaks of several 100 kV, in particular of up to 300 kV, and currents of up to 10 kA can be generated.
• the number of pulsed ones After generating a certain number of pulsed high voltage discharges by the high voltage pulse generator 42, the number of pulsed ones
• High voltage discharges is smaller than the permissible for the sample container 32 number, the sample material 38 is fragmented and the sample container 32 can be separated from the terminal electrodes 39, 40 of the high voltage pulse generator 42 and unopened the assembly 31 are removed. If the sample container 32 was completely cleaned or unused and new prior to fragmentation, after fragmentation it may contain only solid, liquid and / or gaseous constituents of the fragmented sample material which was fragmented during the last application of the sample container. The sample container 32 can thus contain only such contaminants that have arisen during fragmentation, for example due to abrasion of the material of the first and the second electrode 33, 34 and the insulating body 50 (so-called inherent contamination).
• This inherent contamination can in principle be influenced and minimized by a suitable choice of the material of the first and second electrodes 33, 34 and with respect to the quantity of contaminants by a suitable choice of the discharge parameters of the high voltage pulse generator 42.
• the discharge parameters of the high voltage pulse generator 42 are given for example by the duration of the current / voltage pulses, the height of the voltage peaks and the current levels.
• Cross-contamination by previously fragmented samples can advantageously not occur with a single or completely purified use of the sample container 32.
• New or completely cleaned first and second electrodes 33, 34 are preferably used in each case for the fragmentation of new samples.
• sample container 32 withstands the load peaks due to the high voltage discharges and remains sealed so that no material exchange between the sample container 32 and the process container 41 can take place.
• sample container 32 or the insulating body 50 of the sample container 32 withstands the load peaks and remains tight, it preferably contains or preferably consists of polyethylene, in particular of LDPE (low density polyethylene).
• the distance between the mutually facing surfaces of the first and second electrodes 33, 34 is preferably up to a few centimeters.
• the sample container 32 preferably has a volume of between 0.25 and 0.5 liters and is used as a disposable sample container. It is preferably designed in such a way that it reduces the pulse loads occurring during fragmentation with respect to the high voltage to be isolated of up to several 100 kV, in particular up to 300 kV, the high current intensities occurring thereby, in particular of up to 10 kA, can withstand the high power associated therewith, particularly up to 100 megawatts, and the pressure spikes within the sample container 32 caused thereby for a given number of high voltage pulses in the electrodynamic fragmentation so that the sample material 38 can be selectively fragmented.
• the sample container 32 and the arrangement 31 are designed according to the invention such that they the in the in the sample container 32 located dielectric liquid 35 caused by the high voltage discharges shock waves occurring in the unspecified wall of the sample container 32 and the insulator 50 high electric field strengths occurring in the field shaping body 47 high electric field strengths and the impact or the effect of components of the sample material, which strike during the fragmentation on the wall of the sample container 32 and the insulator 50, during a certain number of high-voltage pulses can withstand without the sample container 32 and the assembly 31 are destroyed or damaged.
• This is achieved in particular by the configuration of the sample container 32, the advantages and the design of the field shaping body 47 and the provision of dielectric fluids 35 and 46 both in the sample container 32 and in the process container 41 of the arrangement 31.
• the sample container 32 according to the invention and the arrangement 31 according to the invention can be used, for example, during 300 high-voltage pulses or loaded with up to 300 high-voltage pulses.
• FIG. 5 shows a cross-section of a part of an arrangement 31 with a process container 41 and a sample container 32, which surrounds a field-shaping body 47, as shown schematically in FIG.
• the process container 32 comprises an insulating body 50 having a bottom 51.
• the insulating body 50 is preferably associated with a lid 52.
• the material of the sample container 32 or of the insulating body 50 which is preferably LDPE (low density polyethylene) or which preferably comprises LDPE, additionally serves as a sealing material.
• LDPE low density polyethylene
• LDPE low density polyethylene
• the sample container 32 can be used as the sample container 32.
• LDPE low density polyethylene
• the field Mung body 47 and the first and second electrodes 33, 34 can be used easily manufactured rotary parts. Additional smoothing of the surface of commercially available wide-mouth bottles can lead to a further increase in the seal.
• an upper, unspecified cover-side region of the first, upper electrode 33 and / or a lower, unspecified bottom-side region of the second, lower electrode 34 preferably have sealing grooves 53 , which are produced in particular when introducing the first electrode 33 into the cover 52 or when introducing the second electrode 34 into the bottom 51 of the insulating body 50, preferably by reshaping during clamping.
• unspecified sealing beads in an electrode-side region of the cover 52 and / or during insertion of the second electrode 34 unspecified sealing beads are preferably formed in an electrode-side region of the bottom 51 of the insulating body 50.
• cover-side end portion of the insulating body 50 and / or the isolier emotions lake side of the lid 52 support rings 54, 55 are assigned in the form of an inner piece ring 54 and an outer support ring 55 for further improvement of the seal.
• the inner support ring 54 is preferably provided within a lid groove, while the outer support ring 55 is disposed on the outer side or surface of the end portion of the insulating body 50. If a wide-mouth bottle or another bottle is used as the insulating body 50, then the outer support ring 55 is arranged on the outside of the bottle neck.
• means 57 are preferably provided for receiving the second electrode 34, which are preferably configured as a depression 57.
• the life of the sample container 32 and the insulator 50 is increased by providing dielectric liquid on the inside and outside of the sample container 32, and by providing a field forming body 47 and a gas collecting space 36.
• sample container 32 As a disposable sample container whose components such as the support rings 54, 55, the insulating body 50 and the first and second electrodes 33, 34 are designed simple and inexpensive.
• first exemplary embodiment of the inventive arrangement 1 shown in FIG. 1 with the second exemplary embodiment of the inventive sample container 32 shown in FIGS. 3, 5 or the second exemplary embodiment of the inventive arrangement 31 shown in FIGS 1 illustrated the first embodiment of the inventive sample container 2 are combined.
• the features of the first and the second embodiment of the inventive arrangement or the first and second embodiments of the inventive sample container can be combined.

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• Health & Medical Sciences (AREA)
• Toxicology (AREA)
• Engineering & Computer Science (AREA)
• Food Science & Technology (AREA)
• Sampling And Sample Adjustment (AREA)
• Electrotherapy Devices (AREA)

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• 2007
  • 2007-03-16 DK DK07710803.3T patent/DK2136925T3/da active
  • 2007-03-16 US US12/525,278 patent/US8138952B2/en not_active Expired - Fee Related
  • 2007-03-16 JP JP2009553878A patent/JP4914506B2/ja not_active Expired - Fee Related
  • 2007-03-16 WO PCT/CH2007/000144 patent/WO2008113189A1/fr active Application Filing
  • 2007-03-16 EP EP07710803A patent/EP2136925B1/fr active Active
  • 2007-03-16 AT AT07710803T patent/ATE537903T1/de active
  • 2007-03-16 AU AU2007349730A patent/AU2007349730B2/en not_active Ceased
  • 2007-03-16 CA CA2680667A patent/CA2680667C/fr not_active Expired - Fee Related
  • 2007-03-16 ES ES07710803T patent/ES2378484T3/es active Active
  • 2007-03-16 RU RU2009134499/21A patent/RU2422207C2/ru not_active IP Right Cessation

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