EP2951519A1 - A furnace for preparing fused (homogonised) samples for sample analysis - Google Patents
A furnace for preparing fused (homogonised) samples for sample analysisInfo
- Publication number
- EP2951519A1 EP2951519A1 EP13873188.0A EP13873188A EP2951519A1 EP 2951519 A1 EP2951519 A1 EP 2951519A1 EP 13873188 A EP13873188 A EP 13873188A EP 2951519 A1 EP2951519 A1 EP 2951519A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- crucibles
- furnace
- carousel
- samples
- moving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004458 analytical method Methods 0.000 title claims abstract description 15
- 230000007246 mechanism Effects 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 230000004907 flux Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 230000008602 contraction Effects 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 4
- 230000001419 dependent effect Effects 0.000 claims 2
- 239000000523 sample Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007704 wet chemistry method Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011369 resultant mixture Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
- F27B9/16—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a circular or arcuate path
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/30—Details, accessories, or equipment peculiar to furnaces of these types
- F27B9/38—Arrangements of devices for charging
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/30—Details, accessories, or equipment peculiar to furnaces of these types
- F27B9/39—Arrangements of devices for discharging
Definitions
- the present invention broadly relates to a furnace for preparing fused (homogenised) samples for sample analysis.
- samples such as mineral samples, cement samples and other materials need to be homogenized (or fused) before they can be analysed by analytical
- Sample preparation typically involves mixing the sample with a flux and placing the mixture in a furnace that is heated to form a homogeneous melt.
- the homogenized melt is allowed to cool in a crucible to form a glass bead which is then analyzed or the homogenized melt is cast into a mould which is typically preheated and allowed to cool into a glass bead prior to the analysis.
- the homogenized mix can be allowed to cool before it is digested in an acid or acid mix.
- the molten homogenized sample can be cast into a container, containing the appropriate acid. Once digested, the sample can be further diluted before it is analysed using suitable wet chemistry techniques.
- Available fusion systems that are designed for the above- mentioned purposes allow for batch operation. A batch of the crucibles loaded with the mixture of sample and flux material is places into a furnace. The furnace is then closed and samples are heated. After heat treatment the furnace is opened and the batch of the samples is removed.
- PCT publication number WO2003098140 and South African patent number 2005/05485 disclose a furnace that has a carousel for movement of the batch of samples about an axis.
- the present invention provides further improvement.
- the present invention provides in a first aspect a furnace for preparing fused (homogenised) samples for sample analysis, the furnace comprising:
- a heater arranged for heating an interior portion of the housing to a temperature sufficient for causing melting of each sample
- a carousel positioned in the housing, the carousel having a plurality of receiving stations for receiving crucibles containing respective samples, the carousel being arranged for rotating the crucibles about an axis when the crucibles are positioned in respective receiving stations; and a mechanism for moving the crucibles relative to the respective receiving stations and relative to the housing to load and unload the carousel.
- the heater typically is arranged to heat the crucible with the respective samples, such as a suitable mixture of a mineral sample material and a flux, to a temperature to effect melting of each sample and flux.
- the mechanism for moving the crucibles is arranged to move the crucibles in a direction that has a component perpendicular to the axis about which the carousel is arranged to move the crucibles.
- the housing typically has an access port in a side wall portion through which in use the crucibles are moved in a substantially horizontal direction by the mechanism for moving the crucibles.
- the access port may comprise an access door that is arranged to close the access port.
- the mechanism for moving the crucibles may comprise a first arm having a portion for supporting a crucible and being arranged for contraction and extension along a length of the arm whereby the first arm is arranged such that the crucible can be moved between a receiving station of the carousel and a position that is remote from the carousel .
- the mechanism for moving the crucibles also comprises a second arm for moving the crucibles with the respective samples.
- the second arm may also have a portion for supporting a crucible and may be arranged for contraction and extension along a length of the arm whereby the second arm is arranged such that the crucible with the respective samples can be moved between a receiving station of the carousel and a position that is remote from the carousel.
- the first arm is arranged for positioning the crucibles into the receiving stations of the carousel and the second arm is arranged for removing the crucibles with the respective samples from the receiving stations.
- the furnace may also comprise a device for measuring temperature .
- the furnace typically comprises a control system that is arranged to control operation of the heater, the carousel and the mechanism for moving the crucibles.
- the control system typically is configured to effect removal of a crucible with the respective sample after the sample has been treated in a manner such that the sample forms a homogeneous glass when cooled subsequent to the heat treatment.
- the control system typically comprises a microprocessor and may be arranged to control operation of the furnace such that the first arm in use positions a sequence of crucibles into a sequence of respective receiving stations and the heater subsequently heats the samples in the crucibles during rotation of the crucibles in the carousel.
- the control system typically is arranged to control the furnace such that the second arm removes the crucibles with respective samples sequentially from the receiving stations after completion of a
- the control system controls the control system to predetermined heat treatment.
- control system typically is arranged such that loading, rotation by the carousel, heat treatment and unloading is performed in an automated manner.
- control system typically is arranged such that parameters are selectable by a user.
- the parameters may include a rotation or an oscillation rate of the carousel, a temperature of the furnace or a duration of the heat treatment.
- control system in accordance with one example
- the control system comprises a timer for timing a period of time during which the samples are exposed to the heat treatment.
- the control system with the timer may be arranged to interrupt the heat treatment after a predetermined time or effect an alarm signal.
- the control system may comprise a memory device for storing control parameters.
- the furnace may be arranged to impart a rocking,
- Each receiving station of the carousel typically comprises an aperture that is arranged to receive a respective crucible.
- the furnace may comprise an arrangement for lifting and lowering the crucibles relative to the first and second arms to unload or load the crucibles form or onto the first and second arms, respectively.
- the control system typically is arranged such that the first arm delivers a crucible to a position over a respective receiving station and the arrangement for lowering and lifting lifts the carousel such that the crucible is positioned in the aperture of the respective receiving station.
- the control system typically is arranged such that, after completion of heat treatment, the arrangement for lowering and lifting the crucible lowers the carousel to position the crucible on the second arm and the second arm then moves the crucible to a position outside the housing of the furnace .
- the furnace typically comprises a conveying system that is arranged for conveying a sequence of crucibles to the first arm and a sequence of crucibles away from the second arm of the mechanism for movement of the crucibles.
- the carousel is one of a plurality of carousels.
- a first carousel may be positioned over a second carousel and arranged for rotation about the same axis.
- the access door of the access port typically is arranged for remote controlled operation and the control system typically is arranged to control the operation of the access door in an automated manner to allow operation of the mechanism for moving the crucibles (which typically comprises the above-described first and/or second arm) .
- the control system typically is arranged to control the operation of the access door in a manner such that loss of thermal energy through the access port is reduced or minimised.
- the present invention provides in a second aspect a method of preparing fused (homogenised) samples, the method comprising the steps of: providing a plurality of crucibles with samples to a mechanism for moving the crucibles; moving the crucibles in sequence to respective receiving stations of a carousel of a furnace using the mechanism for moving the crucibles; exposing the samples to heat treatment to melt the samples in the crucibles; rotating the crucibles in respective receiving stations about an axis of the carousel and subsequently removing the crucibles with the respective samples in sequence using the mechanism for moving the crucibles and positioning the crucibles on a conveyor for moving the crucibles away from the furnace.
- the step of moving the crucibles may comprise moving the crucibles in a substantially horizontal direction and typically through an access port in a side wall of a housing of the furnace. Further, the step of removing the crucibles with the respective samples may also comprise moving the crucibles in a direction that is transversal to an axis of rotation of the carousel and typically through an access port in a side wall of a housing of the furnace.
- the method may be conducted in an automated
- the method may comprise selecting parameters, such as a temperature of the furnace or a rotation rate of the carousel.
- the method may comprise imparting a rocking, vibrating or oscillating motion to the samples in the crucibles when the samples are exposed to the heat treatment.
- the method may comprise using a control system to effect removal of a crucible with the respective sample after the sample has been treated in a manner such that the sample forms a homogeneous glass when cooled subsequent to the heat treatment.
- the step of moving the crucibles may comprise using a first arm having a portion for supporting a crucible and being arranged for contraction and extension along a length of the arm whereby the crucible is moveable between a receiving station of the carousel and a position that is remote from the carousel.
- the step of removing the crucibles with the respective samples may comprise using a second arm that has a portion for supporting a crucible and is arranged for contraction and extension along a length of the arm whereby the crucibles with the respective samples are moveable between a receiving station of the carousel and a position that is remote from the carousel.
- the method may also comprise imparting an oscillating motion to the samples in the crucibles during fusion when the crucibles are positioned in the receiving stations.
- the method typically comprises heating the samples to a temperature above the melting point of the sample flux mixture .
- Figures 1 to 4 show schematic cross-sectional views of a furnace for preparing fused (homogenised) samples in accordance with an embodiment of the present invention
- Figure 5 shows a schematic perspective view of the furnace ;
- Figures 6 and 7 show schematic cross-sectional views of the furnace; and
- Figure 8 is s flow chart illustrating a method preparing fused (homogenised) samples in accordance with an
- Embodiments of the present invention relate to a furnace for preparation of fused (homogenized) samples suitable for analytical techniques, such as X-ray fluorescent spectrometry or mechanical analysis techniques such as inductively-coupled plasma mass spectrometry.
- analytical techniques such as X-ray fluorescent spectrometry or mechanical analysis techniques such as inductively-coupled plasma mass spectrometry.
- the furnace 100 comprises a housing 102 in which a carousel 104 is positioned.
- the carousel 104 is arranged for rotation about an axis and Figures 6 and 7 show a drive 105 of the carousel 104.
- the carousel 104 has a plurality of receiving stations 106 that each have an aperture and the apertures are positioned in a ringlike manner along the periphery of the carousel 104.
- Each aperture of a receiving station 106 is sized to receive and hold a crucible 108.
- the crucible 108 has a radial lip that extends in a ring-like manner at an upper portion of the crucible 108 and which rests on the carousel 104 when the crucible 108 is positioned in a respective receiving station 106.
- the furnace 100 is arranged for heating samples to a temperature suitable for melting the samples to generate fused (homogenised) samples that form a homogeneous glass bead when cooled and are suitable for the above-mentioned analysis techniques.
- the furnace is arranged for heating the samples to a temperature
- samples for fusion may for example include mined materials (in powder form) or any other type of mineral that is suitably prepared.
- Sample preparation includes mixing with a flux material and loading a resultant mixture into the crucibles 108.
- the furnace 100 also comprises a mechanism 110 for moving crucibles 108 between respective receiving stations 106 and a location that is exterior to the housing 102.
- the mechanism 110 comprises a first arm 112 and a second arm 114.
- the first arm 112 is arranged for moving the crucibles 108 from the exterior position to a respective receiving station 106 of the carousel 104.
- the second arm 114 is arranged for moving the crucibles 108 out of respective receiving stations 106 and to the exterior location.
- Both arms 112 and 114 have suitable support surfaces for supporting the crucibles 108 and are arranged for moving by suitable electrical or hydraulic means in horizontal directions.
- Figure 1 shows how an end of the second arm 114 is in contact with a crucible 108.
- Figure 2 shows the second arm 114 after it removed the crucible 108 and is in a contracted condition.
- the representation of Figure 3 is similar to that of Figure 2, but the mechanism 110 moved in a direction that is transversal to the rotation direction of the carousel such that the first arm is now positioned opposite the receiving station 106 from which previously a crucible 108 was removed by the second arm 114.
- Figures 4 to 6 show the first arm 112 in an extended condition in which the first arm 112 moved a crucible 108 into the receiving station 106 and Figure 7 shows the furnace 100 with the first arm 112 in a contracted condition .
- the carousel 104 is moveable along its axis in upward and downward direction.
- Figure 6 shows the carousel in an upward position
- Figure 7 shows the carousel in a downwards positions. The upward and downward movement of the carousel 104 is controlled such that the carousel 104 is in a downward position when the arm 112 moves a crucible 108 over a respective receiving station 106.
- the carousel 104 then moves to the upward position such that the crucible 108 is lifted off the arm 112 and is placed in the aperture of the receiving station 106.
- the first arm 112 then retracts.
- the second arm 114 and the carousel 104 operate in a corresponding manner for unloading the crucibles 108.
- Coupled to the furnace 100 is a conveying system from which crucibles 108 are positioned by the second arm 114 and which delivers crucibles 108 to the first arm 112 in a sequential manner.
- a conveying system may take any suitable form and such systems are known in the art.
- the housing 102 of the furnace 100 has an access port 116 at a side portion through which the arms 112 and 114 move the crucibles 108.
- the access port 116 has an access door (not shown) that can be remotely opened and closed when the first or second arms 112, 114 are in use.
- the furnace 100 may also comprise more than one carousel 104 and the carousels may be positioned over one another and arranged for rotation about a common axis driven by the drive 105.
- the furnace 100 comprises a suitable means for moving all carousels up and down such that the arms 112 and 114 are able to operate as described above.
- the furnace 100 may also comprise more than one mechanism for moving the crucibles 108 and the mechanisms may be stacked on top of one another in the same manner as the carousels.
- the furnace 100 comprises control electronics (not shown) that is arranged to allow automated operation of the furnace 100. Further, the furnace 100 comprises
- a temperature sensors (not shown) and is arranged such that a user can select a temperature and a time for the heat treatment. These parameters may be preselected and the control electronics is arranged to operate in accordance with the pre-selected parameters in an automated manner. Consequently, the control electronics controls operation of the drive 105, a heater (not shown), the carousel and the first and second arms 112 and 114. The control electronics is also arranged to control operation of the access door (not shown) at the access port 116 when the first or second arms 112, 114 are in use.
- a drive shaft of the carousel 104 is arranged for imparting an oscillating movement about the axis of the carousel 104 and is also controlled by the control system .
- the furnace may be the above-described furnace 100.
- the method 800 comprises the initial step 802 of providing a plurality of crucibles with samples to a mechanism for moving the crucibles. Further, the method 800 comprises step 804 of moving the crucibles in sequence to respective receiving stations of a carousel of the furnace using the mechanism for moving the crucibles. Step 804 moves the crucibles through an access port in a side wall of the furnace.
- the method 800 comprises step 806 of rotating and oscillating the crucibles in respective receiving stations about an axis of the carousel while exposing the samples to heat treatment in the furnace. The heat is sufficient to cause melting of each sample.
- the method 800 also comprises step 808 of removing the crucibles with respective samples in sequence using the mechanism for moving the crucibles and positioning the crucibles on a conveyor for moving the crucibles away from the furnace .
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Clinical Laboratory Science (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
Claims
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/AU2013/000080 WO2014117202A1 (en) | 2013-01-31 | 2013-01-31 | A furnace for preparing fused (homogonised) samples for sample analysis |
Publications (3)
Publication Number | Publication Date |
---|---|
EP2951519A1 true EP2951519A1 (en) | 2015-12-09 |
EP2951519A4 EP2951519A4 (en) | 2016-11-02 |
EP2951519B1 EP2951519B1 (en) | 2018-08-29 |
Family
ID=51261300
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP13873188.0A Active EP2951519B1 (en) | 2013-01-31 | 2013-01-31 | A furnace for preparing fused (homogenised) samples for sample analysis |
Country Status (2)
Country | Link |
---|---|
EP (1) | EP2951519B1 (en) |
WO (1) | WO2014117202A1 (en) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU921738A1 (en) * | 1978-09-13 | 1982-04-23 | Проектно-Конструкторское Бюро "Укрстальконструкция" Министерства Монтажных И Специальных Строительных Работ Усср | Production line for producing welding electrodes |
KR100289988B1 (en) * | 1998-03-07 | 2001-05-15 | 김화중 | A manufacturing apparatus for gold bar |
WO2003098140A1 (en) * | 2002-05-22 | 2003-11-27 | Innovative Met Products (Pty) Limited | Continuous furnace |
US7172729B2 (en) * | 2003-03-04 | 2007-02-06 | Jose Maria Las Navas Garcia | Mixed sample moisture or ash analyzer |
DE102007006553A1 (en) * | 2007-02-09 | 2008-08-14 | ELTRA Entwicklungs- und Vertriebsgesellschaft von elektronischen und physikalischen Geräten mbH | Thermo gravimetric analyzer for cooling ventilator, blows wind around crucibles, carrousel and heating elements of furnaces during cooling phase |
US8323565B2 (en) * | 2007-04-12 | 2012-12-04 | Leco Corporation | Crucible shuttle assembly and method of operation |
US8592695B2 (en) * | 2010-11-30 | 2013-11-26 | Jose Maria Las Navas Garcia | Stackable crucible, a system using a stackable crucible, and a method of using a stackable crucible |
-
2013
- 2013-01-31 EP EP13873188.0A patent/EP2951519B1/en active Active
- 2013-01-31 WO PCT/AU2013/000080 patent/WO2014117202A1/en active Application Filing
Also Published As
Publication number | Publication date |
---|---|
WO2014117202A1 (en) | 2014-08-07 |
EP2951519B1 (en) | 2018-08-29 |
EP2951519A4 (en) | 2016-11-02 |
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