EP4662473A1 - Fusionssystem und verfahren zur durchführung einer probenfusion damit - Google Patents

Fusionssystem und verfahren zur durchführung einer probenfusion damit

Info

Publication number
EP4662473A1
EP4662473A1 EP24752614.8A EP24752614A EP4662473A1 EP 4662473 A1 EP4662473 A1 EP 4662473A1 EP 24752614 A EP24752614 A EP 24752614A EP 4662473 A1 EP4662473 A1 EP 4662473A1
Authority
EP
European Patent Office
Prior art keywords
sample holder
fusion
loading
area
handling mechanism
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.)
Pending
Application number
EP24752614.8A
Other languages
English (en)
French (fr)
Inventor
Pierre Bouchard
Julien BOISCLAIR
Sébastien DION
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Spectris Canada Inc
Original Assignee
Spectris Canada Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Spectris Canada Inc filed Critical Spectris Canada Inc
Publication of EP4662473A1 publication Critical patent/EP4662473A1/de
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/36Embedding or analogous mounting of samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/0099Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor comprising robots or similar manipulators
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076X-ray fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202Preparing specimens therefor

Definitions

  • the application relates generally to the field of analytical sample preparation, and more particularly, to the field of analytical sample preparation by fusion.
  • High quality and productive sample preparation can be key for chemical analysis of samples using X-Ray Fluorescence Spectrometry (XRF), Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES), Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and Atomic Absorption Spectroscopy (AAS).
  • XRF X-Ray Fluorescence Spectrometry
  • ICP-OES Inductively Coupled Plasma Optical Emission Spectroscopy
  • ICP-MS Inductively Coupled Plasma Mass Spectrometry
  • AAS Atomic Absorption Spectroscopy
  • Fusion process sample preparation can involve heating up the chemical compound to melt the sample/flux, and then cooling down the melt to solidify the sample.
  • the mechanism that holds the sample crucible moves the sample from a heating zone to a cooling zone, and holds the sample crucible during the heating.
  • process temperatures can be quite high, various problems and challenges can arise, such as contamination of the sample, health & safety concerns for operators, challenges and costs associated to selecting materials operable to sustain high temperatures which can be present at the fusion area, and thermal inertia of components which may interfere with or slow the reaching of an intended thermal state.
  • the fusion process can be a bottleneck in a sample analysis process, and therefore, productivity can be a significant additional concern. There always remains room for improvement.
  • a handling mechanism which can handle the movement and transfer of a sample holder between a fusion area and one (or more) loading station(s).
  • the handling mechanism can handle the movement and transfer of the sample holder while another sample holder is loaded in a loading station, allowing an operatorto manually load, refill or recharge samples, crucibles and/or moulds in a loading station while the fusion process is underway for samples in another sample holder.
  • a method of handling a sample comprising: fusing first samples contained in a first sample holder at a fusion area of a furnace; with a handling mechanism moving the first sample holder with the samples along a longitudinal orientation, out from the fusion area, into a loading station outside the fusion area; with the handling mechanism, moving a second sample holder into the fusion area; fusing second samples contained in the second sample holder at the fusion area.
  • the loading station is a first loading station
  • said moving the second sample holderto the fusion area includes moving the second sample holderfrom a second loading station into the fusion area.
  • said moving of the second sample holder includes moving the second sample holder while the first sample holder is in the loading station.
  • said moving of the second sample holder to the fusion area includes positioning the handling mechanism in a loading position outside the fusion area of the furnace.
  • Some embodiments can further include putting the second samples into the second sample holder and putting the second sample holder at the second loading station prior to said moving the second sample holder, and taking the first sample holder from the first loading station.
  • Some embodiments can further include putting the second samples into the second sample holder and loading the second sample holder onto the handling mechanism in a loading position prior to said moving the second sample holder, and taking the first sample holder from the loading station.
  • said putting the second sample holder at a second loading station is done during said fusing of the first samples or during said moving the first sample holder.
  • the loading station is fixed relative to the furnace.
  • the loading station and the handling mechanism are vertically and longitudinally offset from one another.
  • said moving the first sample holder includes engaging the first sample holder with a first loading attachment of the first loading station, and moving the second sample holder includes disengaging the second sample holder from a second loading attachment of the second loading station.
  • said engaging the first sample holder includes moving first sample holder onto the prongs of first loading attachment and disengaging the second sample holder includes moving the second sample holder away from prongs of the second loading attachment.
  • said moving the first sample holder includes engaging the first sample holder with a pouring mechanism outside the fusion area and disengaging the first sample holder from the pouring mechanism outside the fusion area.
  • Some embodiments can further include the pouring mechanism pouring the samples from the first sample holder to a third sample holder between said engaging the first sample holder with the pouring mechanism and said disengaging the first sample holder from the pouring mechanism.
  • Some embodiments can further include the handling mechanism positioning the third sample holder to receive the samples.
  • Some embodiments can further include the handling mechanism moving the third sample holder to the loading station subsequently to said pouring.
  • Some embodiments can further include the handling mechanism moving the third sample holder to a cooling station and the cooling station ventilating the third sample holder for a period of time subsequently to said pouring and priorto said moving the third sample holderto the loading station.
  • said moving the second sample holder into the fusion area includes engaging the second sample holder with an agitation mechanism at the fusion area, and said moving the first sample holder out from the fusion area includes disengaging the first sample holder from the agitation mechanism.
  • the fusion area is enclosed in a heating chamber, the heating chamber having a door, further comprising closing the door and opening the door between said moving the first sample holder out from the fusion area and moving the second sample holder into the fusion area.
  • a fusion system comprising: a furnace having a fusion area, and a heating element; a loading station operable to receive a corresponding sample holder; and a handling mechanism having a base located outside the fusion area, a support operable to receive the sample holder, the handling mechanism operable to move the support into and out from the fusion area and into and out from the loading station.
  • the loading station is a plurality of loading stations, each operable to receive at least one corresponding said sample holder, the support operable to receive at least one said sample holder, the handling mechanism operable to move the support into and out from either one of the plurality of loading stations.
  • the (or each) loading station is fixed relative to the furnace.
  • the loading station(s) have a loading attachment operable to receive the (or each) said sample holder, and a loader door pivotably mounted to the furnace, the loader door operable to selectively allow access to the loading station.
  • the loading attachment may be mounted within a drawer, the drawer being openable to provide manual access to the loading attachment and closeable to provide access to the at least one said sample holder received in the loading attachment by the handling mechanism.
  • Some embodiments can further include a controller operable to control the handling mechanism and for selectively locking or unlocking, for example, the loader door or either one of the drawers in the closed position (depending on the embodiment).
  • the handling mechanism includes a linkage between the base and the support, the linkage being extendible and collapsible on a first side of the base to move the support along a horizontal, longitudinal orientation between a neutral area coinciding with the base and the fusion area, the support movable by the linkage across the neutral area, the linkage further being extendible and collapsible on a second side, the second side opposite the first side relative the neutral area.
  • the loading position ofthe handling mechanism, and/orthe loading station(s) are at the second side (i.e. outside the fusion area).
  • the handling mechanism has an upright displacement mechanism and a horizontal displacement mechanism, wherein the horizontal displacement mechanism is activated to move the sample holder to and from the fusion area.
  • the sample holder is engageable with the loading attachment by moving the sample holder with the horizontal displacement mechanism.
  • the upright displacement mechanism has a upright displacement mechanism base and moves the horizontal displacement mechanism and the support upwardly and downwardly relative to the base.
  • the furnace has a heating chamber having a plurality of walls enclosing the fusion area, and the loading station(s) are located entirely outside the heating chamber.
  • Some embodiments can further include a housing enclosing the furnace, the handling mechanism and the plurality of loading stations.
  • the loading stations are operable to bias a sample holder received therein to an inclined orientation.
  • a method of handling sample holders containing samples within a fusion system having a handling mechanism comprising, with the handling mechanism: moving a first sample holder from a user-accessible area to a fusion area of a furnace; moving the first sample holder from the fusion area to an intermediary station away from the user-accessible area; and moving a second sample holder from a loading station located in the user-accessible area to the fusion area while the first sample holder remains at the intermediary station.
  • the method further comprises, with the handling mechanism, moving the first sample holder from the intermediary station to the user-accessible area.
  • said moving of the first sample holder to the user-accessible area includes moving the first sample holder to a loading station located in the user-accessible area.
  • the method further comprises, with the handling mechanism, moving the second sample holder from the fusion area to the intermediary station. [0041] In some embodiments, the method further comprises, with the handling mechanism, moving the second sample holder from the intermediary station to the user-accessible area by configuring the handling mechanism in a loading position in which the handling mechanism is at least partially inside the user-accessible area.
  • said moving of the second sample holder to the user-accessible area with the handling mechanism being in the loading position is performed while the first sample holder is in a loading station of the user-accessible area.
  • the moving of the first sample holder from the fusion area to the intermediary station includes cooling the first sample holder in the intermediary station.
  • the cooling of the first sample holder includes causing a flow of a cooling fluid around the first sample holder.
  • FIG. 1A is a perspective view of a fusion system
  • Fig. 1 B is a perspective view showing internal components of the fusion system of Fig. 1 A;
  • Fig. 1 C is a cross-sectional view of a portion of the fusion system of Figs. 1A and 1 B;
  • Fig. 1 D is another a cross-sectional view of a portion of the fusion system of Figs. 1A and 1 B;
  • Fig. 1 E is an example of a controller of the fusion system of Figs. 1A and 1 B;
  • Fig. 2A is a perspective view of a sample holder
  • Fig. 2B is a perspective view of the sample holder of Fig. 2A with a plurality of containers;
  • Fig. 2C is a schematic top plan view of terminal ends of agitation or support rods;
  • Fig. 2D is a schematic top plan view similar to the view of Fig. 2C, showing engagement of an integral sample holder to the terminal ends;
  • Fig. 2E is a schematic top plan view similar to the view of Fig. 2C, showing engagement of a sample holder having two loosely connected segments to the terminal ends;
  • Fig. 2F is a partial perspective view, exploded, of another example of a sample holder
  • FIG. 2G is a partial perspective view of yet another example of a sample holder
  • Fig. 2H is a partial perspective view, sectioned, of the sample holder of Fig. 2F;
  • FIG. 3A is a perspective view of a handling mechanism of the fusion system of Figs. 1A and 1 B;
  • FIG. 3B is another view of the handling mechanism of Fig. 3A;
  • FIG. 3C is yet another view of the handling mechanism of Fig. 3A;
  • FIG. 3D is yet another view of the handling mechanism of Fig. 3A;
  • Fig. 3E is a bottom plan view of a linkage of the handling mechanism of Fig. 3A;
  • Fig. 3E1 is an enlarged view of a portion of Fig. 3E;
  • Fig. 3F is a top plan view of the linkage of Fig. 3E;
  • FIG. 3G is yet another view of the handling mechanism of Fig. 3A;
  • FIG. 3H is yet another view of the handling mechanism of Fig. 3A;
  • FIG. 4A is a perspective view of a multiple loading mechanism of the fusion system of Figs. 1A and 1 B;
  • Fig. 4B is a perspective view of drawers of the multiple loading mechanism of Fig. 4A;
  • Figs. 5A and 5B are respectively a side elevation view and a perspective view of the handling mechanism of Fig. 3A and the drawers of Fig. 4B, shown in a first configuration
  • Figs. 5C and 5D are respectively a side elevation view and a perspective view of the handling mechanism of Fig. 3A and the drawers of Fig. 4B, shown in a second configuration
  • Figs. 5E and 5F are respectively a side elevation view and a perspective view of the handling mechanism of Fig. 3A and the drawers of Fig. 4B, shown in a third configuration;
  • Figs. 5G and 5H are respectively a side elevation view and a perspective view of the handling mechanism of Fig. 3A and the drawers of Fig. 4B, shown in a fourth configuration;
  • FIGs. 6A to 6C are three dimensional views of a loading mechanism in accordance with another embodiment for the fusion system of Figs. 1 A and 1 B.
  • a fusion system for the preparation of inorganic analytical samples is disclosed.
  • the fusion system includes a furnace operable to receive containers such as crucibles therein for heating the contents of the containers in order to prepare a fused mixture for analysis.
  • An inorganic sample is solubilized in a fused flux to obtain a fused mixture (also referred to as a sample herein, or as a fused sample) suitable to prepare analytical samples.
  • the analytical sample can be a glass disk for X-ray fluorescence (XRF) analysis, a solution for inductively coupled plasma (ICP) analysis or a solution for atomic absorption (AA) analysis, to name some examples.
  • XRF X-ray fluorescence
  • ICP inductively coupled plasma
  • AA atomic absorption
  • the fusion system can include a furnace having heating element(s), and a sample holder operable to support a plurality of containers such as crucibles in which the fused mixture can be generated or such as moulds in which the fused mixture can be solidified.
  • the furnace has an enclosed heating chamber.
  • the heating elements can be operated to increase the temperature within the heating chamber, which can be referred to as pre-heating the heating chamber, before introducing the sample holder and the crucibles into the heating chamber.
  • the heating elements may be operated only when the sample holder and the crucibles are in a heating position.
  • the sample can stay in the crucible (e.g. mouldable or peroxide application).
  • the samples can be transferred from the crucibles to other containers prior to cooling, and the analytical samples thereby obtained can be operable to sustain subsequent analysis.
  • Such other containers can be moulds in the case of XRF analysis to obtain glass disks, or beakers containing an acidic solution for ICP and/or AA analysis, to name some examples.
  • fuse refers to the process of dissolving material into flux in order to prepare a homogeneous, or near-homogeneous, mixture.
  • material being fused generally includes a fusion flux compound or a mixture of several fusion flux compounds, such that the material to be analyzed can be solubilized upon fusion of the flux material.
  • the flux material is a borate compound.
  • the process may be referred to as a “borate fusion” process.
  • the borate fusion process can include various steps that can be implemented using the fusion system.
  • the borate fusion process can include the following steps:
  • Commonly-used borate flux materials may be selected from the group consisting of lithium tetraborate (U2B4O7), lithium metaborate (LiBCh), sodium tetraborate (Na2B4O?) and combinations thereof, however it will be appreciated that other flux materials could be used and the present disclosure is not limited to use of the flux materials specifically identified herein.
  • the choice of flux material typically depends on the composition of the sample to be analyzed.
  • Additives can optionally be added to the flux material to modify their properties or to help oxidize partially oxidized elements that can be present in a sample to be analyzed.
  • additives that can be added include the following:
  • absorbers such as La2C>3, BaCh or SrO can optionally be added to decrease the matrix effect by increasing X-ray absorption of the flux;
  • fluidizers such as LiF can optionally be added for potentially better transfer of the fused mixture into the mould when preparing an analytical sample for XRF analysis;
  • oxidizing agents such as NH4NO3, NaNCh, KNO3, LiNCh or Sr(NOs)2 can optionally be added to oxidize non-oxidized and/or partially-oxidized inorganic compounds that may be present in the sample to be analyzed; and/or
  • non-wetting agents such as NaBr, LiBr, KI, Csl, NH4I or Lil can optionally be added to reduce stickiness to the crucible and allow easier casting.
  • oxidizing temperature also referred to herein as a “pre-heating temperature”
  • the oxidizing (or pre-heating) temperature can be set between 150°C and 1000°C.
  • the pre-heating of the flux material/oxidizer/sample mixture can be performed at a temperature that decomposes the ammonium nitrate into NO2 and HNO3. At least one of these gases can then oxidize the nonoxidized and/or partially-oxidized inorganic elements present in the mixture.
  • a slow decomposition of the oxidizer occurs, as a slow decomposition typically allows for a longer action of the oxidizer on the nonoxidized and/or partially-oxidized inorganic elements present in the mixture.
  • a “slow decomposition” can for example be triggered by first subjecting the flux material/oxidizer/sample mixture to a first temperature that is lower than the temperature of the main fusion step in the heating chamber. The decomposition of the oxidizer can then occur slower at the first temperature than if it had occurred directly at the fusion temperature. Subsequent oxidizing action on the nonoxidized and/or partially-oxidized inorganic elements are prolonged when performed at the first temperature compared to instances where the flux material/oxidizer/sample mixture is directly subjected to the fusion temperature.
  • a peroxide flux material for example, sodium peroxide Na2C>2.
  • the mixture in the crucible can be heated between 450°C and 650°C with agitation until the peroxide flux melts and the inorganic analytical sample dissolves homogeneously in the fused peroxide flux.
  • the material to be analyzed can include various inorganic materials (also referred to as mineral materials).
  • inorganic materials that can be subjected to the borate fusion process include cement, lime, carbonate, ceramic, glass, slag, refractory material, mining and geological materials, silicate, clay, ores, sulfides, fluorides, bauxite, aluminum, metal-based catalysts, steel, metals, ferroalloys, non-ferrous alloys and mineral/inorganic impurities contained in organic compounds such as polymers or pharmaceutical products.
  • preparing an analytical sample may include the steps of mixing an inorganic sample with a flux material, heating the mixture until the flux material melts and the inorganic sample dissolves into the fused flux material to obtain a fused mixture (sample).
  • flux fusion include the “borate fusion” and the “peroxide fusion” examples evoked above.
  • FIGs. 1A-1 E an example of a fusion system 10 is depicted including a furnace 100 for generating heat.
  • the furnace 100 includes a heating chamber 110 provided with heating element(s) 120 (seen in Fig. 1 D).
  • the heating chamber 110 is an internal volume of the furnace 100 that is delimited by heating chamber walls 1 12.
  • the heating chamber walls 1 12 are interconnected at right angles to form a single, cube-shaped heating chamber 1 10.
  • Other arrangements of the heating chamber walls 112 are possible, and thus so are other shapes for the heating chamber 110.
  • one of the heating chamber walls 112 has a door 114.
  • the door 1 14 can open and close relative a doorway, preferably in a fully or partially automated manner, to provide selective access to the heating chamber 110 through the doorway, as described in greater detail below.
  • the door 114 can be maintained in a closed state during agitating and fusing.
  • the door may include a transparent or translucent section, such as a window, to provide visual access to the heating chamber and allow a person to view the fusion process.
  • the heating chamber wall 112 formed by the door 114 is the only heating chamber wall movable portion, the other heating chamber walls remaining fixed relative to one another throughout operation.
  • the door 114 is a sliding body which translates in the vertical direction to expose the heating chamber 110 and to close it to thereby help thermally insulate or isolate the heating chamber 110 from the environment outside ofthe furnace 100 during the heating step.
  • Other configurations of the door 114 are possible.
  • the door may open and close by pivoting relative to a hinge, or the door may translate in a generally horizontal direction (in the example embodiment, the movement is slightly oblique from horizontal).
  • available space may be limited or costly, and in some embodiments, using a sliding door rather than a hinged door may help limiting the footprint of the equipment.
  • the heating chamber walls and door may be omitted, and the fusion area may not be enclosed within heating chamber walls.
  • the heating elements are in the form of fuel nozzles and operate via combustion, the heat may be sufficiently localized onto the crucibles to avoid the necessity of enclosing the crucibles in walls during the fusion operation, and the fusion area may be in the vicinity of such fuel nozzles.
  • the sample support, crucibles, samples and/or moulds or other containers may be at a significantly lower temperature, such as room temperature, at the time of engagement into the heating chamber.
  • a temperature drop may occur at the time of engaging the sample support(s), crucibles, samples and/or moulds or other containers, into the heating chamber.
  • Such a diminution in temperature may be caused by the opening and closing of the door, and may additionally be caused by absorption of heat from the heating chamber by the sample support, crucibles, samples and/or moulds or other containers.
  • the minimal mass that needs to be placed in the heating chamber 110 is the containers (e.g. crucibles) in which the samples (e.g.
  • the samples may be transferred into other containers (e.g. mould, beaker) after fusion, and it can be required to heat such other containers to the same temperature and therefore move it into and out from the heating furnace together with the samples. Accordingly, the minimal mass may further include such other containers and any support or holder therefore.
  • Another factor that may have an impact on returning to or otherwise achieving the temperature set-point is heat loss through/via any opening across heating chamber walls, such as an opening 116 through which the containers are inserted and subsequently received, as described in greater detail below.
  • openings in the heating chamber walls 112 may be needed for different reasons including managing the chemical fumes produced during the fusion process, to insert the heating element(s) 120, and more. All these openings may have an impact on the temperature distribution/uniformity inside the heating chamber 110 and therefore may have an impact on the heat transfer to the samples.
  • the fusion system has a particular combination of a plurality of features including a handling mechanism 200 (seen in Figs. 1 B and 1 C), an agitation mechanism 300 (seen in Fig. 1 D), a sample holder 12 (seen in Figs. 2A and 2B ), a pouring mechanism 500, and a multiple loading mechanism 400 (seen in Fig. 4B).
  • a handling mechanism 200 (seen in Figs. 1 B and 1 C)
  • an agitation mechanism 300 (seen in Fig. 1 D)
  • a sample holder 12 aseen in Figs. 2A and 2B
  • a pouring mechanism 500 a multiple loading mechanism 400
  • a multiple loading mechanism 400 (seen in Fig. 4B).
  • all these mechanisms, together with the heating chamber are enclosed in an outer housing 15, seen in Fig. 1 , which may be useful both for health and safety reasons and for giving the system an agreeable finished appearance for instance.
  • Different embodiments can have one or
  • the outer housing 15 may include a safety door 15A.
  • the safety door 15A may include a transparent portion for inspection purposes.
  • the safety door 15A may pivot about an axis A1 .
  • the safety door 15A may be opened for cleaning or other operation that may be performed to internal components of the furnace 100.
  • the handling mechanism 200 can have a support 210 operable to carry one or more sample holder(s) 12 as the handling mechanism 200 moves the sample holder(s) 12 throughout different steps of the fusion process.
  • one (or more) sample holder(s) 12 is provided in the form of a component distinct from both the handling mechanism 200 and the agitation mechanism 300.
  • the sample holder 12 can have a plurality of containers which can be either separable from or integrated with the sample holder.
  • more than one sample holder 12 can be provided, such as a first sample holder 12 in which the containers are crucibles and a second sample holder in which the containers are moulds or beakers.
  • the sample holder(s) 12, the handling mechanism 200, and the agitation mechanism 300 can be operable forthe handling mechanism 200 to carry the sample holder(s) via a support as it moves the sample holder(s) into the furnace 100, while a door of the furnace is open, for the handling mechanism 200 to engage the sample holder 12 with the agitation mechanism 300 and to then move the support 210 out from the furnace 100, without the sample holder 12, after which the door can close.
  • the agitation mechanism 300 can agitate the sample holder 12, with the samples contained therein, during the fusion process.
  • the handling mechanism 200 can move the support back into the furnace, disengage the sample holder from the agitation mechanism 300, and move the sample holder 12 out from the furnace.
  • the handling mechanism 200 can further be operable to move a first sample holder 12 having the samples into engagement with a pouring mechanism 500, and then disengage from the first sample holder 12.
  • a second sample holder having moulds or beakers can also be provided.
  • the pouring mechanism 500 can then pourthe samples into the moulds by pivoting the first sample holder 12 around a horizontal axis.
  • the handling mechanism 200 can then remove the first sample holder 12 from the pouring mechanism 500.
  • the handling mechanism 200 can move the samples to an optional, dedicated cooling station 170 to expose the samples to a stream of cool air to accelerate cooling.
  • the multiple loading mechanism 400 can have two or more loading stations for sample holders, and the handling mechanism 200 can be operable to allow to selectively put or remove one or more sample holders from either one of the loading stations in a manner that the loading stations can be loaded or unloaded independently from one another.
  • the step of putting the sample holder into a loading area, directly onto the support of the handling mechanism, or putting samples into a sample holder which is in a loading area or supported by a handling mechanism can be referred to herein as “loading” and the step of removing the sample holder from a loading station, from the support, or of removing solid samples from a sample holder which is in a loading station or on a support, can be referred to herein as “unloading”.
  • any or all of these features, as well as functions associated to the operation of the furnace itself such as the opening and closing of the furnace door and/or activation and deactivation of heating elements, for instance, can include hardware operable to be controlled in a fully or partially automated manner.
  • the fusion system 10 can have hardware which will be referred herein as a controller 20.
  • the controller 20 can be operable to perform functions in a partially or fully automated manner.
  • the controller can include a computer, i.e. in the form of a combination of hardware and software elements, or more purely in the form of hardware elements such as electronics.
  • hardware can include logic gates included as part of a silicon chip of the processor.
  • Software can be in the form of data such as computer-readable instructions stored in the memory system. Alternately, hardware can be based more mainly on solid state electronic elements.
  • the expression computer as used herein is not to be interpreted in a limiting manner. It is rather used in a broad sense to generally refer to the combination of some form of one or more processing units and some form of non-transitory memory system accessible by the processing unit(s).
  • the use of the expression computer in its singular form as used herein includes within its scope the combination of two or more computers working communicatively coupled in a manner to collaborate to perform a given function.
  • the expression “computer” as used herein includes within its scope the use of partial capacities of a processing unit of an elaborate computing system also operable to perform other functions.
  • the expression “controller” as used herein is not to be interpreted in a limiting manner but rather in a general sense of a device, or of a system having more than one device, performing the function(s) of controlling one or more devices.
  • the controller 20 can include a computer 180 such as shown in Fig. 1 E, having a processor 182 and a non-transitory memory 184 with functions defined in the form of software instructions 186 stored in the non-transitory memory.
  • the controller 20 can further include a plurality of I/O interfaces 188 such as wired or wireless connections to a display screen, a touchpad or touchscreen, a keypad, a wired or wireless communications module, and a visual or audible alarm unit, to name a few examples.
  • I/O interfaces 188 such as wired or wireless connections to a display screen, a touchpad or touchscreen, a keypad, a wired or wireless communications module, and a visual or audible alarm unit, to name a few examples.
  • a controller 20 can be used to control, and fully or partially automate, various phases of the overall process or cycle associated with fusion of the samples for various reasons, such as safety, or productivity. Indeed, each phase of the process, whether putting the samples onto the handling mechanism 200, putting the samples onto the agitation mechanism 300, performing the fusion, removing the samples after the fusion, pouring the fused mixture from crucibles into moulds, and/or cooling the samples, for instance, can take a certain amount of time which can cumulatively add up in defining an overall cycle duration, and reducing cycle duration can be a significant factor in increasing the productivity of a given fusion system.
  • the automated or semi-automated movement of hardware components can be based on feedback from one or more sensors, for instance (e.g. servomotor, proximity sensors), or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from one or more sensor, which can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller for instance (e.g. handling mechanism is blocked, or has not reached a given intended position).
  • Such an alarm can be in the form of a visual and/or audible indicator, e.g. triggerthe activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm for instance.
  • the controller 20 can be connected to actuators of the door 114 in a manner to control the opening and closing of the door 114 in a partially or fully automated manner. This control can be performed in a timed manner with the control of other mechanisms, such as the handling mechanism 200, the heating elements 120, and/or the agitation mechanism 300 for instance.
  • One or more door sensors can further be included within the fusion system 10 and communicatively coupled to the controller. Such sensors can include hardware and/or software elements, and can be operable to allow the controller to confirm intended operation of the door (e.g.
  • Such a determination or indication at the controller can be used by the controller in various ways, such as trigger the generation of a visible or audible indication (e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm), and/or be used as a condition for allowing the accomplishment of further automated steps (e.g. the handling mechanism 200 will be controlled by the controller to penetrate into heat chamber only if the door is confirmed to have been successfully opened, or the heating elements 120 will be controlled by the controller to activate/generate fusion heat only if the door is confirmed to have been successfully closed).
  • trigger the generation of a visible or audible indication e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm
  • the handling mechanism 200 will be controlled by the controller to penetrate into heat chamber only if the door is confirmed to have been successfully opened, or the
  • the heating element(s) 120 can be operable to generate heat and raise the temperature of the heating chamber 110.
  • the heating element(s) 120 include multiple heating elements 120 which are at least partially disposed within the heating chamber 110.
  • the heating elements 120 are spaced apart from one another in a first lateral direction D1 .
  • the heating elements 120 are elongated bodies extending in an upright or vertical direction D2 that is transverse to the first lateral direction D1.
  • the heating elements 120 are resistive and generate heat resulting from resistance to an electrical current flowing through the heating elements 120.
  • the furnace 100 is a resistive-heating furnace.
  • the heating can be provided by fuel combustion rather than electrical resistance, for instance.
  • the one or more heating elements 120 can be controlled by the controller 20 in a fully or partially automated manner.
  • the heat element control process can be based on feedback from one or more temperature sensors located in the heating chamber, for instance, or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a temperature sensor, which can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller for instance.
  • Such an alarm can be in the form of a visual or audible indicator, e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm for instance.
  • the temperature of the heating chamber 110 is a factor in the fusion process, such that it may be desirable for the heat transfer to the crucibles holding the samples to be uniform and properly distributed throughout the heating chamber 110. This may be achieved by controlling the size and placement of any openings leading to the heating chamber 110 so as to control the airflow inside the heating chamber 1 10. This may also be achieved by spacing the heating elements 120 in a desired arrangement, such that the crucibles containing the samples are placed in such a way that the distance between the heating elements 120 and the crucibles is uneven.
  • the heating elements 120 include two peripheral heating elements 122 which are disposed furthest from each other in the first lateral direction D1 and which are spaced closest to opposite heating chamber walls 112.
  • the heating elements 120 include two middle heating elements 124 positioned adjacent to each other and in between the peripheral heating elements 122 relative to the first lateral direction D1 .
  • the spacing between the heating elements 122,124 in the first lateral direction D1 is not consistent.
  • the spacing in the first lateral direction D1 between each peripheral heating element 122 and its nearest middle heating element 124 is greater than the spacing in the first lateral direction D1 between the two middle heating elements 124.
  • the spacing in the first lateral direction D1 is smallest between both heating elements 124 nearest to the centre of the heating chamber 110.
  • Another way of addressing uniformity of temperature in the heating chamber 110 is by providing heating elements which are evenly or unevenly interspaced from one another, but which are powered at different levels of electrical power to compensate for any element of the system’s construction which may otherwise lead to unsatisfactory heat distribution within the heat chamber during cooling.
  • the heating element(s) 120 may generate heat for the heating chamber 1 10 by combusting a fuel, such as gas.
  • the heating element(s) 120 may include a combustor, one or more opening(s) in the heating chamber walls 112 through which hot air is admitted, and/or an exhaust for evacuating the hot combustion gases away from the heating chamber 1 10.
  • an enclosure specifically delimiting a heating chamber may not be present, and the crucibles (and potentially the moulds as well) can be exposed directly to a specifically oriented flame during heating in a broader area such as a room in a building.
  • the fusion system 10 may be described as a gas fusion system 10, or a gas fluxer.
  • the furnace 100 has only one heating element 120.
  • the heating element(s) 120 have a horizontal orientation when extending through the heating chamber 110. It will thus be appreciated that the configuration of the heating element(s) 120 may vary, provided that it/they achieve the function of heating the fusion area.
  • the opening 116 can be provided in the form of an archway which is temporarily made accessible to allow for the passage of the support 210 and the sample holder 12 into and out of the heating chamber 110, and which is closed off or inaccessible when the support 210 is outside of the heating chamber 110.
  • the opening 116 is formed or is accessible when the door 1 14 is in an open position, and the opening 116 is closed or inaccessible when the door 114 is in a closed position.
  • the support 210 is capable of displacing into, and retracting from, the heating chamber 110 via the opening 116.
  • the support 210 is thus operable to pass through at least one of the heating chamber walls 112 defining the heating chamber 1 10.
  • the handling mechanism 200 can be fully retracted out from the heating chamber 1 10 during fusion and not be used for holding, supporting, or agitating the sample holder 12 during the fusion phase.
  • the mass which is moved into the fusion area of the furnace, heated to the desired temperature for fusion, and subsequently moved out from the fusion area in a manner to improve temperature stability within the furnace, reduce fusion time, or both.
  • the mass which is moved into and out from the fusion area can be associated to the mass which absorbs heat from the furnace, and reducing this mass may directly reduce the amount of heat which needs to be supplied by heating elements to achieve a given temperature.
  • One way of reducing this mass is to provide a sample holder which is relatively minimalist in terms of mass and a handling mechanism which has a base located outside the fusion area, but which can move the sample holder into and out from the fusion area, and which can be entirely retracted out from the furnace (fusion area) during the fusion operation in a manner to avoid contributing to the mass which is to be heated.
  • an agitation mechanism 300 which has hardware elements which are entirely distinct from hardware elements of the handling mechanism 200, can be associated with the fusion area, and the handling mechanism 200 can be further operable to engage the sample holder 12 with the agitation mechanism 300 prior to fusion, and to disengage the sample holder 12 from the agitation mechanism 300 subsequently to fusion.
  • samples e.g. inorganic sample and flux
  • the containers can be separable from the sample holder 12, or integral to the sample holder 12 depending on the embodiment.
  • the sample holder 12 can be put onto a support 210 of the handling mechanism 200.
  • the handling mechanism 200 can be operable to move the support 210 into and out from a fusion area of the furnace 100.
  • the handling mechanism 200 can be operable to move the support 210 towards and away from a base of the handling mechanism, and the base of the handling mechanism can be located outside of the fusion area, e.g. outside the furnace 100.
  • the support 210 can carry the sample holder 12 while the handling mechanism 200 moves the support 210 and the sample holder 12.
  • the handling mechanism 200 can engage the sample holder 12 with the agitation mechanism 300, at which point it (the support 210) can simultaneously disengage from the sample holder 12, and then move out from the fusion area.
  • the furnace 100 can be activated to generate heat which fuses the samples, which can involve generating heat to reach, maintain, or return to a certain temperature set point for instance, and the agitation mechanism 300 can agitate the samples during the fusion.
  • the handling mechanism via support 210) can disengage the sample holder 12 from the agitation mechanism 300, and move the sample holder 12 out from the furnace 100, to a location where they can be cooled and/or picked up by an operator.
  • a door of the furnace can be opened prior to the moving of the support 210 into the fusion area, be kept open during the engagement of the sample holder 12 with the agitation mechanism 300 and the moving of the support 210 out from the fusion area, closed during the fusing, and reopened for the steps of moving the support 210 back into the fusion area, disengaging the sample holder 12 from the agitation mechanism 300, and moving the sample holder 12 out from the fusion area.
  • Such process steps can be fully or partially automated via a controller 20, which can contribute to reducing the duration of the process steps and/or facilitating the coordination between the action of the door, the action of the handling mechanism 200, and the action of the agitation mechanism 300.
  • Engaging the sample holder 12 with the agitation mechanism 300 can involve lowering the sample holder 12 onto the agitation mechanism 300 whereas disengaging the sample holder 12 from the agitation mechanism 300 can involve raising the sample holder 12 from the agitation mechanism 300, as will be exemplified below.
  • the handling mechanism 200 can be provided in the form of an assembly of components which function/cooperate together to achieve the function of handling the sample holder 12.
  • the handling mechanism 200 has a support 210 which is operable to support the sample holder 12 while the sample holder 12 is displaced into and out from the fusion area such as can be enclosed by a heating chamber 110.
  • the support 210 can further support the sample holder 12 while the sample holder 12 is moved to or from other locations, such as a loading area, cooling area (e.g. cooling station 170) and a pouring station 500, depending on the details of the specific embodiment.
  • Some components of the handling mechanism 200 remain permanently outside of the heating chamber 110, as explained in greater detail below.
  • the support 210 can be moved into and out from the heating chamber 1 10.
  • the support 210 only temporarily remains within the heating chamber 1 10, for the purpose of putting or removing the sample holder 12 in/from the heating chamber 1 10.
  • the support 210 is not present in the heating chamber 110 during the fusing of the sample orwhen heat is being generated by the heating element(s) 120. By remaining outside of the heating chamber 1 10 while heat is generated, the mass of the support 210 does not contribute to absorption of heat energy during the heating step which can help to reduce the time forthe heating chamber 110 to achieve or recover its desired or set-point temperature once the sample holder 12 and the samples have been loaded therein.
  • the support 210 may take any suitable form or be any suitable arrangement of components to achieve its function, and at least one possible configuration for the support 210, operable here specifically to collaborate with the particulars of the sample holder 12 and with the particulars of the agitation mechanism 300 of the illustrated embodiment is described in greater detail below.
  • the handling mechanism 200 can be controlled by the controller 20 in a fully or partially automated manner.
  • the handling mechanism control process can be based on feedback from one or more sensors, for instance (e.g. servomotor, proximity sensors), or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a handling mechanism sensor, which can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller for instance (e.g. handling mechanism is blocked, or has not reached a given intended position).
  • Such an alarm can be in the form of a visual and/or audible indicator, e.g.
  • the handling mechanism control process can be coordinated with other control processes such as a door control process, a pouring mechanism control process, a cooling station control process and/or an agitation mechanism control process.
  • the door can be controlled by the controller 20 in a fully or partially automated manner.
  • the door control process can be based on feedback from one or more sensors, for instance (e.g. servomotor, proximity sensors), or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a door sensor, which can be based on conditions defined in a set of instructions stored in the non- transitory memory of the controller for instance (e.g. handling mechanism is blocked, or has not reached a given intended position).
  • Such an alarm can be in the form of a visual and/or audible indicator, e.g.
  • the door control process can be coordinated with other control processes such as a handling mechanism control process, a heating element control process and/or an agitation mechanism control process.
  • the sample holder 12 can be operable to being selectively supported by either one of the handling mechanism 200 and the agitation mechanism 300 (and optionally via additional mechanisms such as a cooling station, a pouring mechanism 500, or a multiple loading mechanism 400).
  • the sample holder 12 can be operable to be transferred from one mechanism to another in an automated manner which, in this specification, can be referred to as engaging or disengaging the sample holder 12 with the corresponding mechanism by action of the handling mechanism.
  • the sample holder support and transfer scheme can be based on upright rods having terminal ends used for selectively supporting the sample holder by a corresponding one of the mechanisms, and the sample holder having corresponding sockets operable to be engaged by the terminal ends of the rods.
  • the sample holder 12 can have containers which can be removably nested within corresponding ones of container receptors. More specifically, different types of containers can be sized in a manner to fit container receptors, such as crucibles, moulds, beakers, etc. In other embodiments, different models of sample holders can be associated to different kinds of separable containers. In still another embodiment, the containers can be integrated to the sample holder. In the embodiment illustrated, the sample holder engagement scheme can be based on upright rods having terminal ends used for selectively supporting the sample holder, and the sample holder having corresponding sockets (e.g.
  • the sockets can be mounting apertures and can be opened (e.g. through apertures) or closed.
  • the sockets can be male and the terminal ends can be female.
  • the terminal ends of the rods can be tapered, e.g. conical, pyramidal, truncated conical or truncated pyramidal, whereas in other embodiments other mating shapes between the rods and sockets can be used. It will be appreciated that other configurations of the sockets and rod engagement schemes are possible.
  • the agitation mechanism can have a plurality of upwardly oriented agitation rods, and the sample holder can be provided with a first set of upwardly oriented sockets operable to receive terminal ends of the agitation rods.
  • the handling mechanism and more specifically the support, can have a plurality of upwardly oriented handling rods, and the sample holder can have a second set of sockets operable to receive terminal ends of the handling rods.
  • the direction of movement into and out from the fusion area can be characterized as of horizontal and longitudinal orientation, in which case the handling rods and the second set of sockets can be characterized as horizontally and laterally offset from the agitation rods and the first set of sockets, for the agitation rods to be out from interference with the longitudinal displacement of the handling rods.
  • the handling rods can be supported by corresponding, longitudinally oriented prongs of the support, which can be directed towards the fusion area.
  • Fig. 1 D presents further details of an example of an agitation mechanism 300 operable to receive the sample holder 12 from the support 210 of the handling mechanism 200 and for agitating the sample holder 12, and thus the samples, independently of the handling mechanism 200, during the fusion phase.
  • the engagement of the sample holder 12 with the agitation mechanism 300 which can be provided here by vertically lowering the sockets into engagement with the terminal ends of the rods, allows the sample holder 12 to be fully supported by the agitation mechanism 300, thereby allowing the support 210 of the handling mechanism to be thereafter moved out from the heating chamber 110.
  • the sample holder 12 with the containers and any samples contained therein are deposited inside the heating chamber 110 on a feature of the agitation mechanism 300 which remains inside the heating chamber 110 throughout a given instance of the fusion process.
  • the agitation mechanism 300 can agitate the sample holder 12 and the samples it contains while they are within the heating chamber 110, and while the heating element(s) 120 can be controlled in a manner to heat the heating chamber 110 or otherwise achieve a target temperature in the vicinity of the sample.
  • the agitation mechanism 300 may constitute of various collections or assemblies of components which function/cooperate together to achieve the function of agitating the sample during the fusing. At least one possible configuration of the agitation mechanism 300 is described in greater detail below.
  • the agitation mechanism 300 can be controlled by the controller 20 in a fully or partially automated manner.
  • the agitation mechanism control process can be based on feedback from one or more sensors (e.g. servomotors, motion detectors), for instance, or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a sensor associated to the agitation mechanism 300, which trigger can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller 20 for instance.
  • Such an alarm can be in the form of a visual and/or audible indicator, e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm for instance.
  • FIG. 2A a specific embodiment of a sample holder 12, a tray 12T which is operable to carry crucibles 12C, is presented.
  • the tray 12T has multiple apertures 12A (six are shown, but more or fewer apertures 12A are possible), each aperture 12A forming a container receptor operable to receive a corresponding crucible.
  • Fig. 2B shows the sample holder with the crucibles 12C received in the apertures 12A. More particularly, in this example embodiment, each crucible 12C has a crucible lip 12L which has a diameter larger than the diameter of the aperture 12A.
  • the crucible 12C may be placed into the aperture 12A, and the crucible lip 12L rests against part of the tray 12T so that the crucible 12C is supported by the tray 12T. Accordingly, in this embodiment, each crucible 12C is removably mounted to a corresponding sample aperture 12A of the tray 12T. Referring to Fig. 2B, all of the crucibles 12C are shown having the same shape and size. It will be appreciated that the crucibles 12C may have different shapes and may be any receptacle, vessel or container for supporting a sample to be fused. It will also be appreciated that the tray 12T may support containers of different shapes or configurations, such as moulds or beakers.
  • the tray 12T has mounting apertures 12M which are used to engage the sample holder with one or more mechanism(s) or station(s) of the fusion system 10.
  • the mounting apertures 12M include peripheral mounting apertures 12MP which are positioned at opposite extremities of the tray 12T.
  • the peripheral mounting apertures 12MP have a shape which is different from the shape of the other mounting apertures 12M.
  • the peripheral mounting apertures 12MP are obround (i.e. racetrack shaped with a rectangle aperture between two semi-circular apertures), whereas the other mounting apertures are circular, although it will be appreciated that other mounting aperture and peripheral mounting aperture shapes are also possible.
  • the handling mechanism 200 includes both a horizontal displacement mechanism, operable to move the samples into and out from the heating chamber along a longitudinally oriented ingress and egress path, when the door 114 is open, and an upright displacement mechanism, operable to move the samples along the vertical orientation.
  • a horizontal displacement mechanism operable to move the samples into and out from the heating chamber along a longitudinally oriented ingress and egress path, when the door 114 is open
  • an upright displacement mechanism operable to move the samples along the vertical orientation.
  • the expressions horizontal and upright are used here for simplicity, and it will be understood that the orientations can be partially oblique from horizontal or vertical in some embodiments while still being considered generally horizontal or generally upright.
  • the upright displacement mechanism may be omitted in some embodiments.
  • the upright displacement mechanism can be used to lowerthe sample holder 12 into engagement with the agitation mechanism 300, or raise the sample holder 12 out from engagement with the agitation mechanism 300, while the horizontal displacement mechanism can be used to move the support, with or without the sample holder, into and out from the fusion area.
  • the handling mechanism can be operable to move and transfer the sample holder(s) with a support 210.
  • the support can also have upwardly oriented rods, which can be referred to as handling rods for instance.
  • the sample holder can have distinct sets of sockets, such as a first set of sockets operable to receive the agitation or fixed support rod terminal ends, and a second set of sockets operable to receive the handling rods.
  • the sockets of the second set can be laterally offset from the sockets of the first set, as the handling rods can be laterally offset from the agitation or fixed support rods to provide for the step of transferring the sample holder from the handling mechanism to the agitation mechanism or support rods for instance.
  • the handling rods can be brought into an interspersed configuration (i.e. with one or more handling rods being between agitation rods or vice-versa) with the agitation rods (or fixed support rods), with the sample holder being above the agitation rods (or fixed support rods), and then the support of the handling mechanism can be brought down to place the first set of sockets into engagement with the agitation rods (or fixed support rods), and disengage the second set of sockets from the handling rods, at which stage the support can be withdrawn from the fusion area.
  • the handling rods can be secured to longitudinally oriented prongs directed towards the fusion area in a manner that neither the prongs, nor the handling rods, come into interference with the fixed support rods or agitation rods, but rather mesh with them when the support is moved into the fusion area.
  • the support 210 is operable to removably receive and support the sample holder 12.
  • the support 210 can further be operable to removably receive and support a second sample holder such as a mould holder if deemed useful in a given embodiment.
  • Different configurations of the support 210 are possible to achieve this function. For example, and referring to Fig.
  • the support 210 includes a crossbar 212C that extends between and connects a plurality of support arms 212AP, 212AC, 212AP that are transverse to the crossbar 212C and which extend outwardly therefrom, towards the fusion area.
  • the support arms 212AP, 212AC, 212AP are spaced apart along the length of the crossbar 212C.
  • the support arms 212AP, 212AC, 212AP include two peripheral support arms 212AP at opposite ends of the crossbar 212C, and a central support arm 212AC positioned between the peripheral support arms 212AP.
  • Each of the peripheral support arms 212AP, 212AP bears a plurality of holder support rods 212R, and more specifically a first support rod operable to receive the sample holder 12 and a second support rod operable to receive the second sample holder.
  • the holder support rods 212R are bodies which extend upright or vertically.
  • the holder support rods 212R each have a terminal attachment 212T.
  • the holder support rods 212R are spaced apart from each other.
  • the two holder support rods 212R do not have the same height, which is measured between the peripheral support arm 212BP and the terminal attachment 212T. A height of some of the holder support rods 212R is less than the height of other holder support rods 212R. More particularly, and referring to Fig. 3B, the holder support rods 212R include distal holder support rods 212RD which are positioned closest to a distal end of the peripheral support arm 212BP, and also include proximal holder support rods 212RP which are positioned closest to an end of the peripheral support arm 212BP nearest to the crossbar 212C.
  • the height of the distal holder support rods 212RD is greater than the height of the proximal holder support rods 212RP.
  • a positioning of terminal attachments 212T at different levels can correspond to a positioning of corresponding terminal attachments of support rods 117 and agitation rods 314 at different levels.
  • such a positioning of terminal attachments 212T at different levels can allow a certain amount of longitudinal overlap between corresponding sample holders and help in reducing a footprint of the fusion system for instance, or reducing the size of the heating chamber which can reduce heating costs.
  • terminal attachments 212T are conical or pointed ends of the holder support rods 212R.
  • the terminal attachments are surrounded by a flat annular seat portion, and are configured the same way as the terminal attachments of the agitation rods and of the support rods, though other configurations are possible.
  • the terminal attachments 212T of the distal holder support rods 212RD are operable to be inserted into two of the mounting apertures 12M of the tray 12T of the sample holder 12 (see Fig. 3A).
  • the mounting apertures 12M have a diameter that is smaller than the diameter of the distal holder support rods 212RD, such that the tray 12T with the samples is able to rest on the distal holder support rods 212RD and thereby be supported by the support 210.
  • the central support arm 212BC has a bracket 212D with bracket terminal attachments 212DT which are inserted into central mounting apertures 12MC of the tray 12T (see Figs.
  • the central support arm 12BC may also support the sample holder 12.
  • the proximal holder support rods 212RP may be used to support other containers into which the samples may be poured, as explained in greater detail below.
  • Other configurations of the terminal attachments 212T are possible provided that they allow for removably attaching the sample holder 12 to the support 210.
  • the sample holders 12 can be provided with different sets of mounting apertures in order to provide for the step of engaging or disengaging the sample holder 12 from the agitation mechanism 300 using the handling mechanism 200.
  • a first set of mounting apertures such as 12M for example, can be positioned at relative positions operable to engage with the distal support rods 212RD of the support 210 of the handling mechanism
  • a second set of mounting apertures such as 12MP for instance, can be positioned at relative positions operable to engage with the agitation rods 314 of the agitation mechanism 300.
  • the support 210 of the handling mechanism 200 can be operable to avoid interference with the agitation rods 314 of the agitation mechanism 300.
  • the support arms 212AP, 212AC, 212AP can be interspaced in a manner to correspond to the location of spacings between the agitation rods 314 ofthe agitation mechanism 300.
  • the support 210 of the handling mechanism 200 can be brought horizontally into the fusion area in a plane above the terminal ends of the agitation rods 314, and then be lowered in a manner for the terminal ends of the agitation rods 314 to pass between the prongs formed by the support arms 212AP, 212AC, 212AP of the handling mechanism 200 until the sample holder 12 becomes effectively supported by and engaged with the terminal ends of the agitation rods 314, at which point the prongs formed by the support arms 212AP, 212AC, 212AP can be horizontally withdrawn from the fusion area.
  • the prongs can become horizontally engaged between the agitation rods 314 via horizontal movement, and the support 210 of the handling mechanism 200 can then be raised to disengage the sample holder 12 from the terminal ends of the agitation rods 314 (by engaging mounting apertures 12M of the support with the terminal attachments 212T of the distal holder support rods 212RD), at which point the support 210 can be horizontally withdrawn bringing the sample holder 12 with it.
  • the handling mechanism can have a horizontal displacement mechanism 168 which is distinct from and can be operated in a coordinated manner, or independently from a vertical displacement mechanism.
  • the horizontal displacement mechanism 168 includes a linkage 220 extending between a horizontal displacement base and the support 210 which supports the sample holder 12.
  • the linkage 220 is selectively extendible and collapsible, in two opposite sides relative to the horizontal displacement base, and can traverse a “neutral” position illustrated in Fig. 3C. This ability can be useful in providing convenience and flexibility of operation, and potentially in limiting the footprint of the fusion system.
  • the two sides can be referred to as a proximal side and a distal side, referring to a point of view of an operator located in front of the fusion system for instance, with the proximal side being closer to the operator located in front of the fusion system and the distal side penetrating into the fusion area.
  • extending or collapsing the linkage 220 to or from the distal side can be used for moving the sample holder 12 into or out from the fusion area, whereas extending or retracting the linkage 220 to or from the proximal side, as shown in Fig.
  • 3D can be used for moving the sample holder 12 into or out from a sample loading area from where it can more easily be accessed by an operator, for instance.
  • reliability may be a significant design requirement, and a linkage 220 may block, which may be undesired.
  • Eventual blocking in the neutral position shown in Fig. 3C can be a particular concern. It was found that the horizontal displacement mechanism 168 can be designed in a manner to alleviate such concerns, as will now be detailed.
  • the linkage 220 is extendible to move the support 210 (with or without the sample holder 12) longitudinally and horizontally from the neutral position in a first direction T1 , into the heating chamber 1 10 via the opening 1 16 created by open door 1 14.
  • the linkage 220 is also collapsible to displace the support (with or without the sample holder 12) horizontally in a second direction T2 opposite to the first direction T 1 , back to the neutral position.
  • the linkage 220 is also expandable in the second direction T2 from the neutral position, which may be convenient for various reasons, such as the manual loading or unloading of the sample holder 12 from the support 210, or, if a multiple loading mechanism 400 is present in a given embodiment, engaging the multiple loading mechanism 400 for example.
  • Different configurations of the linkage 220 are possible, and an example of one possible configuration for the linkage 220 is now described.
  • the linkage 220 includes a plurality of linkage pairings 222.
  • Two linkage pairings 222 are shown in Figs. 3E and 3F, but more are possible.
  • the linkage pairings 222 are spaced apart laterally from each other in a direction transverse to the first and second directions T1 ,T2.
  • Each linkage pairing 222 has a driving link 224 that is pivotably connected to a driven link 226.
  • the driving link 224 and the driven link 226 of each linkage pairing 222 pivot relative to each other.
  • the driving link 224 is an elongated member which is actively actuated, i.e. to which motive force is applied, in order to expand and collapse the linkage 220.
  • the driven link 226 is an elongate member which responds to an input of force and motion from the driving link 224, in orderto extend and collapse the linkage 220.
  • a distal extremity of the driven links 226 is pivotably mounted to the crossbar 212C of the support 210, such that the support 210 is positioned at a distal extremity of the linkage 220.
  • the crossbar 212C is also a driven link in this linkage, as it constrains the location of the distal end of the driven links which can force to open the angle between driving link and the driven link when the driving link is pivoted.
  • the displacement of the driving links 224 of both linkage pairings 222 in the first pairing of rotational directions R1/R2 and in the second pairing of rotational directions R2/R1 can be coordinated such that the movement of both linkage pairings 222 is synchronized.
  • Each of the linkage pairings 222 may thus be said to form an “accordion-type” mechanism (referred to below as an accordion mechanism) for extending and collapsing the linkage 220.
  • the linkage 220 may also have other configurations.
  • the linkage 220 is an assembly of telescopic members which extend and collapse relative to another to displace the sample holder 12 in the first and second directions T1 ,T2.
  • an accordion mechanism may be operable to be deployable in both directions relative to its base whereas a telescopic member type may be deployable away from and back towards its base on one side of its base only.
  • each driving link 224 extends between a distal end 224A that is pivotably coupled to the driven link 226, and a proximal end 224B.
  • the proximal ends 224B remain permanently outside of the heating chamber 110, whereas the distal ends 224A may enter the heating chamber 110 when the linkage 220 is expanded into the heating chamber 110.
  • the base 251 of the horizontal displacement mechanism 168 can have fixed wheels 228 such as sprockets (or pulleys in an alternate embodiment), each of which is fixed relative to the base.
  • the fixed wheels 228 can be concentric with a pivot axis of the driving link 224.
  • the driven links 226 each have, at their proximal end, a fixed wheel such as a sprocket 240 which does not rotate relative to the corresponding driven link, and which is concentric with the pivot axis of the driven link 226 relative to the driving link 224.
  • the pivoting of the driving link 224 around the axis intersecting its proximal end is also perceived as a rotation of the sprocket 228 in the opposite direction, following the circulation of the chain 238 around its loop.
  • the presence of at least one chain 238 associated to a corresponding driving member can help in regulating the expansion and collapse of the overall linkage and avoiding that the crossbar 212 would become obliquely misaligned, and/or can help in ensuring that the crossbar 212 does not become blocked upon displacement across the neutral position.
  • the presence of a chain 238 and associated sprockets on each one of the two driving members can further be preferred to such end(s).
  • the belts and pulleys or equivalents can be used instead of chains and sprockets.
  • pivoting of the driving link around its proximal end can lead to a controlled extension or retraction of the distal end of the driven link in the T1 orT2 direction independently of the influence ofthe crossbar212C.
  • pivoting the driving link may not lead to pivoting of the driven link relative the driving link.
  • the presence of the loop element and wheels can control the pivoting of the driven link relative the driving link independently of the crossbar 212C, and in a potentially more reliable manner, especially if two loop elements are used on both linkage pairings and for movement across the neutral position, as this can help in avoiding un-symmetric mismatch between the linkage pairings.
  • the pivoting of the driving links in opposite rotational directions R1 ,R2 can lead to pivoting of the driven links 226 in corresponding opposite rotational directions.
  • the fixed wheels 228 and the horizontal movement base 251 can be positioned permanently outside of the heating chamber 110.
  • the driving link 224 may be driven to pivot in any suitable manner.
  • a motor output 230 of an electric motor 263 of the handling mechanism 200 can output a rotational drive to a drive belt 232.
  • the drive belt 232 is mounted about two belt wheels 234 and a tensioner wheel 236.
  • Each of the belt wheels 234 is collocated with one of the fixed wheels 228, such that the belt wheels 234 and driving links 224 rotate together about the same axis, and such that rotation of the belt wheel 234 causes rotation of the drive link 224.
  • the motor output 230 imparts a rotational drive to the drive belt 232, which in turn causes the belt wheels 234 and thus the drive links 224 to rotate in the rotational directions R1 ,R2.
  • each of the fixed wheels 228 is in the form of a sprocket which is meshed with a drive chain 238.
  • Each drive chain 238 is also meshed with a driven sprocket 240 at the distal end 224A of each driving link 224.
  • Each driven sprocket 240 is mounted to, and in fixed rotational relationship with, one ofthe driven links 226 so that rotation ofthe driven sprockets 240 causes rotation of the driven links 226 relative to the driving links 224.
  • each of the driving links 224 has a chain tensioner 242 whose position may be fixed along an elongated slot 244 that extends through each driving link 224 and along some of its length. Displacement of the chain tensioner 242 along the slot 244 allows for varying the tension of the drive chain 238.
  • the linkage 220 is shown in a neutral position, in which the driven links 226 are collapsed toward the driving links 224 and vertically overlap the driving links 224.
  • the linkage pairings 222 may expand in the first pairing of rotational directions R1/R2 in order to displace and expand the linkage 220 in the first direction T1 so as to displace the support 210 and the supported sample holder 12 as shown in Fig. 3B (e.g. to displace the support 210 and the supported sample holder 12 into a heating chamber).
  • the linkage pairings 222 may alternatively expand in the second pairing of rotational directions R2/R1 in order to displace and expand the linkage 220 away from the heating chamber 110 in the second direction T2 so as to displace the sample holder 12 toward a multiple loading mechanism as shown in Fig. 3D (e.g. to displace the support 210 and sample holder 12 away from a heating chamber into a multiple loading mechanism).
  • an example of an upright (e.g. vertical) displacement mechanism 250 is presented in greater detail.
  • the upright displacement mechanism 250 allows for adjusting the vertical position of the support 210, which, in this specific embodiment, is achieved via a vertical movement of the horizontal displacement mechanism 168, and more particularly of the support 210, thereby permitting adjustment of the vertical position of the sample holder 12 in potentially different phases of the fusion cycle.
  • the upright displacement mechanism 250 is connected to the base 251 of the linkage 220 (as shown in Fig. 3F) so as to vertically displace the linkage 220.
  • the upright displacement mechanism 250 may take any configuration to achieve the functionality ascribed to it herein.
  • the upright displacement mechanism 250 has at least one truck 252 or other slidable carrier that is mounted, via supports 254 of the truck 252, to the driving links 224 of the linkage 220.
  • the upright displacement mechanism 250 has at least one rail 256 or other sliding guide which has a vertical orientation and which is mounted to, or provided on, a fixed or immobile mounting bracket 258 of the upright displacement mechanism 250.
  • Two rails 256 are present on the mounting bracket 258 and spaced laterally apart in Figs. 3H and 3G, but more or fewer rails 256 are possible.
  • the mounting bracket 258 is mounted to, or part of, a structural or immobile component of the fusion system 10 (e.g. external walls of the furnace 100).
  • the upright displacement mechanism 250 has two electrical motors 259 and associated endless screw mechanisms mounted to laterally opposite sides of an upright displacement base 261 .
  • the motor 259 actuates a component such as an endless screw or wheel to cause the truck 252 to slide vertically along the rails 256, thereby displacing the truck 252 relative to the mounting bracket 258.
  • Vertical adjustment of the truck 252 causes a corresponding vertical movement of the linkage 220, and thus allows for vertically adjusting the sample holder 12 supported by the linkage 220.
  • the handling mechanism 200 allows for an up-down movement of the sample holder 12 (i.e. with the upright displacement mechanism 250), in addition to a forward-rear movement of the sample holder 12 provided by the linkage 220.
  • cooling of the sample down to solidify the sample into a solid analytical sample can be actively assisted in a manner to further reduce process duration.
  • the fusion system 10 can be provided with a dedicated, actively ventilated, cooling station.
  • a cooling station 170 can be provided outside the heating chamber 1 10, below the generally horizontal (potentially oblique) ingress and egress path taken by the handling mechanism as it carries the samples into or out from the heating chamber.
  • the handling mechanism 200 can be provided with movement capabilities in more than one orientation.
  • the handling mechanism 200 can be provided with horizontal movement capabilities for movement in the orientation of the ingress and egress path, and with vertical movement capabilities for movement between the cooling station 170 and the ingress and egress path.
  • the cooling station 170 in this embodiment, can include one or more ventilators 171 and one or more ducts 172 which can be operable to draw fresh, cool air from outside an outer housing of the fusion system 10 and conveying it and directing it onto the crucibles or moulds holding the samples in a manner to favor heat transfer from the samples and equipment into the flow of air and accelerate the cooling of the samples.
  • a dedicated cooling station may be omitted or located elsewhere, and a handling mechanism can be provided with only horizontal movement capabilities for instance.
  • the one or more ventilators may be controlled by the controller 20 in a fully or partially automated manner.
  • the ventilator control process can be based on feedback from one or more sensors associated to the handling mechanism 200 or to the cooling station, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a such a sensor associated to the cooling operation, which can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller for instance.
  • Such an alarm can be in the form of a visual or audible indicator, e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as yellow light alarm for instance.
  • the pouring step may be automated as a means of accelerating the overall cycle and increasing productivity.
  • the pouring step can be conducted prior to a step of solidifying the sample (e.g. passive or active cooling).
  • a pouring mechanism may be provided to this end. An example pouring mechanism will be detailed below with reference to Figs. 5A to 5J.
  • the fusion system can be provided with more than one loading station, which can be provided as an assembly referred to as a multiple loading mechanism 400.
  • a multiple loading mechanism 400 there can be a period of time associated to the fusion of samples. This period of time can be associated to the time it takes for the handling mechanism to take the sample holder from a loading area, move the sample holder onto the agitation mechanism, exit the fusion area/perform the fusing, move the sample holder from the fusing area back to the loading area, and can further optionally include time associated to a step of pouring and/or active cooling. In an embodiment such as described above, this period of time can be referred to herein as an automated cycle time.
  • the additional period of time can be added to the automated cycle time to determine an “overall” cycle time. For a given fusion system, it can be the overall cycle time which determines the productivity and reducing either the automated cycle time or the additional period of time can lead to improvements in productivity.
  • a multiple loading mechanism 400 can allow reducing or eliminating the additional period of time from the overall cycle time. Indeed, a multiple loading mechanism 400 can have more than one loading station in/from which samples and/or sample holder(s) are put/taken. Moreover, an embodiment having a multiple loading mechanism 400 can be provided with an amount of supports corresponding to the amount of loading stations, with one or more supports being associated to corresponding ones of the loading stations. Accordingly, while the automated cycle is being performed on a first batch of samples and the corresponding sample holder(s), any manual operation associated to the preparation of a second batch of samples and associated sample holder(s) can be performed independently of the automated cycle.
  • the handling mechanism can immediately go to the second loading station and move the second batch of samples along a second fusion cycle, independently of any action associated to retrieving the first batch of samples from the first loading station or reloading a batch of samples in the first loading station.
  • the duration associated to a lengthy process step such as cooling can be taken fully or partially out from the automated cycle time by leaving a first batch of samples at a cooling station while moving a second batch of samples from the second loading station to the fusion area, for instance.
  • Such actions, and associated hardware elements can allow to eliminate or reduce lag between batches and can therefore reduce overall treatment time and increase productivity.
  • the loading stations can be vertically arranged one above the other, with each loading station having a loading support operable to receive one or more sample holders (e.g. a loading support having a first loading attachment for receiving a crucible holder and a second loading attachment for receiving a mould holder).
  • the loading stations can be arranged in a manner to allow the prongs (formed by support arms) and crossbar, of the support to pass freely, while the handling rods reach a position at which the sample holder(s) can become engaged with a corresponding loading attachment.
  • Each loading station can be provided with a corresponding drawer, allowing the drawer to be drawn out to allow manual access to a given sample holder or set of sample holders.
  • each drawer can be provided with an actuator connected to a locking mechanism, and the actuators can be controlled selectively by a controller.
  • An example multiple loading mechanism 400 will be presented below.
  • the handling mechanism 200 can be operable to displace the support 210 into the heating chamber 110 to retrieve the sample holder 12 from the agitation mechanism 300 in the heating chamber 110, and to then displace/retract the sample holder 12 with the samples into the multiple loading mechanism 400.
  • the multiple loading mechanism 400 has a volume of space that is disposed outside of the heating chamber 110.
  • the volume which is associated to the multiple loading mechanism 400 is defined by multiple loading mechanism walls 412 which can assist in impeding ingress of contaminants or the like from the environment.
  • the loading mechanism walls 412 can form part of the outer housing 15.
  • the multiple loading mechanism walls 412 can be external to the furnace 100.
  • the multiple loading mechanism walls 412 are interconnected at right angles to form a single, box-shaped multiple loading mechanism 400.
  • the multiple loading mechanism 400 can be attached to, or protrude from, an otherwise relatively flat external side wall of the furnace 100. In this configuration, the multiple loading mechanism 400 may be accessed to retrieve samples or to reload the loading area with new samples to be fused.
  • Other arrangements of the multiple loading mechanism walls 412 are possible, and thus so are other shapes for the multiple loading mechanism 400.
  • Positioning the multiple loading mechanism 400 outside of the furnace 100 and displacing the support 210 between the multiple loading mechanism 400 and the heating chamber 110 allows for having a sample holder 12 in the heating chamber 110 while also having a separate sample holder 12 in the cooling area of the multiple loading mechanism 400.
  • Such a configuration may allow for starting preparation for a second fusion process with the separate sample holder 12 once the first sample holder 12 has been placed into the cooling area and is free of the heating chamber 110.
  • the multiple loading mechanism 400 and the handling mechanism 200 allow for having a sample holder 12 and samples which are cooling down while the other sample holder 12 with different samples is heating up in the heating chamber 1 10, which may increase productivity and the output of the fusion system 10.
  • the multiple loading mechanism walls 412 defining the internal volume of the multiple loading mechanism 400 are external to the furnace 100 and disposed outside of the heating chamber 1 10.
  • the multiple loading mechanism walls 412 are interconnected at right angles to form a single, box-shaped multiple loading mechanism 400.
  • One of the multiple loading mechanism walls 412, an upper or top wall in the illustrated embodiment, is transparent or includes a transparency 411 so that the internal contents of the multiple loading mechanism 400 may be viewed from outside of the multiple loading mechanism 400.
  • One of the multiple loading mechanism walls 412 has one or more opening(s) 414 therein though which one or more drawer(s) 416A, 416B may be inserted.
  • the number of openings 414 is equal to the number of drawers 416A, 416B in the illustrated embodiment, other configurations are possible, including a configuration where the number of opening(s) 414 is different from the number of drawer(s) 416A, 416B.
  • Each drawer 416A, 416B may have any desired configuration. For example, and referring to Fig.
  • each drawer 416A, 416B has a handle 416H that is fixedly mounted to an outer wall 416W.
  • the outer wall 416W may be flush with the multiple loading mechanism wall 412 defining the opening(s) 414 when the drawer is closed.
  • Each drawer 416A, 416B is slidable on rails or other guides mounted to an inner surface of the multiple loading mechanism walls 412 so that the drawer 416A, 416B may be displaced in a horizontal direction that is parallel to the first and second directions T1 ,T2.
  • each drawer 416A, 416B has walls or other structure which delimit an internal drawer volume 416V.
  • the door 114 of the furnace 100 may provide additional thermal insulation when closed.
  • Each drawer 416A, 416B may have other features as well.
  • the handling mechanism 200 is operable to displace the support 210 and the sample holder 12 containing the samples from the heating chamber 1 10 into the drawer volume 416V of the one or more drawer(s) 416A, 416B.
  • the drawer 416A or 416B is opened, e.g. either automatically via an actuator or by pulling on the handle 416H, the drawer volume 416V becomes accessible, allowing the samples to be retrieved from the drawer volume 416V and/or to reload the loading area with new material to be fused.
  • the two drawers 416A, 416B are positioned one on top of the other, or are disposed vertically one above another.
  • the handling mechanism 200 is operable to displace the support 210 to move the sample holder 12 to and from each of the drawers 416A, 416B.
  • the handling mechanism 200 may be operable to displace the support 210 from the heating chamber 1 10 and to deposit it into an upper, first drawer 416A, and may also be operable to displace the support 210 to retrieve a second sample holder 12 in the lower, second drawer 416B and to displace the second sample holder 12 into the heating chamber 110.
  • the support 210 may be able to vertically displace between the vertically-adjacent first and second drawers 416A, 416B via the upright displacement mechanism 250 of the handling mechanism 200 described above, and/or via another vertical displacement mechanism of the fusion system 10.
  • the multiple loading mechanism 400 may thus function as “storage location” into which multiple sample holders 12 may be loaded and retrieved.
  • the drawers 416A, 416B of the multiple loading mechanism 400 can allow for multiple sample holders 12 to be individually refilled or reloaded via separate access openings 414.
  • the functionality provided by the drawers 416A, 416B of the multiple loading mechanism 400 can allow for simultaneously having a sample holder 12 with samples in the heating chamber 1 10, and a separate sample holder 12 in a corresponding one of the drawers 416A, 416B. This may allow the fusion system 10 to begin a second fusion process once the samples from the first fusion process have been placed into the cooling area and out of the heating chamber 110.
  • one or more of the loading stations has a loading attachment 418.
  • the loading attachment 418 functions to receive the sample holder 12 from the support 210 of the handling mechanism 200 and to support the sample holder 12 within the loading area (provided here in the form of drawer volume 416V) independently of the support 210, so that the support 210 may be withdrawn from the loading area to be used for other purposes.
  • the loading attachment 418 includes an upper arm 418U and a lower arm 418L that is positioned vertically lowerthan the upper arm 418U.
  • the upper and lower arms 418U,418L each extend through the drawer volume 416V in a direction that is transverse to the first and second directions T1 ,T2.
  • Each of the upper and lower arms 418U,418L are operable to receive a separate sample holder 12.
  • each of the upper and lower arms 418U,418L has a corresponding set of support prongs 418P which are spaced apart from each other in the lateral orientation, i.e. along a length of the upper and lower arms 418U,418L.
  • Each of the support prongs 418P is shaped and sized to receive and support a bottom surface of the sample holder 12, such that the sample holder 12 may rest on the support prongs 418P and be supported by the upper and lower arms 418U,418L.
  • the loading attachment 418 includes a motion bracket 418B which extends between and connects adjacent ends of the upper and lower arms 418U,418L.
  • the motion bracket 418B is activated by gravity to cause the motion bracket 418B, the upper and lower arms 418U,418L, and the sample holders 12 supported by the upper and lower arms 418U,418L to rotate about an axis 418A, as described in more detail below.
  • a motorized lock system can be provided for locking and unlocking either one of the drawers.
  • the motorized lock system can be operated manually or in a fully or partially automated manner such as by control via the controller 20 for instance.
  • the drawers 416A, 416B can allow for selectively accessing or closing off a corresponding loading area. This may be achieved using different techniques. One such technique is described with reference to Figs. 5A to 5H. Referring to Figs. 5A and 5B, the support 210 carrying a first sample holder 12B1 and a second sample holder 12B2 is displaced by the handling mechanism 200 in the second direction T2 toward the drawer volume 416V of the drawer 416.
  • the first sample holder 12B1 may support multiple crucibles 12C.
  • the first sample holder 12B1 may thus be the tray 12T described above.
  • the second sample holder 12B2 may have or support containers 12R which contain samples which require cooling in the multiple loading mechanism 400, and which have recently been poured from the crucibles 12C into the containers 12R, as described in greater detail below.
  • the first and second sample holders 12B1 ,12B2 have been displaced by the weight of the crucibles 12C and moulds 12R respectively, to the upper and lower arms 418U,418L.
  • the crucibles and moulds are in the sample holders, their weight causes the holders to displace - get a slight tilt of the crucibles/holders); and the attachment arms can prevent them from falling when the drawer gets opened.
  • other means such as pins, could alternately be used to prevent them falling.
  • the support prongs 418P of the loading stations can be laterally interspersed with the corresponding handling rods.
  • the upper and lower arms 418U,418L support the first and second sample holders 12B1 ,12B2. More particularly, the support prongs 418P are contacting a bottom surface of the first and second sample holders 12B1 ,12B2, such that the first and second sample holders 12B1 ,12B2 are resting on the support prongs 418P and supported by the upper and lower arms 418U,418L. Referring to Figs. 5E and 5F, with the first and second sample holders 12B1 ,12B2 being supported by the upper and lower arms 418U,418L, the loading attachment 418 is able to rotate or pivot the first and second sample holders 12B1 ,12B2.
  • the weight of 12C and 12R cause the motion bracket 418B, the upper and lower arms 418U,418L, and the supported first and second sample holders 12B1 ,12B2 to rotate or pivot downwardly about their respective pivot axes. Once they have pivoted downwardly, each of the first and second sample holders 12B1 ,12B2 form a non-zero angle with the horizontal plane. While the first and second sample holders 12B1 ,12B2 are in their downwardly pivoted and supported position within the drawer volume 416V as shown in Figs. 5G and 5H, the support 210 can be displaced by the handling mechanism 200 in the first direction T1 away from the drawer to be used for other purposes. The drawer may subsequently be opened, and a technician may access the first and second sample holders 12B1 ,12B2 to retrieve cooled samples from the containers 12R, or to fill the crucibles 12C with new material to be fused in the heating chamber 110.
  • the multiple loading mechanism 400 can be controlled by the controller 20 in a fully or partially automated manner.
  • the multiple loading control process can be based on feedback from one or more sensors, for instance (e.g. servomotor, proximity sensors), or can be automated based on prior calibration, to name some examples.
  • the controller 20 can have a function to trigger an alarm based on an indication received from a sensor, which can be based on conditions defined in a set of instructions stored in the non-transitory memory of the controller for instance (e.g.
  • Such an alarm can be in the form of a visual or audible indicator, e.g. trigger the activation of a graphical user interface element on the display screen, or trigger a given level of alarm on a light tower indicator 22, such as an orange or red light alarm for instance.
  • FIG. 6A to 6C another embodiment of the loading mechanism is shown at 1400.
  • FIG. 6A-4B For the sake of conciseness, only features differing from the multiple loading mechanism 400 of Figs. 4A-4B are described below.
  • the loading mechanism 1400 includes a loader door 1401 that encloses a volume external to the furnace 100 and disposed outside the otherwise generally rectangular parallelepiped shape of the heating chamber 110.
  • the volume enclosed by the loader door 1401 will be referred to herein as an internal volume or a user-accessible area in that the user is able to access this internal volume to put or remove sample holders.
  • a top wall of the loader door 1401 may be transparent to allow an operator to view the inside of the loading mechanism 1400.
  • the loader door 1401 is pivotably mounted to the outer housing 15 of the fusion system 10. The loader door 1401 may therefore pivot about axis P1 (Fig. 6B) between a closed position depicted in Fig.
  • the loader door 1401 may rotate about a direction such that an upper wall of the loader door 1401 moves away from the outer housing 15 of the fusion system 10 when moving from the closed position to the open position.
  • the pivoting of the door into the open position gives access to the furnace 100.
  • an actuator 1402 such as a solenoid, is used to lock the loader door 1401 in the closed position.
  • the actuator 1402 is shown in Fig. 6B.
  • the controller may be operatively connected to the actuator 1402 to lock the loader door 1401 in the closed position when, for instance, the samples inside the internal volume of the loader door 1401 are too hot to be handled by an operator or when a fusion process is still on going.
  • a sensor 1403 may be operatively connected to the loader door 1401 and able to generate a signal to the controller, the signal indicative of whether the loader door 1401 is in the closed position or the open position.
  • the fusion system 10 includes a loading station 1410, in this embodiment the loading station 1410 is a single loading station, and the handling mechanism 200 is operable to pick up the sample holder(s) from the loading station 1410 to move the sample holder(s) to other locations within the fusion system 10.
  • the sample holder(s) may include samples.
  • the loading station 1410 is disposed in a fixed relationship with regards to the fusion system 10 and the outer casing 15. Put differently, the loading station 1410 is non-movable relative to the outer casing 15 and the furnace 100. The loading station 1410 protrudes from an otherwise relatively flat external side wall of the furnace 100.
  • the loader door 1410 is used to selectively allow access to the loading station 1410.
  • the loading station is enclosed by the loader door 1410 in the closed position of the loader door 1410 and is manually accessible to an operator in the open position of the loader door 1410.
  • the loading station 1410 includes beams 1410A and a sample support member 1410B secured to the beam and extending from one of the beams to the other.
  • the way the sample support member 1410B supports the sample holder may be the same as how the sample holder is supported in the cooling station 170 or by the agitation mechanism described herein above.
  • challenges associated to potential sample holder misalignment described above in relation with other sample holder supporting elements of the system may also arise in the context of the sample support member 1410B.
  • the sample holder may have a plurality of containers which can be either separable from or integrated with the sample holder [0164]
  • the samples may be laid on the sample support member 141 OB.
  • the beams 1410A may be mounted to a structure of the fusion system 10 and protrude outside the outer casing 15 as shown.
  • the handling mechanism 200 described above with reference to Figs. 3A-3H may also be used as a loading station, thus providing a second loading station as shown in Fig. 6C.
  • the handling mechanism 200 may have a loading position depicted in Fig. 6C and in which an operator may load or unload sample holder(s) from the handling mechanism 200.
  • the support 220 of the handling mechanism 200 extends outside of the otherwise generally rectangular parallelepiped shape of the furnace 100 and protrudes from an otherwise relatively flat external side wall of the furnace 100.
  • a vertical and longitudinal offset may be present between the loading station 1410 and the support 220 of the handling mechanism 200 so that the sample holder(s) 12 supported by both of the loading station 1410 and the support 220 of the handling mechanism 200 are both simultaneously accessible by the operator.
  • the fusion system 10 thus defines two positions for loading samples: a top load position and a bottom load position.
  • the top and bottom load positions may be referred to in the alternative as a first load position and a second load position.
  • the top load position is defined by the loading station 1410 of the loading mechanism 1400 while the bottom load position is defined by the handling mechanism 200 in the loader position.
  • the inverse may be possible in an alternate embodiment.
  • the bottom load position is the lowest loading/unloading position and in this position the samples are placed directly on the support 220 of the handling mechanism 200.
  • the bottom load position is available at the start before starting a fusion cycle and at the end when both fusion cycles are completed.
  • the bottom load position may also be available at other times when two cycles are in simultaneous progress.
  • the top load position is the highest loading/unloading position.
  • the samples are placed in the loading station 1410, which is fixed relative to the furnace 100. This position is available at the start before starting a fusion cycle, while a fusion cycle is underway in the furnace 100, and at the end when both fusion cycles are complete. This corresponds to the position that the operator can use to reload a new fusion cycle while the other fusion cycle is in progress.
  • the loading mechanism 1400 having been described above, the operation of the latter and the way the handling mechanism 200 interacts with the loading mechanism 1400 will now be described.
  • the handling mechanism 200 moves a first sample holder from the user-accessible area to the fusion area of the furnace 100; moving the first sample holder from the fusion area to an intermediary station away from the user-accessible area; and moving a second sample holder from the loading station 1410 located in the user-accessible area to the fusion area while the first sample holder remains at the intermediary station.
  • the intermediary station may correspond to the cooling station 170 or any other locations at which the sample holders may rest.
  • the handling mechanism 200 moves the first sample holder from the intermediary station to the user-accessible area.
  • the moving of the first sample holder to the user-accessible area may include moving the first sample holder to the loading station 1410 located in the user-accessible area.
  • the handling mechanism 200 may also move the second sample holder from the fusion area to the intermediary station.
  • the handling mechanism may move the second sample holder from the intermediary station to the user-accessible area by configuring the handling mechanism in a loading position in which the handling mechanism is at least partially inside the user-accessible area.
  • the moving of the second sample holder in the user-accessible area with the handling mechanism being in the loading position is performed while the first sample holder is in a loading station of the user-accessible area.
  • the moving of the first sample holder from the fusion area to the intermediary station may include cooling the first sample holder in the intermediary station.
  • the cooling of the first sample holder may include causing a flow of a cooling fluid around the first sample holder.
  • the handling mechanism 200 continues to have the following two functions. First, the handling mechanism 200 transports the samples holders 12 to different system positions inside the furnace 100. Second, the handling mechanism 200 acts as a support for the loading and discharging of the samples, as explained above. An operator may load two sample holders 12, at the same time. More specifically, a first sample holder 12 may be loaded directly into the handling mechanism 200, when it is in the loader position, and a second sampler holder 12 may be loaded into the loading station 1410 of the loading mechanism 1400. The controller can guide the operator in the process of loading sample holders via a user interface, such as via a graphical user interface displayed on a display screen.
  • a user interface such as via a graphical user interface displayed on a display screen.
  • the controller may then control the movements of the sample holders throughout the fusion cycles, and thus be enabled to manage the simultaneous start of two fusion cycles by a single command, thereafter managing the process of handling the two sample holders in a manner to avoid undesired scenarios such as leaving a sample holder in the furnace too long, collisions between sample holders, etc.
  • the controller may be operable to track the position of the two sample holders at any point in time of the overlapping fusion cycles.
  • the controller of the fusion system 10 may allow the unloading of two sample holders at the same time: a first sample holder may be positioned into the loading station 1410 of the loading mechanism 1400 and be unloaded therefrom, while the second sample holder may be supported within the loading station 1410 by the handling mechanism 200 and unloaded therefrom.
  • the handling mechanism 200 may require some adjustments of certain operations. For instance, if an operator desires to start two fusion cycles at the same time, the controller may be required to start the fusion cycling of the sample loader loaded in the handling mechanism 200 before continuing with the sample holders that are in the loading station 1410 of the loading mechanism 1400. If samples are ready to be unloaded while there is another fusion cycle in progress, the controller may be required to unload these samples into the loading station 1410 of the loading mechanism 1400 to release the handling mechanism 200. If the operator starts two fusion cycles at the same time, then the fusion cycle that corresponds to the samples that are in the handling mechanism may not be cancelled.
  • the cancelling of the fusion cycles may be caused by the controller receiving a signal from an inspection camera or other sensor, or from a user command.
  • the signal indicative of an adverse situation in the furnace 100.
  • the fusion system 10 may provide a camera inspection position allowing the camera to take a picture and perform inspection analysis, such as via machine vision.
  • the controller may cause the samples to be displaced in the camera inspection position with the handling mechanism 200 when the samples are loaded in the bottom load position. If the operator starts a fusion cycle from the top load position, the controller may cause the handling mechanism 200 to displace the samples from the loading station 1410 to the camera inspection position. If the operator starts two fusion cycles at the same time, the controller may first perform inspection with the camera from the bottom load position then proceed by using the handling mechanism 200 to displace the samples from the loading station 1410 to the camera inspection position.
  • the loading and unloading position of samples may vary depending on how the operator uses the instrument.
  • Sample holders which have been loaded into the loading station 1410 may be unloaded from the handling mechanism following a fusion cycle, or vice versa.
  • the controller may assist the operator in tracking the position of the sample holders throughout the process, such as via a graphical user interface displayed on a display screen of the controller, for instance. This can help in avoid any mistake as to which sample holder is which without having to provide any marking or identification on the sample holders themselves.
  • the operator may be required to manually unlock the loader door 1401 to prevent its accidental opening. While the samples are being loaded into the furnace 100, or otherwise while the loader door 1401 is open, the controller may stop the ventilation to prevent heat from the furnace 100 from entering the instrument, that is, to avoid overheating the system.
  • Sample holders also referred to herein as cassettes
  • crucibles may be cooled before unloading to avoid burning the operator and to avoid damaging the loading station.
  • the controller may cause the handling mechanism 200 to displace the sample holders in a specific position that will allow to cool at the same time all the cassettes/crucibles/molds that are inside the fusion system 10. For example, in this position, the controller may cause cooling of one or more of the sample holders that are in the pouring mechanism, sample holders located at the cooling station, and/or sample holders located in the handling mechanism 200.
  • the fusion system 10 may have a cooling station 170 (Fig. 1 C) as described above to allow the samples to the cooled. For example, if both fusion cycles are in progress, then the controller may fetch samples located in the furnace 100 with the handling mechanism 200 and place them in the cooling position. While a first sample holder 12 is located in the cooling station 170, the handling mechanism 200 may fetch a second sample holder 12 located at the loading station 1410 and move the second sample holder 12 from the loading station 1410 into the furnace 100. While the second sample holder 12 is in the furnace 100, the handling mechanism 200 may retrieve the first sample holder 12 from the cooling station 170 and move it onto the loading station 1410.
  • the handling mechanism 200 may retrieve the second sample holder 12 and move it to the cooling station 170, otherwise into a flow of cooling air in the furnace 100, and then into the internal volume of the loading door 1401 , or directly into the internal volume of the loading door 1410. In cases where pouring is required, the pouring may be performed at the pouring station by the pouring mechanism 500 immediately after retrieving the sample holders 12 from the furnace 100.
  • the controller may allow the operator to unlock the loader door 1401 to load and unload the samples and start a new fusion cycle only when: 1) no fusion cycle is started, 2) both fusion cycles are completed, or one fusion cycle in progress and the other is complete or not started yet.
  • the controller may cause the system to wait a prescribed amount of time during a cooling phase to allow the glass disks to solidify before loading into the furnace 100 the samples of the other fusion cycle that is pending. This time may be an adjustable system setting.
  • the controller may cause: the performing of the cooling for a given amount of time for the first fusion cycle; pause the countdown for the cooling phase of the first fusion cycle while maintaining an active ventilation; inspecting with a camera the crucibles and molds of the second fusion cycle; stopping the ventilation; loading the samples of the second fusion cycle into the furnace 100; reactivating the ventilation of the first fusion cycle and continue with the remainder of the prescribed time.
  • the controller may cause the samples to be placed in a specific position to take an adequate picture and perform an analysis.
  • the controller may mitigate a situation where the inspection camera is not enabled.
  • the controller may prompt the operator to confirm the following information before starting the fusion cycle: 1) the presence of a mold for each selected position if the fusion cycle requires the pouring step; 2) the presence of a crucible for each selected position if the fusion cycle requires NWA step; 3) no cassette is present in the handling mechanism if the fusion cycle that is about to start is only concerned with the samples that are in the loading station of the loading mechanism 1400.
  • the fusion system 10 may wait for samples to be loaded into the furnace in the following situations: 1) there is a cassette and crucibles in the pouring mechanism and there is a cassette and molds in the cooling station; 2) there is a cassette and molds in the cooling station; 3) the crucibles in the pouring mechanism are straightened; 4) the crucibles in the pouring mechanism are not yet straightened.
  • the controller may prompt the operator for confirmation that the correct samples have been inserted in the correct loading position. This validation may not be performed with the camera in some cases. This step may only be required when the handling mechanism is accessible to the operator for loading/discharging samples.
  • the controller may: 1) notify the operator of the time remaining before the operator needs to close and lock the loader door 1401 ; 2) enable a status indicator in a specific color (e.g., blue); 3) when there is a prescribed amount of time left (e.g., 30 seconds), notify the operator with a buzzer; 4) when the time to close the loader door 1401 is up, stop the buzzer, flash the status indicator and display a message asking the operator to close the loader door 1401 ; 5) the fusion cycle that is in the furnace may remain paused as long as the operator does not lock the loader door 1401 while keeping the temperature setpoint of the last heating step; 6) when the operator locks the loader door 1401 , continue the fusion cycle that was paused in the furnace, update the temperature setpoint, etc.; and 7) when the fusion cycle that was paused is complete, display
  • the controller may not block the other current fusion cycle. For instance, if, during the cooling step of a first fusion cycle, the camera emits a signal indicative of an adverse condition for the second fusion cycle, the controller may automatically abort the second fusion cycle and continue with the first fusion cycle. In this case, the controller may not display a message waiting for confirmation from the operator because this may block the fusion of the first fusion cycle and the operator may not be present in front of the fusion system 10 to carry out these steps.
  • the operator may be required to open both of the loader door 1401 and the safety door 15A. Then, if only one fusion cycle is started, the controller may be required to unload the samples into the handing mechanism because the operator may open the loader door 1401 to easily access the samples.
  • the disclosed loading mechanism 1400 may allow the operator to start two fusion cycles simultaneously, and the controller may display statuses of both. There may be an ID that identifies a group of samples for a given fusion cycle. Because the operator may start two fusion cycles at the same time, the controller may associate a batch ID for each fusion cycle and associates a position to each of the batch ID.
  • the batch ID may be automatically incremented when the operator prepares a new fusion cycle and may be reset automatically every day.
  • the load position identifies the loading/unloading position in the instrument, i.e. where the operator should place the batch ID (cassettes, crucibles, molds and samples) for the next fusion cycle and where the operator can remove them when the fusion cycle is complete.
  • the fusion system 10 disclosed herein may help improve the robustness, reliability, productivity, quality of results, and/or ease of use of the fusion process. In so doing, the fusion system 10 may reduce the need for technician time or labour and thus contribute to reducing staffing costs associated with the fusion process.
  • One or more mechanism(s) as presented herein, or it(s) control scheme can lead to reducing overall cycle time or otherwise increase productivity of a given fusion system.
  • the potential robustness of the fusion system 10 may help to lower down or idle time of the machine and thus lower cost of operations to maximize profits and margins in the contract analysis business.
  • the use of the powered and mechanized handling mechanism 200 may allow for automatic and/or autonomous/semi-autonomous fusion cycles.
  • the fusion system 10 includes a 6- position resistive-heating furnace wherein 6 positions in the furnace can undergo corresponding fusion process steps simultaneously.
  • one or more detection means can be provided to automatically validate the position of, or the presence or absence of, a given element of the system or sample.
  • the detection means can be selected as a function of the specific embodiment based on the knowledge of persons having ordinary skill in the art and can, for example, include one or more of a proximity sensor, a camera, a video camera, a weight sensor, or any other suitable type of sensor.
  • a sensor can be used to determine the presence or absence of containers in the sample support (e.g.
  • the controller may prompt, at the user interface, the user to confirm that an element of the system or samples are at a given position, present, or absent, at any suitable point of the fusion process, and proceed to the next step of the fusion process contingent upon receiving, from the user interface, the requested confirmation from the operator.

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  • Analytical Chemistry (AREA)
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EP24752614.8A 2023-02-08 2024-02-08 Fusionssystem und verfahren zur durchführung einer probenfusion damit Pending EP4662473A1 (de)

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PCT/CA2024/050166 WO2024164086A1 (en) 2023-02-08 2024-02-08 Fusion system and method of performing sample fusion therewith

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