专利摘要:

公开号:NL2012385A
申请号:NL2012385
申请日:2014-03-07
公开日:2015-11-18
发明作者:Marinus Josephus Maria De Kok Franciscus
申请人:Skalar Holding B V;
IPC主号:
专利说明:

DEVICE, SYSTEM AND METHOD FOR ANALYZING A SAMPLE
The invention relates to an apparatus, system and method for analyzing a sample in a sample holder.
Various techniques can be used to perform a chemical analysis of samples. A sample is burned for certain chemical analyzes. Burning is a reaction between oxygen (O2) and, for example, carbon (C) or nitrogen (N). It may also be other components that react with oxygen and are analyzed.
The resulting compounds (CO2 or NO2 or NyOx) are measured in sensors. The amount of CO2 or NO2 or NOx that is measured is a measure of the amount of C or N that has been present in the sample. If both C and N are present in a sample, they can be measured simultaneously.
GB 2 184 033 A discloses a system for analyzing the composition of a substance dissolved in a solvent. First, the solvent is removed by heating the substance in a first oven to a first temperature. The fabric is then heated in a second oven. The component released during the latter heating can be measured in a gas analyzer. However, the known system can only measure one component which, moreover, is released at a single temperature, i.e. the prevailing temperature in the second oven.
To perform a chemical analysis in which two or more components are measured, devices are known in which the sample is placed in a sample holder and the whole of the sample holder and sample is then placed in an oven of a certain temperature. In many cases, among other things, the temperature of the oven determines the efficiency of the combustion. For some analyzes it is necessary to first have a sample burn at a low temperature, then at a somewhat higher temperature and then at an even higher temperature. During or after burning, the flue gasses are pumped out of the oven and sent to the sensors for analysis.
In situations where the samples have to be kept at different temperatures for specific time intervals in order to be able to measure different components, this can be done by placing the sample holder with sample in the oven and increasing the temperature in the oven each time so that the sample is subjected to a desired temperature profile or temperature trend ..
A drawback of this is that it sometimes takes quite a long time to raise the temperature from a low to a higher temperature. Moreover, it takes even more time to get a high temperature back to a lower one, for example to make the oven suitable for processing a subsequent sample. After all, cooling generally takes more time than heating the oven. This means that the processing of the sample takes a lot of time, which limits the efficiency of the analysis.
A further drawback of the known method is that the oven must always be heated, which costs a lot of energy. Furthermore, the frequent heating and cooling of the oven and thus the expansion and shrinking of the parts of the oven form a stop on the construction of the oven, which can reduce the service life of the oven or require additional maintenance to the oven.
It is an object of the invention to provide a method and device of the type mentioned in the preamble in which at least one of the said drawbacks has been removed or reduced.
It is a further object of the invention to provide a method and apparatus with which the sample analyzes can be performed quickly and efficiently.
It is another object of the invention to provide a device that requires relatively little maintenance and / or has a long service life.
According to a first aspect of the invention, at least one of the objectives is achieved in an assembly for analyzing a sample in a sample holder, the assembly comprising: - a device, the device comprising: - a furnace for heating the sample in the sample container, wherein the oven has a heating space with at least two heating zones of different temperatures; - a displacement unit for displacing the sample holder through the heating space; wherein the displacement unit is adapted to move the sample holder at least from a first heating zone in the heating space to a second heating zone in the heating space; - measuring equipment connected to the heating space for analyzing the medium released during heating, wherein the displacement unit is adapted to guide the sample holder along the heating zones of the heating space at such speeds that the sample in the sample holder is within a predetermined temperature time- range and that the measuring equipment is designed to analyze the medium released in the first heating zone and in the second heating zone.
In the embodiment with a single heating zone, the displacement unit can be arranged to move the sample from a position outside the heating space of the oven to a position in the heating space. In that case, the sample moves from, for example, room temperature to the heating zone in which a preset temperature deviates. from the room temperature. In other embodiments, the heating space comprises at least two heating zones of different temperatures. The displacement unit is here arranged to move the sample holder (inter alia) from the first heating zone in the heating space to the second heating zone.
The sample is moved in a controlled manner from one heating zone to the other and exposed to a different temperature per zone. The temperature within a single heating zone can therefore remain the same during the sample analysis. Instead of raising or lowering the temperature in the oven to achieve the desired temperature profile of the sample, in embodiments of the invention this is accomplished by the displacement of the sample.
In certain embodiments, moving the sample includes moving the sample holder from starting position to a position in the first heating zone, then moving the sample holder from the first heating zone to a position in the second heating zone (with different temperature) and finally moving the sample holder. moving the sample holder to the starting position. In other embodiments, after displacement to a position in the second heating zone, one or more displacements take place to one or more further heating zones. Furthermore, the sample holder does not always have to be moved back to the starting position. For example, embodiments are conceivable in which the sample holder with the remains of the sample, burned or not, is directed to a different position to be removed there. In the above embodiments, the oven has only one or two heating zones. In other embodiments, the oven may comprise three, four or more heating zones.
There are versions in which the temperature distributed over a heating zone is virtually constant. Almost constant can mean, for example, that the temperature at different positions and different times within a zone varies a maximum of 5% with respect to the average temperature. The temperature increases between the different heating zones, the temperature increases abruptly in some versions and more gradually in others.
In other embodiments, the temperature in a heating zone is not constant, but increases, for example, within a heating space in a certain direction of the heating space, for example in an upward direction in the case of a vertical heating space. In certain embodiments of the invention, the difference in (average) temperature between each of the different heating zones is at least 50 degrees Celsius, and preferably more than 100 degrees Celsius. In other embodiments, the temperature in a particular direction, for example the upward direction, continuously increases over a temperature range of at least 50 degrees Celsius, preferably more than 100 or even more than 400 degrees Celsius. In a specific embodiment, the temperature in the heating zones is 105, 450, 600 and 900 degrees Celsius, respectively.
The temperature in a heating zone preferably remains constant during the heating and analysis. However, the temperature can be set to a different value before or after heating the sample. Such an adjustable temperature of one or more of the heating zones makes it possible, for example, to use the oven for different types of analyzes, different compositions of the sample, quantity of sample, etc.
The temperature gradually increases or decreases between zones. The speed of transporting the sample in combination with the various (controllable) temperatures determines the time-temperature graph associated with a particular sample combustion.
The sample is burned for certain chemical analyzes. The heating space then functions as a combustion space. The resulting connections in the discharged medium are measured in the sensors. The amount that is measured is a measure of the amount of one or more components that were originally present in the sample. In certain analyzes it is necessary to first burn the sample at a low temperature, then at a somewhat higher temperature and then at an even higher temperature. After burning, the discharge medium (i.e. the flue gases) is removed from the combustion space, for example by allowing it to flow out of the heating space under its own power or by pumping it out of the heating space, fed to the sensors for analysis.
To change the temperature of the sample in a suitable manner to enable proper analysis, it must be exposed to the correct ambient temperatures (i.e., the temperatures in the heating chamber) at the correct time intervals. In other words, the sample must be kept within a certain temperature-time range. The analysis may, for example, prescribe that in a first time interval the sample must be exposed to a constant, relatively low temperature, in a subsequent second time interval to a constantly increasing temperature (from the constant, relatively low temperature to a constant, relatively high temperature) exposed to the constant, relatively high temperature in a subsequent third time interval. The analysis may then stop, but in other examples the sample is further warmed up and kept at a constant, even higher temperatures in a number of further time intervals.
Said temperature-time range can be realized by guiding the displacement unit of the sample holder with a specific velocity profile along the temperature heating zones. The sample holder can be passed along the heating zones of the heating chamber at such speeds that the sample in the sample holder is continuously within the predetermined temperature-time range. In certain embodiments, said speed profile is predetermined and programmed, for example, in a memory of the control unit of the displacement unit. The speed profile can be defined in various ways. The device, for example the control unit thereof, can be adapted to adjust the instantaneous speed of the sample holder depending on the position of the sample holder in the heating space. It is also possible for the device to adjust the instantaneous speed of the sample holder depending on the passage of time from a start time.
In other versions, this speed profile can also be calculated "on the fly". Furthermore, it is possible to use one or more temperature sensors connected to the control unit which are arranged at one or more different positions within the heating space. The control unit can thereby control the displacement of the sample holder depending on the sensor signals received. The control unit may, for example, be adapted to determine target speeds of the sample holder and control the displacement of the sample holder at the target rates depending on the observed temperature or temperatures and the residence time of the sample holder in the heating space.
In certain embodiments of the invention, the device comprises a gas supply unit for supplying gas to the heating space, for example because this gas is required for the analysis. This gas can be oxygen required for the combustion process of the sample. Supply of other gases is also possible. The gas is preferably supplied to a first end of the heating space and the medium to be discharged (such as flue gases in the case of a combustion) is discharged along the opposite ends of the heating space.
The device may comprise a medium discharge tube connected to the heating space for discharging medium released during heating (such as gas, liquid and / or solid particles) to measuring equipment which is adapted to give one or more measuring signals representative of the composition of the medium in the medium discharge tube. The medium can be recycled or not. For this purpose, in certain embodiments, a recirculation line is provided.
In a particular embodiment of the invention, the heating space is an elongated upright, preferably vertical, space. In particular, the heating space can be formed within an elongated pipe. The pipe is preferably made of material that conducts heat well. The displacement unit can in this case be adapted to guide a support for supporting the sample holder in upward and downward direction through the heating space. In this embodiment, the heating zones are located at different height positions, wherein generally (but not limited to) the warmer heating zones are at a higher position than the colder heating zones.
In the case that the heating space is formed in an elongated pipe, heating elements may be provided along part of the length of the pipe or along the entire pipe. The heating elements can be arranged for heating the heating space via heating of the pipe itself and / or for directly heating the heating space. In certain embodiments, heating elements are only provided along one or more of the relatively warm heating zones and the other heating zones are free of heating elements. Where there are no heating elements, the heating space will nevertheless be heated as a result of the conduction of heat via the pipe wall. In further embodiments, the pipe wall is also free of insulating material at the location where it is free from heating elements, while insulating material is provided at the location of the heating elements. Due to heat radiation to the outside, where there are no heating elements, the temperature in the heating space can be relatively low, while at other positions the temperatures can rise to much higher values.
According to another aspect of the invention, a method for analyzing a sample in a sample holder is provided. Use can be made of the device as described herein. The method comprises: - heating the sample in the sample holder by moving the sample holder along a first heating zone of a first temperature; - collecting medium generated by heating the sample; - measuring and subsequently analyzing the collected medium; - further heating the sample in the sample holder by moving the sample holder along a second heating zone from a second temperature higher than the first temperature; - collecting medium generated by heating the sample; - measuring and subsequently analyzing the collected medium, wherein the sample holder is moved along the heating zones of the heating space at such speeds that the sample in the sample holder falls within a predetermined temperature-time range.
In embodiments of the invention, the sample is moved along three or more heating zones. The temperature in the heating zones is different here.
The (internal) temperature of the sample is preferably set by adjusting the displacement speeds at which the sample holder is moved along the heating zones. Preferably, the temperatures in the different heating zones remain constant during the passage of the sample holder along the heating zones. Only by varying the speed of the sample holder (more particularly the support for the sample holder) is it already possible to keep the sample within the desired temperature-time range.
The method may comprise guiding the sample container with a preset speed profile along the heating zones of different temperatures. This makes simple control of the displacement unit possible. In other embodiments, the speed profile is determined “on the fly”, whether or not on the basis of received measurement signals, such as signals representative of measured temperatures, for the composition of the sample, etc. This embodiment is more complex and will in many situations not are necessary, but makes it possible, for example, to adjust the speed profile to the extent necessary.
According to a third aspect of the invention, an assembly of at least one device as defined herein and measuring equipment for analyzing the medium released during heating via the device becomes.
Further advantages, features and details of the invention will be elucidated on the basis of the following description of some embodiments thereof. Reference is made in the description to the accompanying figures, in which:
Figure 1 shows a cross-section through an embodiment of an analysis device according to the invention;
Figure 2A shows the embodiment of Figure 1 wherein the sample holder is in a low position;
Figure 2B shows the embodiment of Figure 1 wherein the sample holder is in a center position;
Figure 2C shows the embodiment of Figure 1 wherein the sample holder is in a high position; and
Figure 3 shows a graph of the temperature range within which the sample must be kept in the sample holder over time.
Figure 1 shows an analysis device 1, which is composed of an oven 2 and a displacement unit 3. The displacement unit functions as an introduction system for introducing a sample into the oven. On a carousel (not shown in the figures) a number (for example about twenty) of sample holders 10, for example sample cups, are arranged. An amount of sample (m) to be analyzed is provided in each of the sample holders. The displacement unit is designed such that it can pick up a sample holder from the carousel and move it to the oven 2.
In the embodiment shown, the oven 2 comprises an upright tube 5 made of ceramic material, inside which an elongated heating space 6 is formed. A heating unit is arranged around a part of this tube 5. The heating unit comprises a housing 4 in which one or more spiral-shaped heating elements 12 are arranged. The heating elements can give off an amount of heat that is sufficient to bring the temperature in the heating space 6 to a sufficiently high level. The heating elements can be of any type. In the embodiment shown, the heating elements 12 are connected to an electrical supply unit (not shown). The power supply unit, driven by a control unit 29 (shown schematically in Figure 1), can be supplied with current through the heating elements 12 so that they start to release heat.
In the embodiment shown, the heating elements 12 are arranged on the outside of the tube 5, so that the heating elements first give off heat to the tube and then the tube gives off heat to the inner space 6. In other embodiments, however, the heating elements are placed directly in the heating space to immediately heat up the heating space.
In order to prevent too much heat from being lost at various locations, one or more insulation packages 7 are provided around the pipe 5. The lower end of the tube 5 is coupled via a coupling with gasket, for example an elastic O-ring 15, to a frame 9 which is stably placed on a substrate. With respect to this frame 9, which, like the tube 6, is stationary, a rod 8 of the displacement unit 3 can be displaced in an upward or downward direction (direction P15, Figure 1). This displacement is driven by a drive 14. schematically shown in figure 1. This drive 14 can be any drive and a further description thereof can be omitted.
Furthermore, an entrance opening 5 is provided at the lower end of the tube 6. A gas inlet 13 (indicated by dotted lines) can be connected to this entrance opening. This gas inlet 13 makes it possible to supply a desired gas (direction P2, figure 1), for example oxygen, to enable combustion of the sample (m) in the sample holder 10.
As shown in Fig. 1, the upper end of the rod 8 is provided with a support 22 on which a replaceable sample holder 10 can be mounted in a stable manner.
The support 22 of the sample holder 10 can be led via the drive 14 and controlled by the control unit 29 from a starting position not shown in the figures via the entrance opening 5 into the tube 5 to a first, lower position. This position is shown in Figure 2A. From the first position, the support can be moved to a second position (Figure 2B), a third position (Figure 2C) and back to the starting position (P3, Figure 1).
At the upper end the tube 5 is connected to a medium discharge tube 18. This medium discharge tube 18 is connected with its entry part 17 to the inner space 6 of the tube 5. The entry part 17 is connected to the via a clamp coupling 16 by means of an O-ring. tube 5 connected. The medium that flows upwards in the tube, consisting of what is left of the gas previously introduced via the entrance opening 5 and the gases / liquid and / or solid particles of the sample released, can be discharged via the medium discharge tube 18 in the direction of the processing unit 19. In this processing unit, the medium may or may not be treated in a processing unit 20 and analyzed in an analyzing unit 21. In some embodiments, the optionally treated and analyzed medium is discharged elsewhere. In other embodiments, a part of the supplied, treated and analyzed medium is fed back into the gas supply 13 to the tube 5 via a recirculation line 25 (shown in broken lines in Figure 1).
By switching on the heating elements 12, a number of heating zones can be created in the heating space 6 of the tube 5. Each heating zone has temperatures that differ from the temperatures in another zone. Figure 2A, for example, shows that on the underside of the tube 5, where there are no heating elements 12, the temperature in the first heating zone 30 of the heating space 6 has a first, low value (T layer). At a slightly higher position, where heating elements 12 are present, a second heating zone 31 is realized. In this second heating zone 31, the (average) temperature (T center) is a lot higher. Above that is the third heating zone 32 where the (average) temperature (Thoog) is much higher.
In certain embodiments, the differences in temperature at different positions within the same heating zone are relatively small, so that when a sample M is disposed in a particular heating zone, the sample is more or less subjected to the same temperature. In other embodiments, however, the temperature in two or more of the heating zones is gradual. In Figures 2A-2C, for example, the temperature in the second heating zone can increase from bottom to top and a gradual transition between the second and third heating zone has been created. In all of these embodiments, it is possible to subject the sample to a desired temperature for a desired time interval by properly selecting the speed profile with which the support 22 is guided along the heating zones.
Referring to Figure 3, an example is given of how a sample (m) can be heated within a predetermined temperature-time range. In a first time interval 41, the sample (m) is dried at a drying temperature (T |). Subsequently, the support 22 with sample holder 10 is sent via the entrance opening 5 to the first position (as shown in Fig. 2A). In the position shown in Figure 2A, the sample is in the first heating zone. In this zone the tube 5 is not surrounded with the aforementioned insulating material. The tube is indeed warm, since the heat from the heating element 12 also heats the tube part in the first heating region via conduction, but due to radiation of heat to the environment, the temperature within the first heating zone can be kept relatively low. Due to the direct presence of the heating element, whether or not in combination with the insulating material, the temperature in the next heating zone 31 is considerably higher (preferably more than 50 degrees Celsius, more than 100 degrees Celsius or, as the specific example, approximately 150 degrees Celsius higher).
During the displacement of the sample holder support (i.e. in the second time interval 42), the temperature increases with a predetermined rise value per time unit. In the example, the temperature in time interval 42 increases by 70 degrees Celsius per minute. The temperature at the first position is the previously mentioned first low temperature. This low temperature (T2) in the example is approximately 450 degrees Celsius. During the third time interval 43, the sample continues to be subjected to this first temperature. In the subsequent fourth time interval 44, the temperature increases again (for example by 70 degrees Celsius per minute) until the aforementioned second, middle temperature (T3) is reached. In the example, this temperature (T3) is 600 degrees Celsius. The sample is now at the middle position shown in Figure 2B in the heating space 6. After a rise in temperature in the sixth time interval (for example again by 70 degrees Celsius per minute), the third, highest temperature value (T4) is reached. The sample holder support 22 is now at the highest position shown in Figure 2C. In the specific example, the highest temperature values are 900 degrees Celsius. After having been subjected to the highest temperature during the seventh time interval 47, the sample is removed from the over by leading the sample holder support 22 back down to the starting position. The sample holder can now be removed and discharged for further processing (for example a cleaning operation) and the device is ready for the analysis of a subsequent sample.
The outlined temperatures and time intervals are simply only determined by the speed at which the sample holder support 22 is passed through the heating space 6. The temperature in the different heating zones 30-32, as mentioned above, remains substantially constant. The sample is therefore only heated by guiding it at a suitable position within the heating space 6 at a suitable speed, whether or not varying, without the oven itself having to be further heated or cooled down. This is advantageous because it allows the whole analysis to be carried out more quickly and the various parts of the oven are no longer exposed to temperatures that vary considerably over time. Because the temperature within the different heating zones can be kept at different but substantially constant values, the life of the oven is relatively long. The material of the furnace does not therefore always have to undergo a cooling on heating and the associated shrinkage or expansion.
Depending on the sample used (type of material, quantity, quality, etc.), it is possible in certain versions to determine in advance which speed profile must be given to the support in order to heat up the sample according to the appropriate temperature-time profile.
The speed profile can then, for example, be stored in the control unit 29 and be repeated each time for a new sample. No further measurement of the temperatures or other physical parameters within the tube 5 is required. In certain embodiments, however, sensors (such as temperature sensors, humidity sensors or the like) are provided in and around the heating space 6. These temperature sensors emit signals, on the basis of which the control unit 29 can calculate a suitable speed profile. This version is more complex and will not be necessary in most cases. However, in cases where there are large differences in quality within a batch of samples, the implementation can offer a solution. For example, in certain embodiments, a temperature sensor is provided in the heating space 6, but this sensor is not used during the analysis itself and only serves as prior calibration, that is, before the analysis of the sample is started.
Because the sample remains in the same tube 5 during the entire analysis and the medium is discharged via the same outlet tube as a result of the heating of the sample and / or the supply of gases to the tube, a quick and well-reproducible analysis of the sample can be realized. .
The device according to the invention is suitable for carrying out countless analysis methods. An illustrative example is an analysis method in which the discharged medium consists of combustion gases that are released when the sample is burned at different temperatures. These combustion gases can be led from the furnace 2 via the line 18 to a second furnace where, among other things, all nitrogen components are oxidized to N x O y. After this, these gases are led through a Peltier cooler that ensures that water is condensed and removed from the gas stream. A small portion of these combustion gases is transported by a helium gas stream to the copper reducer furnace where the NxOy is reduced to N2. The last step is to pass the gas through a CO2 scrubber and magnesium perchlorate water carrier. The gas stream consisting of N2 and He (carrier gas) is fed to a thermal conductivity detector and measured.
The invention is not limited to the embodiments thereof described and shown herein. The scope of the invention is determined by the following claims, within the medium released during heating via the device.
权利要求:
Claims (35)
[1]
An assembly for analyzing a sample in a sample holder, comprising: - a device, the device comprising: - an oven for heating the sample in the sample holder, the oven having a heating space with at least two heating zones of different temperature ; - a displacement unit for displacing the sample holder through the heating space; wherein the displacement unit is adapted to move the sample holder at least from a first heating zone in the heating space to a second heating zone in the heating space; measuring equipment connected to the heating space for analyzing the medium released during heating, characterized in that the displacement unit is adapted to guide the sample holder along the heating zones of the heating space at such speeds that the sample in the sample holder is within a predetermined temperature-time range and that the measuring equipment is designed to analyze the medium released in the first heating zone and in the second heating zone.
[2]
An assembly according to claim 1, wherein the displacement unit is adapted to guide the sample holder with a preset speed profile along the heating zones of different temperatures.
[3]
An assembly according to claim 1 or 2, wherein the displacement unit is adapted to adjust the temperature trend over time of the temperature of the sample in the sample holder by varying the speed of movement of the sample holder along at least two heating zones.
[4]
An assembly according to claim 3, wherein the device is adapted to expose the sample to the desired temperature at the desired moment only by varying the speed at substantially constant temperatures in the respective heating zones.
[5]
An assembly according to any one of the preceding claims, wherein the assembly is adapted to adjust the instantaneous speed of the sample holder depending on the position of the sample holder in the heating space.
[6]
An assembly according to any one of the preceding claims, wherein the assembly is adapted to adjust the instantaneous speed of the sample holder depending on the time course from a start time.
[7]
An assembly according to any one of the preceding claims, wherein the device is adapted to control the temperatures in the different heating zones and the speed of transporting the sample in such a way that the sample conforms to a predetermined sample combustion according to the time-temperature graph is heated.
[8]
An assembly according to any one of the preceding claims, wherein the heating space defines an elongated upright, preferably vertical, space, and wherein the displacement unit is adapted to guide a support for supporting the sample holder upwards and downwards through the heating space.
[9]
An assembly according to any one of the preceding claims, wherein the measuring equipment is adapted to measure nitrogen and / or carbon components.
[10]
An assembly according to any one of the preceding claims, wherein the oven is adapted to partially or completely burn the sample in the sample container and / or wherein the measuring equipment is adapted to perform a first measurement of the composition of a sample at a first temperature released medium when the sample is in the first heating zone and performing a second measurement of the composition of the medium released at a second temperature, higher than the first temperature, when the sample is in the second heating zone.
[11]
An assembly according to any one of the preceding claims, wherein the displacement unit is adapted to move the sample holder from a first position outside the oven to a second position in the first heating zone within the oven, from the second position within the first heating zone to a third position in the second heating zone within the oven and from the third position to a further position outside the second heating zone, wherein the further position is preferably in a further heating zone and / or wherein the further position is preferably a position outside the oven, for example the first position.
[12]
An assembly according to any one of the preceding claims, wherein the oven is arranged to keep each of the heating zones at a substantially constant temperature.
[13]
An assembly according to any one of the preceding claims, comprising a gas supply unit for supplying gas to the heating space.
[14]
Assembly as claimed in any of the foregoing claims, comprising a medium discharge tube connected to the heating space for discharging medium released during heating to measuring equipment which is adapted to give one or more measuring signals representative of the composition of the medium in the medium drain pipe.
[15]
An assembly according to claim 13 or 14, comprising a recirculation conduit connected between the gas supply unit and medium discharge tube for recirculating at least a part of the discharged medium.
[16]
An assembly according to any one of the preceding claims, comprising: - one or more temperature sensors arranged at one or more different positions within the heating space; - a control unit for controlling the displacement of the sample holder, wherein the control unit is adapted to determine target speeds of the sample holder and control the target speeds with respect to the observed temperature or temperatures and the residence time of the sample holder in the heating space movement of the sample holder.
[17]
17. Assembly as claimed in any of the foregoing claims, comprising a first and second heating zone, wherein the first heating zone is at a smaller height than the second heating zone.
[18]
An assembly according to any one of the preceding claims, comprising: - a drive for driving the displacement of a sample holder support in the heating space; - a control unit for controlling the drive.
[19]
Assembly as claimed in any of the foregoing claims, wherein the heating space is formed by an elongated pipe and wherein heating elements are arranged along at least a part of the length of the pipe.
[20]
A device for analyzing a sample in a sample holder, comprising a device as defined in any one of the preceding claims, wherein the device is adapted to be connected to measuring equipment which is adapted to analyze the heating when heated in the heating space of medium released from the device.
[21]
A method for analyzing a sample in a sample holder, preferably in an apparatus according to any one of the preceding claims, the method comprising: - heating the sample in the sample holder by moving the sample holder along a first heating zone of a first temperature; - collecting medium generated by heating the sample; - measuring and subsequently analyzing the collected medium; characterized by - further heating the sample in the sample holder by moving the sample holder along a second heating zone from a second temperature higher than the first temperature; - collecting medium generated by heating the sample; - measuring and subsequently analyzing the collected medium, wherein the sample holder is moved along the heating zones of the heating space at such speeds that the sample in the sample holder falls within a predetermined temperature-time range.
[22]
A method according to claim 21, comprising guiding the sample container along a pre-set speed profile along the heating zones of different temperatures.
[23]
A method according to any one of claims 21-22, comprising adjusting the temperature variation over time of the (internal) temperature of the sample in the sample by varying the speed of movement of the sample holder along at least two heating zones. sample holder
[24]
A method according to any of claims 21-23, comprising only exposing the sample to the desired temperature at the desired moment by varying the speed at substantially constant temperatures in the respective heating zones.
[25]
A method according to any of claims 21-24, comprising adjusting the instantaneous speed of the specimen holder depending on the position of the sample holder in the heating space and / or comprising adjusting the instantaneous speed of a sample time depending on the time course of a start time. the sample holder.
[26]
A method according to any of claims 21-25, comprising controlling the temperatures in the different heating zones and the speed of transporting the sample such that the sample is heated in accordance with the time-temperature graph associated with a predetermined sample combustion. .
[27]
A method according to any one of claims 21-26, comprising measuring nitrogen and / or carbon components and / or comprising first measuring the components released in a first temperature zone and then measuring the components released in a second temperature zone.
[28]
A method according to any of claims 21-27, the method comprising moving the sample holder along a number of heating zones with the temperature in the heating zones differing from each other.
[29]
A method according to any one of the preceding claims 21-28, comprising adjusting the (internal) temperature of the sample by adjusting the displacement speeds at which the sample holder is moved along the heating zones.
[30]
A method according to any of claims 21-29, comprising: - moving the sample holder from a first position outside of an oven to a second position in the first heating zone within the oven, - subsequently moving the second position within the first heating zone to a third position in the second heating zone within the oven; and - moving the third position to a further position outside the second heating zone.
[31]
A method according to any one of claims 21-30, comprising adjusting the instantaneous speed of the sample holder depending on the position of the sample holder in the heating space and / or comprising adjusting the instantaneous speed of a sample time depending on the time course of a start time. the sample holder.
[32]
A method according to any one of claims 21-31, comprising discharging medium released during heating to measuring equipment and outputting one or more measuring signals representative of the composition of the medium in the medium discharge tube.
[33]
A method according to any of claims 21-32, comprising supplying gas to the heating space and / or recycling at least a part of the discharged medium.
[34]
A method according to any one of claims 21-33, comprising: - observing the temperatures at one or more different positions within the heating space; - determining target speeds of the sample holder depending on the observed temperature or temperatures and the residence time of the sample holder in the heating space; - moving the sample holder at the target speeds.
[35]
The method of any one of claims 21 to 34, wherein when the heating space defines an elongated upright, preferably vertical, space, the method comprises guiding the sample container up and down through the heating space.
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同族专利:
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引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题
US3954408A|1974-11-29|1976-05-04|Sandoz, Inc.|Apparatus and process for chromatographic product detection|
GB2080232A|1980-07-22|1982-02-03|Leco Corp|Crucible loading-unloading apparatus|
GB2184033A|1985-12-11|1987-06-17|Analink Dev Ltd|An apparatus for and a method of removing solute from solvent|
WO2005043152A1|2003-10-21|2005-05-12|Petroleum Analyzer Company, Lp|A fast system for detecting detectible combustion products and method for making and using same|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
NL2012344|2014-03-02|
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