Method and apparatus for sensing measurements of a material sample

Abstract

A method and a device for sensing measurements of a material sample are formed according to the invention, so that deviations from regular measurement characteristics are detected on the basis of the measurement curve and a corresponding documentation is provided for the analysis and evaluation of a service technician.

Description

Technical Field

[0001] This invention relates to a method for sensing and measuring material samples, particularly through thermal analysis. Background Technology

[0002] Such methods are well known and include, for example, dynamic differential calorimetry (DSC - Differential Scanning Analysis), thermogravimetric analysis (TGA), and combinations thereof, such as simultaneous thermal analysis (TGA / DSC), but also thermomechanical analysis (TMA) or dynamic mechanical analysis (DMA).

[0003] In this type of method, the operator typically places the desired material sample into the measuring device, applies a measurement program or selects one from a set of predefined measurement programs, and then performs the measurement on the measuring device.

[0004] Especially due to the extremely high measurement accuracy achieved, even minor disturbances can cause measurement deviations exceeding tolerance limits. In some cases, faults may exist in the measuring equipment that have been identified as malfunctions by internal monitoring, triggering corresponding warning messages according to pre-defined fault protocols. If a fault is identified in this way, it may have already been remedied by the field operator or a maintenance technician called in for this purpose.

[0005] In other cases where the measuring equipment itself does not report a fault, but discrepancies that were initially undetected may still exist, finding the root cause of the fault is more time-consuming and not easily done by the operator of the measuring equipment, typically laboratory personnel. Instead, a maintenance technician familiar with the measuring equipment will be responsible for determining the cause of the fault in the field. Whether the maintenance technician checks the measuring equipment based on his or her experience or follows a test protocol, repeatedly determining the cause of the fault is very time-consuming. Users typically do not allow this problem to be solved by having maintenance technicians log into the field control using a remote control system (such as Team Viewer). This is also inconvenient, as it results in unfavorable working hours and long periods of inactivity for the maintenance technicians who must continuously monitor the measurements, some of which run overnight and / or for several hours, such as eight hours overnight. Summary of the Invention

[0006] Therefore, the object of the present invention is to develop a system of the type described above, such that in the event of a failure, the measuring device can be restored to full functionality with a smaller net time consumption.

[0007] This objective is achieved, in terms of system technology, by means of a method for sensing and measuring a material sample, particularly by thermal analysis, wherein the material sample is predetermined, and preparation work for performing the measurement is performed by means of an automatically guided operator-machine interaction at a first position, and then, during the execution of the predetermined measurement procedure, the measurement is automatically performed at the first position by means of a measuring device, wherein one or more deviations are determined by automatically comparing, in particular at least partially, measurement curve segments and reference values ​​and / or processes associated with these measurement curve segments—wherein the measurement curve segments are assigned the influence range of sub-units of the measuring device—and, based on the determined deviations, in particular, possible sources of interference are automatically selected at least partially, for the determined deviations, the possible sources of interference being presented in the form of deviations between the functional states of one or more sub-units and their corresponding target states.

[0008] In this context, the present invention is based on the knowledge that, in order to more quickly determine the cause of interference, a process is first automatically executed, namely, performing measurements according to a predetermined measurement procedure. This process takes a considerable amount of time, particularly exceeding one hour. The measurement procedure preferably lasts even longer than two hours, particularly exceeding three hours. In a preferred configuration of the method, the measurement procedure runs overnight and continues at least partially between 6 PM local time at the first location and 8 AM the following day.

[0009] For the operator at the user's location, there is no loss of working time. For example, he or she can invoke the electronic diagnostic tool before leaving the laboratory, such as proactively after a report of deviation from target function or at the request of a maintenance technician. Guided by the electronic diagnostic tool, necessary preparatory work is performed, and the measurement program is started, which then runs automatically. The diagnostic measurement program can be performed by measuring blanks or using defined samples. The diagnostic measurement program can be selected by the user's operator but cannot be changed.

[0010] To notify the user operator that a diagnostic measurement program is running, a warning about the running program is preferably generated and preferably displayed on the screen of the measuring device's controller.

[0011] Because the sub-units of the measuring equipment have different ranges of influence, any deviations in their functional states can also be reflected in a few, but distributable, segments of the measurement curve. On the other hand, it can be determined, at least roughly or more precisely, which type of change in the functional state of a sub-unit qualitatively leads to which type of change in a specified segment of the measurement curve. The selection of possible sources of interference has been based on advanced knowledge of the measuring equipment, grounded in actual system / pre-defined measurements performed. Based on this knowledge, maintenance technicians can perform more targeted maintenance work in the field, or operators can make simple adjustments and / or replace (replaceable) sensors in the field. For example, various potential sources of interference are excluded during the selection process, which must be considered only based on operator reports of previous laboratory measurements. These include, in particular, operator-caused errors, incorrect equipment settings / measurement parameters, and / or specific error messages generated by the measuring equipment itself.

[0012] Regardless of the degree to which the selection of potential sources of interference is automatically supported, remote maintenance technicians, not on-site, can receive relevant data. This data may already include pre-analysis and evaluation, or it may be in an intermediate processing form, and optionally, further analysis can be performed remotely relative to the measurement location, but these analyses are still based on actual measurements. Furthermore, unlike Team Viewer, on-site and remote coordination is no longer required, meaning no more time is wasted on-site or remotely. In other words, measurements performed according to predetermined measurement procedures and the analysis of the results based on them can be decoupled in time and / or space, especially decoupling. The division of measurement curve segments can be configured according to the instrument / module used for measurement.

[0013] The present invention also provides a control program for controlling the execution of the method according to the invention, as well as a correspondingly equipped and designed measuring device and controller. Attached Figure Description

[0014] Figure 1 A measurement curve according to an embodiment of the present invention is shown;

[0015] Figure 2 An exemplary segment of a measurement curve according to an embodiment of the present invention is shown;

[0016] Figure 3 An exemplary segment of a measurement curve according to an embodiment of the present invention is shown. Detailed Implementation

[0017] Further preferred embodiments are set forth in the dependent claims.

[0018] After measurements are performed according to a predetermined (diagnostic) measurement procedure executed by the operator on-site, the measurement results / measurement curves, along with the allocation or identification of the executed measurement procedure and / or the information derived therefrom, such as deviations identified in document form (e.g., .zip document) and / or choices made, can be compiled, particularly manually or automatically, and transmitted, for example, by the operator to a remote second location, where, for example, a maintenance technician can analyze and evaluate the measurement curves, and further analysis and evaluation of the curves can then be carried out. In particular, the document contains the characteristics of the modules (sub-units) and measuring devices / instruments involved.

[0019] Specific measurement programs can be pre-defined for different measurement devices, such as DSC, TGA, TGA / DSC, or even TMA and DMA. Preparation operations and measurement programs are thus coordinated or adapted to the measurement device, and in a preferred embodiment, the electronic diagnostic tool may include multiple pre-defined measurement programs and assign operator-initiated self-diagnostics to the measurement device.

[0020] For the measuring device in the sense of this invention, in addition to the actual measuring sensor, influencing sub-units may also be considered, which participate in the measurement or help determine the environment of the measurement, such as cooling systems, furnaces, gas supplies and combinations thereof (if provided).

[0021] During analysis and evaluation, maintenance technicians can, for example, determine whether measured values ​​are within acceptable tolerances. If an error is detected in a section, maintenance technicians can more easily identify possible causes (sources of interference). In cases where only a limited number of possible sources of interference appear to be present, especially when remedial measures for these interferences are within the operator's capabilities, feedback information can be returned to the field operator along with the content of that information. Alternatively or additionally, especially in more challenging situations, maintenance technicians can use prepared spare parts / setups to remedy the situation on-site.

[0022] The software used to perform diagnostic measurement procedures can be implemented in a Windows-like manner, for example, within control software (PC software) or device software (firmware), where the operator clicks, for example, a "Service" tab and selects below the "Diagnostics" tab. The operator then interacts with the machine in a guided manner, following instructions given via the machine interface to complete necessary preparatory work in a "wizard-like" fashion. For example, the operator must activate the cooling system, establish a gas supply connection, ensure the sensor is clean, and provide a predetermined material sample, such as a predetermined reference sample, for example, a 40 μl aluminum sample. Alternatively, the sample can be measured in a specific, predetermined type of sample crucible. In this case, the reference side and sample side of the sensor (especially a DSC sensor) can be specifically configured similarly.

[0023] After the preparatory measures have been performed, in a preferred embodiment, the operator may also determine the storage location for storing the automatically determined measurement results and any related primary analysis and evaluation results.

[0024] Finally, the operator can give the command to start the measurement.

[0025] In a preferred configuration, the progress of the diagnostic measurement procedure over time is displayed on the screen, especially in warning signs, to prevent the operator from interrupting the ongoing diagnostic measurement procedure.

[0026] In another preferred configuration of the method, potential sources of interference are electronically controlled to be turned on / off in order to detect these sources of interference.

[0027] The determined data preferably includes measurement curves, such as measured temperature and heat flow curves for DSC. In a preferred configuration, the measurement curves are displayed unfiltered, meaning that filtering typically present in the application measurements is disabled. In this way, if needed, the cause of a fault can be identified from subtle changes that would be undetectable due to filtering.

[0028] Preferably, at least one curve is generated in a graph suitable for the measurement method and specifically added to a time-temperature plot, time-heat flow plot (for DSC), or, for example, a temperature-mass plot (TGA), and is appended to it. For example, in the accompanying configuration for DSC, such a measurement curve is divided into 11 segments. Figure 1 The diagram shows the initial deflection in segment 1. The lowest achievable temperatures are visible in segments 2 through 4, providing information about cooler performance, with isothermal drift, noise, and distortion also included in segment 4. Drift and artifacts can be identified in segment 5, while the highest temperatures (the extent of influence of the heater and cooler) are reached in segments 6 and 7, where isothermal drift, noise, and distortion also affect segment 6. Segments 8 and 9 relate to noise and atmosphere control (gas supply), while segment 10 can be assigned to temperature control, and isothermal drift, noise, and distortion take effect in segment 11.

[0029] For example, if the temperature of -70° is determined in section 4 at a expected temperature of, for example, -85°, possible sources of interference could include excessively high laboratory temperatures, insufficient airflow to the cooler, contaminated or clogged filters in the cooling unit, incorrect thermal contact of the cooler flange due to installation, damaged insulation, incorrect installation of the cooling temperature sensor, or damage to the cooling unit.

[0030] In a preferred configuration, a time subdivision segment of a measurement curve (e.g., temperature) is assigned to a time-defined segment of another measurement curve and offset (drift) and artifacts are checked within it.

[0031] Slow changes in the driving force over time are considered "drift." For example, drift as a time effect can be caused by temperature, pressure, aging, position (leveling of measuring equipment), etc. Rapid, isolated changes primarily caused by mechanical or electronic influences are considered artifacts. Slow or rapid oscillating changes indicate that the quantity involved is approaching its resonant frequency.

[0032] For example, from Figure 2 In the attached diagram for section 5, based on the drift and artifacts of the heat flow, the following are included in the selection as possible sources of interference: improperly closed furnace lid (mechanical error), improperly closed furnace lid (contamination), loose sensor, sensor off-center or twisted, contaminated sensor, warped crucible, or uncleaned sensor.

[0033] In section 6, based on the deviation from the expected temperature, the possible sources of interference selected are, for example, reduced cooling capacity, incorrect installation of the heater at the furnace, a problem with the furnace power amplifier, incorrect installation of the PT100, or incorrect control voltage of the voltage source.

[0034] From the heat flow noise in sections 8 and 9 (with and without gas), for example... Figure 3 As shown, there is no gas in section 8 of the upper curve, while there is gas in section 9 of the lower curve. The possible sources of interference include an improperly closed furnace lid, a loose sensor, a deformed crucible, an uncleaned furnace, or general gas supply problems.

[0035] As can be seen above, documentation compiled by electronic diagnostic tools can contain data records that fully describe the measuring device.

[0036] It can also be seen that such electronic diagnostic tools can be used in various DSC, TGA and TGA / DSC, TMA and DMA instruments.

[0037] If the document is transmitted to a remote second location, advance information on performance deviations in measurements actually performed according to the predetermined measurement procedure is also available at that location. This allows maintenance technicians performing analysis and evaluation to inform the operator of the measuring equipment about the (possible) causes. In any case, the received information is communicated to maintenance technicians in advance before on-site inspection and troubleshooting.

[0038] In a further preferred configuration, repair tools and / or materials are compiled based on the transmitted documents. This reduces the likelihood of any additional on-site appointments.

[0039] As can be seen from the above, in order to diagnose and determine the measurement according to the predetermined measurement procedure, it is not necessary for maintenance technicians to be on site.

[0040] In a further preferred configuration, the selection function is provided with a learning mode, and there are extensions for considering other possible additional reasons.

[0041] In this case, it is preferable to specify that the selection function is extended based on feedback information, which includes information about the comparison of earlier manual checks of the measuring device with previously selected possible sources of interference.

[0042] The present invention is not limited to the features explained by example.

Claims

1. A method for sensing and measuring a material sample by thermal analysis, wherein, The material sample is predetermined, and preparation work for performing the measurement is performed by means of an operator-machine interaction automatically guided at a first position. Then, during the execution of the predetermined measurement procedure, the measurement is automatically performed at the first position by means of a measuring device. The measurement curve is obtained by measurement and the measurement curve is divided into multiple measurement curve segments with the influence range of the sub-units of the measuring device assigned to it. The deviation between the measured value of one or more of the measurement curve segments and the reference value is determined by at least partially automatically comparing the measurement curve segments with the influence range of the sub-units of the measuring device assigned to them and the reference values ​​and / or processes associated with these measurement curve segments. Based on the determined deviation, possible sources of interference are selected at least partially automatically. For the determined deviation, the possible sources of interference are presented in the form of deviations between the functional states of one or more sub-units and their corresponding target states.

2. The method according to claim 1, wherein, An automatically compiled document, which at least contains measurement curves and / or possible sources of interference, is transmitted to a second location remote relative to the first location and can be used for further analysis and evaluation.

3. The method according to claim 2, wherein, The document additionally includes information about the identity and / or characteristics of the measuring device and / or its subunits, optionally including its temporal variation during measurement, identification of the first location, measurement curves and / or measurement logs of the measurements performed at the first location.

4. The method according to claim 2 or 3, wherein, During automated operator-machine interaction, the measurements performed, and / or the compilation of the document, no operations originating from a second location occur that affect these processes.

5. The method according to claim 2 or 3, wherein, There is no access option originating from the second location to the electronic platform, which controls the automatically guided interaction, the measurements performed, and / or the compilation of the documents at the first location.

6. The method according to claim 2 or 3, wherein, After providing transportation to the person at the second location who received the document, the measuring equipment is inspected at the first location, at least in part, manually.

7. A computer program product, when executed on a measuring device for sensing measurements of a material sample, wherein the computer program product controls the measuring device for the method according to any one of the preceding claims, the sensing measurements being performed via thermal analysis.

8. An apparatus for sensing and measuring a material sample, comprising a computer program product according to claim 7 and / or a controller for guiding operator-machine interaction according to claim 1 and a measuring device for executing a measurement program according to claim 1.

9. The apparatus according to claim 8, wherein, The controller is capable of controlling the device to perform the method according to any one of claims 2 to 6.

10. The apparatus according to claim 8, wherein, The device is a thermal analyzer, and the controller relates to the comparison and / or selection of the measurement curve segments according to claim 1 and / or the automatic compilation of documentation according to claim 2.

11. A system for sensing measurements of material samples by thermal analysis, the system having measuring devices designed to perform a predetermined measurement procedure, and a controller that controls the measuring devices based on the performance of an automatically guided operator-machine interaction to perform measurements according to the predetermined measurement procedure, wherein a measurement curve is obtained by measurement and the measurement curve is divided into multiple measurement curve segments with influence ranges assigned to sub-units of the measuring devices, and is designed to: determine one or more deviations between the measurement curve segments and the reference values ​​by at least partially automatically comparing the measurement curve segments with influence ranges assigned to the sub-units of the measuring devices and reference values ​​and / or processes associated with these measurement curve segments; and, based on the determined deviations, at least partially automatically select possible sources of interference, wherein the possible sources of interference are presented in the form of deviations between the functional states of one or more sub-units and their corresponding target states.

12. The system of claim 11, wherein the controller is designed to perform the method of any one of claims 2 to 6.

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