METHOD AND DEVICE FOR SENSORY MEASUREMENT OF A MATERIAL SAMPLE

Abstract

In association with a method and a device for sensory measurement of a material sample, a measurement curve is used to detect deviations from the regular measuring characteristics of the device. A corresponding file can be made available to a service technician for evaluation.

Claims

1. A method of sensory measurement of a predetermined material sample that has been prepared by preparatory actions for performing the sensory measurement by means of an automatically-guided operator-machine interaction at a first location, the method comprising the steps of: performing the measurement automatically at the first location using a measuring apparatus while carrying out a predetermined measuring program and generating a measurement curve comprising a plurality of sections, comparing, at least partially automatically, sections of the generated measurement curve to predetermined reference values for the sections of the measurement curve; determining, from the comparing step, one or more deviations of the generated measurement curve; and making, at least partially automatically, a selection of possible sources of causative interference for the determined deviations, wherein the sources of causative interference are deviation of the functional state of at least one sub-unit of the measuring apparatus from a target state; wherein spheres of influence of sub-units of the measuring apparatus have been pre-assigned to the sections of the measurement curve.

2. The method of claim 1, further comprising the steps of: automatically compiling a file that comprises at least the measurement curve(s) and/or the possible interference sources; and transmitting the compiled file to a second location remote from the first location for further evaluation.

3. The method of claim 2, wherein the compiled file further comprises information about identity and/or characteristics of the measuring apparatus and/or its sub-units, optionally including its time profile during the measurement, an identification of the first location, the measurement curve(s) and/or measurement logs of the measurement performed at the first location.

4. The method of claim 1, wherein, any one of the following steps are carried out without any actions originating from the second location that would influence the steps: predetermining the material sample and carrying out the preparatory actions; performing the measurement automatically; and compiling the file.

5. The method of claim 1, wherein, all of the following steps are carried out without any actions originating from the second location that would influence the steps: predetermining the material sample and carrying out the preparatory actions; performing the measurement automatically; and compiling the file.

6. The method of claim 1, wherein the second location has no access to an electronic platform for issuing instructions regarding any of the of steps of: predetermining the material sample and carrying out preparatory actions, performing the measurement or compiling the file.

7. The method of claim 2, comprising the steps of: receiving the file at the second location and evaluating the measurement curves in the file; preparing spare parts and/or settings at the second location based on the evaluation; and using the spare parts and/or settings to remove sources of causative interference at the first location.

8. The method of sensory measurement of claim 1, wherein the sensory measurement comprises a thermal analysis.

9. A control software, which, when executed on a measuring apparatus for sensory measurement of a material sample, in particular by thermal analysis, controls the measuring apparatus for a method according to claim 1.

10. A control software, which, when executed on a measuring apparatus for sensory measurement of a material sample, in particular by thermal analysis, controls the measuring apparatus for a method according to claim 2.

11. A device for sensory measurement of a material sample, in particular a thermal analyzer, with a control software according to claim 9.

12. The device for sensory measurement of a material sample according to claim 11, comprising: a controller for guiding the operator-machine interaction; and a measuring apparatus for carrying out the measuring, wherein the control software comprises instruction such that the controller executes, in particular, the comparison of the measurement curve sections or the making of the selection of possible sources of causative interference.

13. A device for sensory measurement of a material sample, in particular a thermal analyzer, with a control software according to claim 10.

14. The device for sensory measurement of a material sample, according to claim 13, comprising: a controller for guiding the operator-machine interaction; and a measuring apparatus for carrying out the measuring, wherein the control software comprises instruction such that the controller executes, in particular, said comparison of the measurement curve sections, said making of the selection of possible sources of causative interference and the compiling of the file.

15. The device according to claim 14, wherein the controller is capable of controlling the device for performing the method according to claim 3.

16. A system for sensory measurement of a material sample, in particular by thermal analysis, comprising: a measuring apparatus designed for carrying out a predetermined measuring program; and a controller which controls the measuring apparatus following the performance of an automatically guided operator-machine interaction to perform the measurement according to the predetermined measuring program, which is designed to: determine one or more deviations, by an in particular at least partially automatic comparison of measurement curve sections to which there is an assignment of spheres of influence of sub-units of the measuring apparatus, with reference values and/or courses related to these measurement curve sections; based upon the determined deviations, in particular, at least in part automatically, to make a selection of possible causative interference sources present in the form of a deviation of the functional state of one or more of the subunits from their respective target state for the determined deviation.

17. The system according to claim 16, the controller being designed to carry out the method according to claim 1.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The disclosed invention will be better understood when reference is made to the accompanying figures, wherein:

[0028] FIG. 1 is a plot of temperature as a function of time for an exemplary thermogravimetric apparatus;

[0029] FIG. 2 is a plot of power as a function of time (and also of temperature) for a portion of the FIG. 1 plot; and

[0030] FIG. 3 is a plot of power as a function of elapsed time for two segments of the FIG. 1 plot.

DETAILED DESCRIPTION OF THE DRAWINGS

[0031] Preferably, at least one curve is generated in a diagram that is suitable for the measurement method, in addition to a time-temperature diagram, also a time-heat flow diagram (for DSC) or, for example, a temperature-mass diagram (TGA), are generated and, in particular, added to the file. In FIG. 1, the attached configuration used for DSC, such a temperature vs. time measurement curve is divided into 11 segments. The initial deflexion in segment 1 can be seen. The lowest attainable temperatures, which provide information about the performance of the cooler, are visible in segments 2 to 4, whereby isothermal drift, noise and distortion are also included in section 4. In section 5, a drift and artifacts can be identified, while in sections 6 and 7 the highest temperatures reached (sphere of influence of heaters and coolers), whereby isothermal drift, noise and distortion can also have an influence in segment 6. Sections 8 and 9 are of interest with regard to noise, as well as with regard to atmospheric control (gas supply), while section 10 can be assigned to a temperature control, whereas isothermal drift, noise and distortion play a role in section 11.

[0032] If, for example, a temperature of e.g. −70° is determined in section 4 at an expected temperature of e.g. −85°, the selection of possible sources of interference may include a laboratory temperature that is possibly too high, an insufficient air flow of the cooler, contaminated or blocked filters of the cooling unit, incorrect thermal contact of a cooler flange due to the installation, damaged insulation, an incorrectly installed cooling temperature sensor or damage to the cooling unit.

[0033] In a preferred configuration, the temporally subdivided sections of a measurement curve (e.g., temperature) are assigned temporally defined sections of another measurement curve and are examined therein for shifts (drift) and artifacts.

[0034] A slow change, the driving force of which is time, is considered to be a “drift”. For example, drift, which is a time effect, can be caused by temperature, pressure, aging, position (leveling of the measuring apparatus) or the like. Fast, individual changes that mainly result from mechanical or electronic influences are regarded as artifacts. Oscillating changes, slow or fast, indicate that a quantity involved is getting close to its resonance frequency.

[0035] From the attached illustration of FIG. 2 for section 5 of FIG. 1, for example, from the drift and the artifacts from the heat flow, the following possible causative source of interference are included in the selection: an incorrectly closed furnace lid (mechanical error), an incorrectly closed furnace lid (contamination), a loose sensor, an off-centre or twisted sensor, a contaminated sensor, warped crucible, or a sensor that has not been cleaned.

[0036] In a deviation from the expected temperature in section 6, the possible causative sources of interference selected would be, for example, impaired cooling capacity, an improperly installed heater at the furnace, a faulty furnace power amplifier, an improperly installed PT100, or an incorrect control voltage for the voltage supply.

[0037] FIG. 3 illustrates the response of heat flow in two different segments of the FIG. 1 data to elapsed time. From the noise in the heat flow in sections 8 and 9 (with and without gas), with section 8 without gas in the upper curve, and section 9 with gas in the lower curve, possible causative sources of interference that can be deduced are an incorrectly closed furnace lid, a loose sensor, a deformed crucible, a furnace that has not been cleaned or problems with the gas supply in general.

[0038] From the above it can be seen that the file which is compiled by the electronic diagnostic tool can contain a data record that completely describes the measuring apparatus.

[0039] It can also be seen that such an electronic diagnostic tool can be used for various DSC, TGA and TGA/DSC, TMA and DMA instruments.

[0040] If the file is transmitted to a distant second location, advance information about performance deviations in a measurement actually performed according to the predetermined measuring program is also available at this location, which allows an evaluating service technician to inform the operator of the measuring apparatus about the (probable) cause. In any case, the service technician is informed in advance by the information received before an on-site inspection and troubleshooting takes place.

[0041] In a further preferred configuration repair tools and/or materials are compiled subject to the transmitted file. This reduces the likelihood of any additional on-site appointment.

[0042] As apparent from the above, for making the diagnosis and determination of the measurement according to a predetermined measuring program, the presence of the service technician on site is not required.

[0043] In a further preferred configuration, the selection function is provided with a learning mode, and there are extensions for additional consideration of other possible additional causes.

[0044] In this context it is preferably provided that the selection function is expanded as a function of feedback information containing information about a comparison of an earlier manual check of the measuring apparatus with the previously selected possible causative sources of interference.

[0045] The invention is not limited to the features explained by way of example.