CN113609659B - Method, device and equipment for determining evaporation loss determination test conditions - Google Patents
Method, device and equipment for determining evaporation loss determination test conditions Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 330
- 230000008020 evaporation Effects 0.000 title claims abstract description 257
- 238000001704 evaporation Methods 0.000 title claims abstract description 257
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- 238000005259 measurement Methods 0.000 claims abstract description 106
- 238000002411 thermogravimetry Methods 0.000 claims abstract description 51
- 238000010998 test method Methods 0.000 claims abstract description 35
- 238000003860 storage Methods 0.000 claims abstract description 16
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Abstract
The invention discloses a method for determining evaporation loss determination test conditions, which comprises the following steps: analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method, and determining the value range of the test influence factors; adopting an orthogonal test method, and obtaining a plurality of test conditions according to the value range of the test influence factors; and comparing and analyzing the test result of the evaporation loss measurement of the known sample under each test condition according to the evaporation loss result of the known sample acquired in advance, and determining the optimal test condition. The invention also discloses a device, equipment and storage medium for determining the evaporation loss measurement test conditions, which can analyze the test conditions of the evaporation loss measurement of the known sample by utilizing a thermogravimetric analysis method and an orthogonal test, further determine the optimal test conditions and realize the rapid determination of the evaporation loss of the brake fluid under the optimal test conditions.
Description
Technical Field
The invention relates to the technical field of measurement, in particular to a method, a device and equipment for determining evaporation loss determination test conditions.
Background
The evaporation performance of the brake fluid has very important significance for the lubricating performance, the service life and the normal performance and the reliability of a brake system when the brake fluid is used at a higher temperature, and is an important high-temperature performance index of the brake fluid. The evaporation loss of the brake fluid is unqualified, and when the vehicle brakes to generate high temperature, a large amount of brake fluid can be evaporated, so that braking failure is caused, serious and even complete evaporation of the brake fluid is possible, braking is impossible, serious safety accidents are caused, and life safety of people is directly endangered. Therefore, it is necessary to measure the evaporation loss of the brake fluid, and a brake fluid having a good high-temperature stability and a low evaporation loss is used.
The national standard GB 12981-2012 (motor vehicle brake fluid) annex H prescribes a detection method for the evaporation performance of the brake fluid, a specified amount of brake fluid is kept at a constant temperature of 100 ℃ for 168 hours, and the evaporation loss mass fraction is calculated according to the mass change before and after the constant temperature, and the test period under the test condition is too long to rapidly detect the evaporation loss of the brake fluid, so that the requirement of rapid detection of scientific research production is difficult to meet.
Disclosure of Invention
The embodiment of the invention aims to provide a method, a device and equipment for determining evaporation loss measurement test conditions, which can analyze the test conditions of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method and an orthogonal test, further determine optimal test conditions and realize rapid determination of evaporation loss of brake fluid under the optimal test conditions.
In order to achieve the above object, an embodiment of the present invention provides a method for determining evaporation loss measurement test conditions, including:
analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method, and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
adopting an orthogonal test method, and obtaining a plurality of test conditions according to the value range of the test influence factors;
and comparing and analyzing the test result of the evaporation loss measurement of the known sample under each test condition according to the evaporation loss result of the known sample acquired in advance, and determining the optimal test condition.
As an improvement of the scheme, the adoption of the orthogonal test method obtains a plurality of test conditions according to the value range of the test influence factors, and the method specifically comprises the following steps:
determining a plurality of recommended values of the test influence factors corresponding to the test influence factors according to the value range of the test influence factors;
And acquiring a plurality of test conditions according to a plurality of recommended values of the test influence factors corresponding to the test influence factors by adopting an orthogonal test method.
As an improvement of the above-described scheme, the test influencing factors include an evaporation reference time and a diameter of the through hole;
then, the analysis of the test conditions of evaporation loss measurement of the known sample by using the thermogravimetric analysis method, the determination of the value range of the test influence factor specifically includes:
analyzing test results of evaporation loss measurement of a plurality of known samples under different evaporation reference time by utilizing a thermogravimetric analysis method, and determining a value range of the evaporation reference time;
and analyzing the test results of evaporation loss measurement of the known samples with different diameters by utilizing a thermogravimetric analysis method, and determining the value range of the diameters.
As an improvement to the above, the test influencing factors further include the sampling amount of the known sample;
then, the analyzing the test condition of the evaporation loss measurement of the known sample by using the thermogravimetric analysis method to determine the value range of the test influencing factor further comprises:
and analyzing the test results of evaporation loss measurement of the known samples under a plurality of different sampling amounts by utilizing a thermogravimetric analysis method, and determining the value range of the sampling amounts.
As an improvement of the above solution, the determining, according to the value range of the test influencing factor, a plurality of recommended values of the test influencing factor corresponding to the test influencing factor specifically includes:
determining a plurality of recommended evaporation reference time values according to the value range of the evaporation reference time;
determining a plurality of diameter recommended values according to the value range of the diameter;
determining a plurality of recommended sampling quantity values according to the sampling quantity value range;
and acquiring a plurality of test conditions by adopting an orthogonal test method according to a plurality of recommended values of the test influence factors corresponding to the test influence factors, wherein the method specifically comprises the following steps:
and acquiring a plurality of test conditions according to the evaporation reference time recommended value, the diameter recommended value and the sampling amount recommended value by adopting an orthogonal test method.
In order to achieve the above object, an embodiment of the present invention further provides a device for determining evaporation loss measurement test conditions, including:
the influence factor range determining module is used for analyzing at least two test influence factors of evaporation loss determination of a known sample by utilizing a thermogravimetric analysis method and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
The test condition acquisition module is used for acquiring a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method;
and the optimal test condition determining module is used for comparing and analyzing the test result of the evaporation loss measurement of the known sample under each test condition according to the evaporation loss result of the known sample acquired in advance to determine the optimal test condition.
As an improvement of the above solution, the test condition acquisition module specifically includes:
the recommended value determining unit is used for determining a plurality of recommended values of the test influence factors corresponding to the test influence factors according to the value range of the test influence factors;
and the test condition acquisition unit is used for acquiring a plurality of test conditions according to a plurality of recommended values of the test influence factors corresponding to the test influence factors by adopting an orthogonal test method.
As an improvement of the above-described scheme, the test influencing factors include an evaporation reference time and a diameter of the through hole;
the influence factor range determining module specifically includes:
the evaporation reference time range determining unit is used for analyzing test results of evaporation loss determination of a plurality of known samples under different evaporation reference time by utilizing a thermogravimetric analysis method and determining the value range of the evaporation reference time;
And the diameter range determining unit is used for analyzing the test results of evaporation loss measurement of the known samples with different diameters by utilizing a thermogravimetric analysis method and determining the value range of the diameters.
To achieve the above object, an embodiment of the present invention further provides a determining apparatus of evaporation loss measurement test conditions, including a processor, a memory, and a computer program stored in the memory and configured to be executed by the processor, the processor implementing the determining method of evaporation loss measurement test conditions according to any one of the embodiments described above when executing the computer program.
To achieve the above object, an embodiment of the present invention further provides a computer readable storage medium, where the computer readable storage medium includes a stored computer program, where the computer program when executed controls a device where the computer readable storage medium is located to execute the method for determining the evaporation loss measurement test condition according to any one of the above embodiments.
Compared with the prior art, the method, the device, the equipment and the storage medium for determining the evaporation loss measurement test conditions are disclosed by the embodiment of the invention, at least two test influence factors of the evaporation loss measurement of the known sample are analyzed by utilizing a thermogravimetric analysis method, and the value range of the test influence factors is further determined; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole; obtaining a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method; the optimum test conditions are determined by comparing and analyzing the test results of evaporation loss measurement of the known sample under each test condition based on the previously acquired evaporation loss results of the known sample. Therefore, the embodiment of the invention can analyze the test conditions of the evaporation loss measurement of the known sample by utilizing a thermogravimetric analysis method and an orthogonal test, and further determine the optimal test conditions so as to realize the rapid measurement of the evaporation loss of the brake fluid under the optimal test conditions.
Drawings
FIG. 1 is a flow chart of a method for determining evaporation loss measurement test conditions according to an embodiment of the present invention;
FIG. 2 is a graph of typical brake fluid thermogravimetric analysis provided by an embodiment of the present invention;
FIG. 3 is a table showing the effect of different pore diameters on the evaporation loss of brake fluid according to an embodiment of the present invention;
FIG. 4 is a table showing the effect of different sampling amounts on the evaporation loss of brake fluid according to an embodiment of the present invention;
FIG. 5 is a table comparing the effect of different gas flows on brake fluid evaporation loss according to an embodiment of the present invention;
FIG. 6 is a table of orthogonal test factors versus level provided by one embodiment of the present invention;
FIG. 7 is a diagram of orthogonal test designs and results tables provided by one embodiment of the present invention;
FIG. 8 is a table of stability test results provided by an embodiment of the present invention;
FIG. 9 is a table of accuracy test results provided by an embodiment of the present invention;
FIG. 10 is a block diagram showing the construction of a device for determining evaporation loss measurement test conditions according to an embodiment of the present invention;
FIG. 11 is a block diagram illustrating a test condition acquisition module according to an embodiment of the present invention;
FIG. 12 is a block diagram illustrating a configuration of an influence factor range determination module according to one embodiment of the present invention;
FIG. 13 is a block diagram illustrating another exemplary influence factor range determination module according to an embodiment of the present invention;
fig. 14 is a block diagram showing the construction of a device for determining evaporation loss measurement test conditions according to an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, a flow chart of a method for determining evaporation loss measurement test conditions according to an embodiment of the invention is shown.
The method for determining the evaporation loss measurement test condition can be executed by a client, and the client can be user terminal equipment such as a computer, a mobile phone, a tablet and the like; the client can be loaded with various application programs including application programs of calculation analysis class and used for presenting a picture of data analysis. By way of example, the client may include a display screen for presenting a user interface for presenting a picture of data analysis and interacting with a user, and a processor; the processor is configured to run a computational analysis program, generate a user interface, and control the display of the user interface on the display screen.
Specifically, the method includes steps S11 to S13:
s11, analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method, and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
s12, adopting an orthogonal test method, and obtaining a plurality of test conditions according to the value range of the test influence factors;
s13, comparing and analyzing test results of evaporation loss measurement of the known sample under each test condition according to the evaporation loss results of the known sample acquired in advance, and determining the optimal test condition.
In step S11, as an example, a known sample is placed in a crucible device, an experiment is performed by using a thermogravimetric analyzer with each change of the value of the experimental influence factor by using a controlled variable method, a thermogravimetric analysis chart of the known sample corresponding to each experiment is obtained, and the value range of each experimental influence factor is determined by analyzing and comparing all the thermogravimetric analysis charts; specifically, the crucible device is an aluminum crucible device and comprises a crucible and a matched crucible cover, wherein the crucible cover is provided with at least one through hole opened by a needle head with a certain outer diameter, the crucible cover and the crucible are sealed (the through hole is not sealed) by a sample sealing machine, and the sealed empty crucible mass and the mass of an added known sample are respectively weighed by a microbalance for subsequent calculation of evaporation loss.
In step S12, the orthogonal test method is a design method for researching multiple factors and multiple levels, and selects partial representative points from the overall test according to orthogonality for testing, wherein the representative points have the characteristics of uniform dispersion and alignment and comparability, and the embodiment can quickly and efficiently determine the optimal combination (optimal test condition) from the value ranges corresponding to different types of test influence factors by adopting the orthogonal test method. And selecting a representative numerical value from the value range of the test influence factors, and combining the representative numerical values corresponding to the test influence factors by adopting an orthogonal test method to obtain a plurality of test conditions.
In step S13, assuming that the known sample is a brake fluid having an evaporation loss result of 76.12%, the optimum test conditions are determined based on the evaporation loss result of the known sample obtained in advance, by comparing the test results of evaporation loss measurement performed on the known sample under each test condition.
It should be noted that the known sample is not limited to the sample corresponding to the specific evaporation loss result listed above, and may be selected according to practical situations.
In this embodiment, at least two test influencing factors of evaporation loss measurement of a known sample are analyzed by utilizing a thermogravimetric analysis method, so as to determine a value range of the test influencing factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole; obtaining a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method; the optimum test conditions are determined by comparing and analyzing the test results of evaporation loss measurement of the known sample under each test condition based on the previously acquired evaporation loss results of the known sample. Therefore, the embodiment of the invention can analyze the test conditions of the evaporation loss measurement of the known sample by utilizing a thermogravimetric analysis method and an orthogonal test, and further determine the optimal test conditions so as to realize the rapid measurement of the evaporation loss of the brake fluid under the optimal test conditions.
In one embodiment, the orthogonal test method in step S12 obtains a plurality of test conditions according to the range of values of the test influencing factors, and specifically includes steps S121 to S122:
s121, determining a plurality of recommended values of the test influence factors corresponding to the test influence factors according to the value range of the test influence factors;
s122, acquiring a plurality of test conditions according to a plurality of recommended values of the test influence factors corresponding to the test influence factors by adopting an orthogonal test method.
Specifically, selecting a plurality of recommended values of the test influence factors corresponding to the test influence factors from the range of values of the test influence factors according to a preset selection rule; and combining a plurality of recommended values of the test influence factors corresponding to each test influence factor by adopting an orthogonal test method to obtain a plurality of test conditions. The selection rule can be the number of preset values, and the recommended values of the plurality of test influence factors are determined to be the arithmetic series according to the size of the value range and the number of the values. It should be noted that the selection rule is not limited to the specific rule, and the value may be taken according to the actual situation.
In one embodiment, the test influencing factors include an evaporation reference time and a diameter of the through hole;
then, the step S11 of analyzing the test conditions for evaporation loss measurement of the known sample by using the thermogravimetric analysis method and determining the range of the values of the test influencing factors specifically includes steps S111 to S112:
s111, analyzing test results of evaporation loss measurement of a plurality of known samples under different evaporation reference time by utilizing a thermogravimetric analysis method, and determining the value range of the evaporation reference time.
S112, analyzing test results of evaporation loss measurement of a plurality of known samples with different diameters by utilizing a thermogravimetric analysis method, and determining the value range of the diameters.
Specifically, the evaporation reference time refers to the total consumption of the evaporation loss measurement of the known sample, and the thermogravimetric analyzer is preset with a temperature control program before the evaporation loss measurement of the known sample.
The temperature control program of the thermogravimetric analyzer is set as an initial temperature of 40 ℃, is increased to 180 ℃ at a rate of 10 ℃/min, and is finally kept at the temperature of 180 ℃ for 25min. Referring to the typical brake fluid thermogravimetric analysis curve shown in fig. 2, the abscissa indicates the evaporation time of the brake fluid, and the ordinate indicates the mass percent of evaporation loss, and as can be seen from fig. 2, the longer the evaporation reference time is, the larger the evaporation loss result is; the evaporation reference time cannot be selected too short, which results in the evaporation reference time still being in the temperature rising section of the instrument, which affects the precision and accuracy of the test result, while too long results in the reduction of the analysis efficiency, so that the suitable reference time is selected between 20min and 35min.
It should be noted that the temperature control procedure of the thermogravimetric analyzer is not limited to the specific temperature control process, and may be set according to practical situations.
For example, the evaporation reference time is preset to be 30min, the sampling amount of a known sample for evaporation loss measurement is 10.0+/-0.2 mg, the evaporation loss measurement of the known sample is respectively carried out under different diameters by adopting a thermogravimetric analyzer, a plurality of evaporation loss results corresponding to the diameters are obtained, and the value range of the diameters is determined according to the evaporation loss results. Referring to the effect of the diameter of the through hole on the evaporation loss of the brake fluid (known sample) shown in fig. 3, it is understood from fig. 3 that, in a certain range, the larger the diameter of the through hole is, the larger the evaporation performance result (evaporation loss result) is, but too large the diameter of the through hole causes deterioration of repeatability and deformation of the crucible cover made of aluminum, while too small the diameter of the through hole causes excessively long test time.
In one embodiment, the test influencing factors further comprise a sampling amount of the known sample;
then, the step S11 of analyzing the test conditions of the evaporation loss measurement of the known sample by using the thermogravimetric analysis method to determine the value range of the test influencing factor, and the step S113 of:
And S113, analyzing test results of evaporation loss measurement of known samples under a plurality of different sampling amounts by utilizing a thermogravimetric analysis method, and determining the value range of the sampling amount.
The evaporation reference time is preset to be 30min, the diameter of the through hole is 1.52mm, evaporation loss measurement of known samples is carried out under different sampling amounts by adopting a thermogravimetric analyzer, a plurality of evaporation loss results corresponding to the sampling amounts are obtained, and the value range of the diameter is determined according to the evaporation loss results. Referring to the effect of the sampling amount on the evaporation loss of the brake fluid (known sample) shown in fig. 4, it is understood from fig. 4 that the larger the sampling amount of the brake fluid is, the smaller the evaporation performance result (evaporation loss result) is. Considering the tolerance and the test efficiency of the test instrument, the maximum sample amount adopted in the research is not more than 10mg; too small a sample size easily causes a weighing error, so the minimum sample size study range is defined as 6mg.
Further, the test influencing factors also include the gas flow rate.
Specifically, referring to FIG. 5, when the sampling amount is 10.0 mg.+ -. 0.2mg, the evaporation reference time is 30min, the diameter of the through hole is 1.52mm, the total gas flow rate is 20 mL/min-90 mL/min, the influence of the change in the gas flow rate on the evaporation loss result of the brake fluid is small, and when the total gas flow rate is 70 mL/min-90 mL/min, the fluctuation of the evaporation loss result is less than 0.4%, because the influence of the total gas flow rate on the experimental result is small in a certain range, the total gas flow rate is selected to be 80mL/min (12/48/20, i.e. oxygen is 12mL/min, nitrogen is 48mL/min, and shielding gas is 20 mL/min).
It should be noted that the test influencing factors may also include the size of the crucible, the shape of the crucible, etc., and the test influencing factors may be selectively analyzed according to actual situations.
In one embodiment, the determining, in step S121, a plurality of recommended values of the test influencing factors corresponding to the test influencing factors according to the range of values of the test influencing factors specifically includes steps S1211 to S1213:
s1211, determining a plurality of evaporation reference time recommended values according to the value range of the evaporation reference time;
s1212, determining a plurality of diameter recommended values according to the value range of the diameter;
s1213, determining a plurality of recommended sampling amount values according to the sampling amount value range;
then, in step S122, an orthogonal test method is adopted, and a plurality of test conditions are obtained according to a plurality of recommended values of test influencing factors corresponding to the test influencing factors, including:
and acquiring a plurality of test conditions according to the evaporation reference time recommended value, the diameter recommended value and the sampling amount recommended value by adopting an orthogonal test method.
As can be seen from fig. 2 to 5, the total gas flow has little influence on the experimental results in a certain range by analyzing the influence factors of the thermogravimetric analysis, and the main influence factors are the sampling amount, the diameter of the through hole and the evaporation reference time. The optimal test conditions can be rapidly determined by adopting an orthogonal test method. Referring to the orthogonality test factors and levels in FIG. 6, the sample size and evaporation reference time were 5 levels, and the diameter of the via was 3 levels for the orthogonality test, wherein the two levels 1.08mm (level 4) and 1.52mm (level 5) for the better diameter were repeated, referring to the orthogonality test design and results in FIG. 7, using L25 (5 6 ) The orthogonal test chart is designed, a brake fluid sample with the evaporation loss result of 76.12% is selected for testing, and the analysis in the table 5 shows that the optimal test condition is A 4 B 4 C 2 Namely, when the sample amount (sampling amount) was 9 mg.+ -. 0.2mg, the pore diameter (diameter of the through hole) was 1.52mm, and the evaporation reference time was 32min, the evaporation loss of the brake fluid was 76.65%, which was closest to the reference value of 76.12%. By extremely poor analysis, the primary and secondary sequences of the factors affecting the evaporation loss of the brake fluid are evaporation reference time>Pore diameter>Sampling amount.
In summary, compared with the prior art, the method for determining the evaporation loss measurement test conditions disclosed by the embodiment of the invention can analyze the test conditions of the evaporation loss measurement of the known sample by utilizing a thermogravimetric analysis method and an orthogonal test, and further determine the optimal test conditions so as to realize the rapid determination of the evaporation loss of the brake fluid under the optimal test conditions.
In order to ensure the stability of the evaporation loss result measurement of the brake fluid under the optimal test conditions, which is obtained by the determination method of the evaporation loss measurement test disclosed by the embodiment of the invention, the evaporation loss result of the brake fluid sample is repeatedly measured under the optimal test conditions: referring to fig. 8, 4 different types of brake fluid samples were selected for 5 repeated determinations to verify the precision of the method, and the 4 different types of brake fluids were analyzed with evaporation losses ranging from 56% to 99% and a relative standard deviation of less than 1.3%, which indicated that the evaporation loss results of the brake fluid could be stably determined under the optimal test conditions obtained in the examples of the present invention.
In order to ensure the accuracy of the evaporation loss result measurement (thermogravimetric analysis) of the brake fluid by applying the optimal test conditions obtained by the determination method of the evaporation loss measurement experiment disclosed by the embodiment of the invention to the determination of the evaporation loss result of the brake fluid, the determination of the evaporation loss result is carried out on 50 brake fluids by utilizing the national standard method (GB 12981-2012 annex H) and the optimal test conditions obtained by the embodiment of the invention respectively, see the comparison analysis result of the thermogravimetric analysis method and the GB12981-2012 annex H shown in FIG. 9, the difference value of different methods is calculated by comparing the data of the thermogravimetric analysis method and the data of the GB12981-2012 annex H, the evaporation loss of the brake fluid in the range of 39% -99% is calculated, the evaporation loss difference value of 64% of the sample is within 5%, the evaporation loss difference value of 80% of the sample is within 10%, the results of 12 brake fluid samples tested failed according to the GB12981-2012 annex H (the evaporation loss is greater than 80%), the results tested by the thermogravimetric analysis method are failed, and the results tested by the thermogravimetric analysis method are both qualified. Therefore, the evaporation loss of the brake fluid is tested by utilizing a thermogravimetric analysis method, so that the accuracy is better; it is worth to say that the data measurement and calculation instrument comprises a TG 209F 3 thermogravimetric analyzer of NETZSCH company, a DLX-191 brake fluid evaporation loss tester of Dalian electronic instrument limited company and a XPE26 METTLER TOLEDO microbalance of METTLER TOLEDO company, switzerland; it should be noted that the adopted apparatus is not limited to the specific model, and the apparatus may be selected according to the actual implementation.
Referring to fig. 10, a schematic structural diagram of a determining device for determining evaporation loss test conditions according to an embodiment of the present invention is shown. The evaporation loss measurement test condition determining apparatus 10 includes:
the influence factor range determining module 11 is used for analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
the test condition acquisition module 12 is used for acquiring a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method;
the optimal test condition determining module 13 is configured to determine optimal test conditions according to the evaporation loss result of the known sample obtained in advance, and compare and analyze the test result of evaporation loss measurement performed on the known sample under each test condition.
In the influence factor range determining module 11, for example, a known sample is placed in a crucible device, an experiment is performed every time the value of the influence factor of the experiment is changed by using a thermogravimetric analyzer by using a control variable method, a thermogravimetric analysis chart of the known sample corresponding to each experiment is obtained, and the value range of each experiment influence factor is determined by analyzing and comparing all the thermogravimetric analysis charts; specifically, the crucible device is an aluminum crucible device and comprises a crucible and a matched crucible cover, wherein the crucible cover is provided with at least one through hole opened by a needle head with a certain outer diameter, the crucible cover and the crucible are sealed (the through hole is not sealed) by a sample sealing machine, and the sealed empty crucible mass and the mass of an added known sample are respectively weighed by a microbalance for subsequent calculation of evaporation loss.
In the test condition acquisition module 12, the orthogonal test method is a design method for researching multiple factors and multiple levels, and is to select partial representative points from the overall test according to orthogonality for testing, wherein the representative points have the characteristics of uniform dispersion and uniformity and comparability, and the optimal combination (optimal test condition) can be quickly and efficiently determined from the value ranges corresponding to different types of test influence factors by adopting the orthogonal test method. And selecting a representative numerical value from the value range of the test influence factors, and combining the representative numerical values corresponding to the test influence factors by adopting an orthogonal test method to obtain a plurality of test conditions.
In the optimum test condition determining module 13, assuming that the known sample is a brake fluid whose evaporation loss result is 76.12%, the optimum test conditions are determined by comparing and analyzing the test results of evaporation loss measurement of the known sample under each test condition based on the evaporation loss result of the known sample acquired in advance.
It should be noted that the known sample is not limited to the sample corresponding to the specific evaporation loss result listed above, and may be selected according to practical situations.
In the present embodiment, the determination device 10 of the evaporation loss measurement test condition analyzes at least two test influencing factors of the evaporation loss measurement of the known sample by using the thermogravimetric analysis method, thereby determining the value range of the test influencing factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole; obtaining a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method; the optimum test conditions are determined by comparing and analyzing the test results of evaporation loss measurement of the known sample under each test condition based on the previously acquired evaporation loss results of the known sample. Therefore, the determination device 10 for evaporation loss measurement test conditions provided in the embodiment of the invention can analyze the test conditions of evaporation loss measurement of the known sample by using a thermogravimetric analysis method and an orthogonal test, and further determine the optimal test conditions, so as to realize rapid determination of evaporation loss of the brake fluid under the optimal test conditions.
In one embodiment, referring to fig. 11, the test condition acquisition module 12 specifically includes:
a recommendation value determining unit 121, configured to determine a plurality of recommendation values of test influencing factors corresponding to the test influencing factors according to the value range of the test influencing factors;
and a test condition acquisition unit 122, configured to acquire a plurality of test conditions according to a plurality of recommended values of test influencing factors corresponding to the test influencing factors by using an orthogonal test method.
Specifically, selecting a plurality of recommended values of the test influence factors corresponding to the test influence factors from the range of values of the test influence factors according to a preset selection rule; and combining a plurality of recommended values of the test influence factors corresponding to each test influence factor by adopting an orthogonal test method to obtain a plurality of test conditions. The selection rule can be the number of preset values, and the recommended values of the plurality of test influence factors are determined to be the arithmetic series according to the size of the value range and the number of the values. It should be noted that the selection rule is not limited to the specific rule, and the value may be taken according to the actual situation.
In one embodiment, the test influencing factors include an evaporation reference time and a diameter of the through hole;
Then, referring to fig. 12, the influence factor range determining module 11 specifically includes:
and the evaporation reference time range determining unit 111 is used for analyzing the test results of evaporation loss measurement of the known samples under a plurality of different evaporation reference times by utilizing a thermogravimetric analysis method and determining the value range of the evaporation reference time.
A diameter range determining unit 112 for analyzing the test results of evaporation loss measurement of known samples at several different diameters by using thermogravimetric analysis, and determining the value range of the diameters.
Specifically, the evaporation reference time refers to the total consumption of the evaporation loss measurement of the known sample, and the thermogravimetric analyzer is preset with a temperature control program before the evaporation loss measurement of the known sample.
The temperature control program of the thermogravimetric analyzer is set as an initial temperature of 40 ℃, is increased to 180 ℃ at a rate of 10 ℃/min, and is finally kept at the temperature of 180 ℃ for 25min. Referring to the typical brake fluid thermogravimetric analysis curve shown in fig. 2, the abscissa indicates the evaporation time of the brake fluid, and the ordinate indicates the mass percent of evaporation loss, and as can be seen from fig. 2, the longer the evaporation reference time is, the larger the evaporation loss result is; the evaporation reference time cannot be selected too short, which results in the evaporation reference time still being in the temperature rising section of the instrument, which affects the precision and accuracy of the test result, while too long results in the reduction of the analysis efficiency, so that the suitable reference time is selected between 20min and 35min.
It should be noted that the temperature control procedure of the thermogravimetric analyzer is not limited to the specific temperature control process, and may be set according to practical situations.
For example, the preset evaporation reference time is 30min, the sampling amount of a known sample for evaporation loss measurement is 10.0 mg+/-0.2 mg, the evaporation loss measurement of the known sample is respectively carried out under different diameters by adopting a thermogravimetric analyzer, a plurality of evaporation loss results corresponding to the diameters are obtained, and the value range of the diameters is determined according to the evaporation loss results. Referring to the effect of the diameter of the through hole on the evaporation loss of the brake fluid (known sample) shown in fig. 3, it is understood from fig. 3 that, in a certain range, the larger the diameter of the through hole is, the larger the evaporation performance result (evaporation loss result) is, but too large the diameter of the through hole causes deterioration of repeatability and deformation of the crucible cover made of aluminum, while too small the diameter of the through hole causes excessively long test time.
In one embodiment, the test influencing factors further comprise a sampling amount of the known sample;
then, referring to fig. 13, the influence factor range determining module 11 further includes a sampling amount range determining unit 113:
and the sampling amount range determining unit 113 is used for analyzing the test results of evaporation loss measurement of the known samples under a plurality of different sampling amounts by utilizing a thermogravimetric analysis method and determining the value range of the sampling amount.
The evaporation reference time is preset to be 30min, the diameter of the through hole is 1.52mm, evaporation loss measurement of known samples is carried out under different sampling amounts by adopting a thermogravimetric analyzer, a plurality of evaporation loss results corresponding to the sampling amounts are obtained, and the value range of the diameter is determined according to the evaporation loss results. Referring to the effect of the sampling amount on the evaporation loss of the brake fluid (known sample) shown in fig. 4, it is understood from fig. 4 that the larger the sampling amount of the brake fluid is, the smaller the evaporation performance result (evaporation loss result) is. Considering the tolerance and the test efficiency of the test instrument, the maximum sample amount adopted in the research is not more than 10mg; too small a sample size easily causes a weighing error, so the minimum sample size study range is defined as 6mg.
It should be noted that, the working process of the specific evaporation loss measurement test condition determining device 10 may refer to the working process of the evaporation loss measurement test condition determining method in the above embodiment, and will not be described herein.
Referring to fig. 14, there is provided a determining apparatus 20 for evaporation loss measurement test conditions according to an embodiment of the present invention, including a processor 21, a memory 22, and a computer program stored in the memory 22 and configured to be executed by the processor 21, the steps in the determining method embodiment of the evaporation loss measurement test conditions being implemented by the processor 21 when the computer program is executed, for example, steps S11 to S14 described in fig. 1; alternatively, the processor 21 may implement the functions of the modules in the above-described apparatus embodiments, such as the influence factor range determining module 11, when executing the computer program.
Illustratively, the computer program may be split into one or more modules that are stored in the memory 22 and executed by the processor 21 to complete the present invention. The one or more modules may be a series of computer program instruction segments capable of performing a specific function for describing the execution of the computer program in the evaporation loss determination test condition determination device 20. For example, the computer program may be divided into an influence factor range determination module 11, a test condition acquisition module 12, and an optimum test condition determination module 13, each of which functions specifically as follows:
the influence factor range determining module 11 is used for analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
the test condition acquisition module 12 is used for acquiring a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method;
The optimal test condition determining module 13 is configured to determine optimal test conditions according to the evaporation loss result of the known sample obtained in advance, and compare and analyze the test result of evaporation loss measurement performed on the known sample under each test condition.
The specific operation of each module may refer to the operation of the determining device 10 for determining evaporation loss measurement test conditions described in the above embodiments, and will not be described herein.
The determining device 20 for determining the evaporation loss measurement test condition may be a computing device such as a desktop computer, a notebook computer, a palm computer, a cloud server, etc. The determining device 20 of the evaporation loss measurement test conditions may include, but is not limited to, a processor 21, a memory 22. It will be appreciated by those skilled in the art that the schematic diagram is merely an example of a determination device of evaporation loss measurement test conditions, and does not constitute a limitation of the determination device 20 of evaporation loss measurement test conditions, and may include more or less components than those illustrated, or may combine certain components, or different components, for example, the determination device 20 of evaporation loss measurement test conditions may further include an input-output device, a network access device, a bus, and the like.
The processor 21 may be a central processing unit (Central Processing Unit, CPU), but may also be other general purpose processors, digital signal processors (Digital Signal Processor, DSP), application specific integrated circuits (Application Specific Integrated Circuit, ASIC), off-the-shelf programmable gate arrays (Field-Programmable Gate Array, FPGA) or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, or the like. The general purpose processor may be a microprocessor or the processor may be any conventional processor or the like, and the processor 21 is a control center of the evaporation loss measurement test condition determining apparatus 20, and connects the respective parts of the entire evaporation loss measurement test condition determining apparatus 20 using various interfaces and lines.
The memory 22 may be used to store the computer program and/or module, and the processor 31 may implement the various functions of the evaporation loss measurement test condition determining apparatus 20 by executing or executing the computer program and/or module stored in the memory 22 and invoking data stored in the memory 22. The memory 22 may mainly include a storage program area and a storage data area, wherein the storage program area may store an operating system, an application program (such as a sound playing function, an image playing function, etc.) required for at least one function, and the like; the storage data area may store data (such as audio data, phonebook, etc.) created according to the use of the handset, etc. In addition, the memory 22 may include high-speed random access memory, and may also include non-volatile memory, such as a hard disk, memory, plug-in hard disk, smart Media Card (SMC), secure Digital (SD) Card, flash Card (Flash Card), at least one disk storage device, flash memory device, or other volatile solid-state storage device.
The module integrated by the evaporation loss measurement test condition determining apparatus 20 may be stored in a computer-readable storage medium if implemented as a software functional unit and sold or used as a separate product. Based on such understanding, the present invention may implement all or part of the flow of the method of the above embodiment, or may be implemented by a computer program to instruct related hardware, where the computer program may be stored in a computer readable storage medium, and when the computer program is executed by a processor, the computer program may implement the steps of each of the method embodiments described above. Wherein the computer program comprises computer program code which may be in source code form, object code form, executable file or some intermediate form etc. The computer readable medium may include: any entity or device capable of carrying the computer program code, a recording medium, a U disk, a removable hard disk, a magnetic disk, an optical disk, a computer Memory, a Read-Only Memory (ROM), a random access Memory (RAM, random Access Memory), an electrical carrier signal, a telecommunications signal, a software distribution medium, and so forth.
Those skilled in the art will appreciate that implementing all or part of the above-described methods in accordance with the embodiments may be accomplished by way of a computer program stored on a computer readable storage medium, which when executed may comprise the steps of the embodiments of the methods described above. The storage medium may be a magnetic disk, an optical disk, a Read-only memory (ROM), a random access memory (RandomAccessMemory, RAM), or the like.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.
Claims (8)
1. A method for determining evaporation loss measurement test conditions, comprising:
analyzing at least two test influence factors of evaporation loss measurement of a known sample by utilizing a thermogravimetric analysis method, and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
Adopting an orthogonal test method, and obtaining a plurality of test conditions according to the value range of the test influence factors;
according to the evaporation loss results of the known samples obtained in advance, comparing and analyzing the test results of evaporation loss measurement of the known samples under each test condition, and determining the optimal test conditions;
the test influencing factors comprise evaporation reference time and the diameter of the through hole;
then, the analysis of the test conditions of evaporation loss measurement of the known sample by using the thermogravimetric analysis method, the determination of the value range of the test influence factor specifically includes:
analyzing test results of evaporation loss measurement of a plurality of known samples under different evaporation reference time by utilizing a thermogravimetric analysis method, and determining a value range of the evaporation reference time;
and analyzing the test results of evaporation loss measurement of the known samples with different diameters by utilizing a thermogravimetric analysis method, and determining the value range of the diameters.
2. The method for determining evaporation loss measurement test conditions according to claim 1, wherein said obtaining a plurality of test conditions according to the range of values of said test influencing factors by using an orthogonal test method comprises:
Determining a plurality of recommended values of the test influence factors corresponding to the test influence factors according to the value range of the test influence factors;
and acquiring a plurality of test conditions according to a plurality of recommended values of the test influence factors corresponding to the test influence factors by adopting an orthogonal test method.
3. The method for determining evaporation loss measurement test condition according to claim 1, wherein said test influencing factor further comprises a sampling amount of said known sample;
then, the analyzing the test condition of the evaporation loss measurement of the known sample by using the thermogravimetric analysis method to determine the value range of the test influencing factor further comprises:
and analyzing the test results of evaporation loss measurement of the known samples under a plurality of different sampling amounts by utilizing a thermogravimetric analysis method, and determining the value range of the sampling amounts.
4. The method for determining evaporation loss measurement test conditions according to claim 3, wherein determining a plurality of recommended values of the test influencing factors corresponding to the test influencing factors according to the range of values of the test influencing factors comprises:
determining a plurality of recommended evaporation reference time values according to the value range of the evaporation reference time;
Determining a plurality of diameter recommended values according to the value range of the diameter;
determining a plurality of recommended sampling quantity values according to the sampling quantity value range;
and acquiring a plurality of test conditions by adopting an orthogonal test method according to a plurality of recommended values of the test influence factors corresponding to the test influence factors, wherein the method specifically comprises the following steps:
and acquiring a plurality of test conditions according to the evaporation reference time recommended value, the diameter recommended value and the sampling amount recommended value by adopting an orthogonal test method.
5. A device for determining evaporation loss measurement test conditions, comprising:
the influence factor range determining module is used for analyzing at least two test influence factors of evaporation loss determination of a known sample by utilizing a thermogravimetric analysis method and determining the value range of the test influence factors; the known sample is a sample with known evaporation performance, and is contained in a crucible device when evaporation loss is measured, wherein the crucible device comprises a crucible and a crucible cover, and the crucible cover is provided with at least one through hole;
the test condition acquisition module is used for acquiring a plurality of test conditions according to the value range of the test influence factors by adopting an orthogonal test method;
The optimal test condition determining module is used for comparing and analyzing the test result of the evaporation loss measurement of the known sample under each test condition according to the evaporation loss result of the known sample acquired in advance, and determining the optimal test condition;
the test influencing factors comprise evaporation reference time and the diameter of the through hole;
the influence factor range determining module specifically includes:
the evaporation reference time range determining unit is used for analyzing test results of evaporation loss determination of a plurality of known samples under different evaporation reference time by utilizing a thermogravimetric analysis method and determining the value range of the evaporation reference time;
and the diameter range determining unit is used for analyzing the test results of evaporation loss measurement of the known samples with different diameters by utilizing a thermogravimetric analysis method and determining the value range of the diameters.
6. The evaporation loss measurement test condition determining apparatus according to claim 5, wherein said test condition obtaining module comprises:
the recommended value determining unit is used for determining a plurality of recommended values of the test influence factors corresponding to the test influence factors according to the value range of the test influence factors;
And the test condition acquisition unit is used for acquiring a plurality of test conditions according to a plurality of recommended values of the test influence factors corresponding to the test influence factors by adopting an orthogonal test method.
7. A determination device of evaporation loss measurement test conditions, characterized by comprising a processor, a memory and a computer program stored in the memory and configured to be executed by the processor, the processor implementing the determination method of evaporation loss measurement test conditions according to any one of claims 1 to 4 when executing the computer program.
8. A computer-readable storage medium, characterized in that the computer-readable storage medium comprises a stored computer program, wherein the computer program, when run, controls a device in which the computer-readable storage medium is located to perform the method of determining the evaporation loss measurement test condition according to any one of claims 1 to 4.
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