CN111780835A - Calibration method for high-efficiency liquid phase transfer liquid flowmeter - Google Patents
Calibration method for high-efficiency liquid phase transfer liquid flowmeter Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 166
- 239000007791 liquid phase Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 239000012530 fluid Substances 0.000 claims abstract description 12
- 238000005259 measurement Methods 0.000 claims description 82
- 238000004128 high performance liquid chromatography Methods 0.000 description 13
- 238000005303 weighing Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01F25/00—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume
- G01F25/10—Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume of flowmeters
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Abstract
The invention discloses a method for calibrating a high-efficiency liquid-phase transfer liquid flowmeter, and relates to the technical field of high-efficiency liquid-phase transfer liquid flowmeter calibration. The main technical scheme of the invention is as follows: a method of calibrating a high performance liquid phase dispense fluid flow meter, comprising: selecting a plurality of measuring points in the measuring range of the high-efficiency liquid-phase transfer liquid flowmeter, and acquiring the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point, the quality of liquid flowing through each measuring point and the elapsed time of each measuring point; obtaining the indication value error of the high-efficiency liquid-phase transfer liquid flowmeter according to the measured value of each measured high-efficiency liquid-phase transfer liquid flowmeter, the mass of liquid flowing through each measuring point and the time elapsed by each measuring point; obtaining a repeatability detection result of the high-efficiency liquid phase transfer liquid flowmeter according to the indication error; and calibrating the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error and the repeatability detection result.
Description
Technical Field
The invention relates to the technical field of high-efficiency liquid-phase transfer liquid flowmeter calibration, in particular to a method for calibrating a high-efficiency liquid-phase transfer liquid flowmeter.
Background
The high performance liquid phase transfer liquid flowmeter is used for measuring the liquid flow rate of a carrier flow system in a high performance liquid chromatography system and can also be used for controlling the liquid flow of a branch system of precision flow control, the measurement range is 50 ul-25 mL, the accuracy requirement is +/-1%, and the repeatability requirement is +/-0.5%. The flowmeter is widely applied to chromatographic measuring instruments, particularly high performance liquid chromatographs, and has small flow and high precision, so that no standard calibration method is available at present for calibrating the flowmeter so as to ensure the measuring quality of the flowmeter.
Accordingly, providing a calibration method for a high performance liquid phase dispense fluid flow meter is a problem that needs to be addressed.
Disclosure of Invention
In view of this, the present invention provides a calibration method for a high performance liquid phase transfer liquid flow meter, and mainly aims to calibrate the high performance liquid phase transfer liquid flow meter.
In one aspect, the present invention provides a method for calibrating a high performance liquid phase dispense fluid flow meter, comprising:
selecting a plurality of measuring points in the measuring range of the high-efficiency liquid-phase transfer liquid flowmeter, and acquiring the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point, the quality of liquid flowing through each measuring point and the elapsed time of each measuring point;
obtaining an indication error of the high-efficiency liquid-phase transfer liquid flowmeter according to the measured value of the high-efficiency liquid-phase transfer liquid flowmeter, the mass of liquid flowing through each measuring point and the time elapsed by each measuring point;
obtaining a repeatability detection result of the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error;
and calibrating the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error and the repeatability detection result.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
In this embodiment, the obtaining an indication error of the hplc flowmeters according to the measured value of each measured hplc flowmeter, the mass of the liquid flowing through each measurement point, and the elapsed time at each measurement point includes:
obtaining the standard instantaneous volume flow of each measuring point according to the mass of the liquid flowing through each measuring point and the time elapsed by each measuring point;
obtaining the indicating value error corresponding to each measuring point according to the standard instantaneous volume flow of each measuring point and the measured value of each measuring point;
and selecting the indicating value error of the high-efficiency liquid-phase transfer liquid flowmeter from the indicating value errors of the plurality of measuring points.
In this embodiment, the obtaining the standard instantaneous volume flow rate of each measurement point according to the mass of the liquid flowing through each measurement point and the elapsed time of each measurement point includes:
determining the density of the liquid according to the liquid calibration temperature;
obtaining the calculated volume of each measuring point according to the ratio of the mass of the liquid flowing through the measuring point to the density of the liquid at the liquid calibration temperature;
and obtaining the standard instantaneous volume flow of each measuring point according to the ratio of the calculated volume of each measuring point to the elapsed time of each measuring point.
In this embodiment, the obtaining an indication error corresponding to each measurement point by the standard instantaneous volume flow at each measurement point and the measured value at each measurement point includes:
the indication error is deltai，
Wherein, ViThe measured value of the ith measuring point is the measured value of the ith measuring point;
Vi0is the standard instantaneous volume flow at the ith measurement point.
In this technical solution, the obtaining a repeatability detection result of the hplc flowmeters according to the indication error of each measurement point includes:
selecting a measuring point with the largest indication value error, and obtaining the measured value of the measuring point for multiple times;
obtaining an arithmetic mean value of the measured values according to the measured values obtained for multiple times;
and obtaining a repeatability detection result of the high-efficiency liquid phase transfer liquid flowmeter according to the arithmetic mean value of the measured values.
In this technical solution, the obtaining an arithmetic average of the measured values according to the measured values obtained multiple times includes:
the arithmetic mean of the measured values is
Wherein, ViThe measured value obtained for the ith time;
n is the number of times the measured value is obtained.
In this embodiment, the obtaining a repeatability detection result of the hplc flowmeters according to the arithmetic mean of the measured values includes:
repeatability detection result S of high performance liquid phase transfer liquid flowmeternIn order to realize the purpose,
wherein,
calculating a numerical average for said measured values;
Viis the measured value obtained at the ith time.
In this technical solution, the selecting an indication error of the high performance liquid phase transfer liquid flowmeter from the indication errors of the plurality of measurement points includes:
and selecting the indicating error with the largest error value from the indicating errors of the plurality of measuring points as the indicating error of the high-efficiency liquid phase transfer liquid flowmeter.
In the technical scheme, the measuring range of the high-efficiency liquid phase transfer liquid flowmeter is 50 ul-25 ml.
In this embodiment, the number of the measurement points is 4, which are 0.5ml, 1ml, 10ml and 20ml, respectively.
The invention provides a calibration method of a high-efficiency liquid-phase transfer liquid flowmeter, which comprises the steps of selecting a plurality of measuring points in a measuring range of the high-efficiency liquid-phase transfer liquid flowmeter, obtaining an actual measurement value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point, the quality of liquid passing through each measuring point and the time required by each measuring point, obtaining an indication error of the high-efficiency liquid-phase transfer liquid flowmeter according to the actual measurement value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point and the quality of liquid passing through each measuring point in a certain time, obtaining a repeatability detection result of the high-efficiency liquid-phase transfer liquid flowmeter according to the indication error of the high-efficiency liquid-phase transfer liquid flowmeter, and finally calibrating the high-efficiency liquid-phase transfer liquid flowmeter according to the indication error and the repeatability detection result. The calibration method of the high performance liquid chromatography liquid flowmeter provided by the invention can calibrate the high performance liquid chromatography liquid flowmeter which has small flow and high precision and is used for measuring the liquid flow rate of a carrier flow system in a high performance liquid chromatography system and the liquid flow control of a precision flow control branch system.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic flow chart of a method for calibrating a high performance liquid switching fluid flow meter according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of another method for calibrating a high performance liquid phase dispense fluid flow meter according to an embodiment of the present invention;
fig. 3 is an installation diagram of a calibration method for a hplc flowmeter according to an embodiment of the present invention.
Reference numerals and descriptions:
the high performance liquid phase is transferred to a liquid flowmeter 10, a volumetric flask 12 and a balance 14.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to the embodiments, structures, features and effects of a calibration method for a high performance liquid phase transfer liquid flow meter according to the present invention with reference to the accompanying drawings and preferred embodiments.
An embodiment of the present invention provides a calibration method for a high-efficiency liquid-phase-transfer liquid flowmeter, as shown in fig. 1, the method includes:
as shown in FIG. 3, in the calibration method of the high efficiency liquid phase transfer liquid flowmeter 10, a stopwatch, a single-line volumetric flask 12, a 0.1 ℃ graduated glass liquid thermometer or a platinum resistance thermometer and an electronic balance 14 are required as tools, the volumetric flask 12 is arranged below the high efficiency liquid flow meter 10, the electronic balance 14 is arranged below the volumetric flask 12, the liquid metered by the high efficiency liquid flow meter 10 flows into the volumetric flask 12 for weighing, when the calibration is performed, the pumping stability of the high efficiency liquid flow meter 10 is firstly determined, on the premise that the flow rate of a pipeline is stable, the mass of the liquid flowing through the high efficiency liquid flow meter 10 at each measuring point and the actual measurement value of the high efficiency liquid flow meter 10 and the mass of the liquid flowing through each measuring point are obtained by weighing for a certain time, the measuring range of the high efficiency liquid flow meter 10 is 50 ul-25 ml, and a plurality of measuring points are selected between 50 ul-25 ml, and the time is counted by a stopwatch in the measuring process, so that the time elapsed after the liquid completely flows at each measuring point is obtained.
102, obtaining an indication error of the high-efficiency liquid-phase transfer liquid flowmeter according to an actually measured value of the high-efficiency liquid-phase transfer liquid flowmeter, the mass of liquid flowing through each measuring point and the elapsed time of each measuring point;
103, obtaining a repeatability detection result of the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error;
and 104, calibrating the high-efficiency liquid-phase transfer liquid flowmeter 10 according to the indicating value error and the repeatability detection result.
In the embodiment of the invention, a plurality of measurement points are selected in the measurement range of the high efficiency liquid phase transfer liquid flowmeter 10, the actual measurement value of the high efficiency liquid phase transfer liquid flowmeter 10 of each measurement point, the mass of liquid passing through each measurement point and the time required for each measurement point to pass are obtained, the indication error of the high efficiency liquid phase transfer liquid flowmeter is obtained according to the actual measurement value of the high efficiency liquid phase transfer liquid flowmeter 10 of each measurement point and the mass of liquid passing through each measurement point in a certain time, then the repeatability detection result of the high efficiency liquid phase transfer liquid flowmeter is obtained according to the indication error of the high efficiency liquid phase transfer liquid flowmeter, and finally the high efficiency liquid phase transfer liquid flowmeter is calibrated according to the indication error and the repeatability detection result. The calibration method of the high performance liquid chromatography liquid flowmeter provided by the invention can calibrate the high performance liquid chromatography liquid flowmeter which has small flow and high precision and is used for measuring the liquid flow rate of a carrier flow system in a high performance liquid chromatography system and the liquid flow control of a precision flow control branch system.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
As shown in fig. 2, another calibration method for a high-efficiency liquid-phase transfer liquid flowmeter according to an embodiment of the present invention includes:
204, selecting the largest indication error in the indication errors of the plurality of measuring points as the indication error of the high-efficiency liquid phase transfer liquid flowmeter;
and selecting the measuring point with the largest indication value error, and repeatedly obtaining the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of the measuring point for many times.
and 208, calibrating the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error and the repeatability detection result. .
In the calibration method of the high efficiency liquid phase transfer liquid flowmeter 10, a plurality of measurement points are selected in the measurement range of the high efficiency liquid phase transfer liquid flowmeter 10, the measured value of the high efficiency liquid phase transfer liquid flowmeter 10 of each measurement point, the mass of liquid flowing through each measurement point and the elapsed time of each measurement point are obtained, the standard instantaneous volume flow of each measurement point is obtained according to the mass of the liquid passing through each measurement point and the elapsed time of each measurement point, the indication error of the corresponding measurement point is obtained according to the standard instantaneous volume flow of each measurement point and the measured value of each measurement point, the indication error with the largest error value is selected from the obtained indication errors of the plurality of measurement points to be used as the indication error of the high efficiency liquid phase transfer liquid flowmeter 10 of the invention, then the measurement point corresponding to the indication error is selected, and the measurement point is repeatedly measured for a plurality of times, the calibration method of the high performance liquid chromatography liquid flowmeter 10 provided by the invention can calibrate the high performance liquid chromatography liquid flowmeter 10 which is used for measuring the liquid flow rate of a carrier flow system in the high performance liquid chromatography system and the liquid flow control of a precision control branch system, and has small flow and high precision.
Wherein, step 202 specifically includes:
step 2021, determining the density of the liquid according to the liquid calibration temperature;
the temperature of the liquid is affected by the stabilization, and when the temperature is constant, the density of the liquid at the calibration temperature of the liquid is confirmed.
Step 2022, obtaining the calculated volume of each measuring point according to the ratio of the mass of the liquid flowing through the measuring point to the density of the liquid at the liquid calibration temperature;
the density of the liquid is different for different liquid calibration temperatures, and the density of the liquid is determined from the different liquid calibration temperatures, although the specific data corresponding to the liquid density is known for the different liquid calibration temperatures.
Step 2073, obtaining the standard instantaneous volume flow rate of each measurement point according to the ratio of the calculated volume of each measurement point to the elapsed time of each measurement point.
In this embodiment, the calculated volume V of each measurement point is obtained by weighing the mass m of liquid flowing through it, from the mass m of liquid flowing through it and the density p of the liquid,then obtaining each measurement according to the calculated volume V of each measurement point and the time passed by each measurement pointStandard instantaneous volume flow V of a measuring point0，
In this embodiment, the indication error corresponding to each measurement point is obtained by the standard instantaneous volume flow rate of each measurement point and the measured value of each measurement point, wherein the number of the measurement points may be four, and the number of the measurement points is respectively 0.5ml, 1ml, 10ml and 20ml, and the mass of the liquid at each measurement point and the elapsed time at each measurement point are respectively obtained, so as to obtain the calculated volume at each measurement point, and further obtain the standard instantaneous volume flow rate at each measurement point.
Wherein, step 203 specifically comprises:
the obtaining of the indication error corresponding to each measurement point through the standard instantaneous volume flow of each measurement point and the measured value of each measurement point comprises:
the indication error is deltai，
Wherein, ViMeasured value of the ith measurement point is in ml;
Vi0is the standard instantaneous volume flow in ml for the ith measurement point.
In this example, the standard instantaneous volume flow rates of 0.5ml, 1ml, 10ml, 20ml for each of the four measurement points were obtained by the above calculation method.
Wherein, step 206 specifically comprises:
the obtaining an arithmetic average of the measured values according to the measured values obtained a plurality of times includes:
the arithmetic mean of the measured values is
Wherein, ViThe measured value obtained for the ith time;
n is the number of times the measured value is obtained.
Selecting a measuring point corresponding to the largest indication error from the indication errors of the plurality of measuring points, repeatedly acquiring actual measured values of the measuring point for a plurality of times, and calculating an arithmetic mean value of the actual measured values acquired for the plurality of times, wherein the acquiring times is at least 10 times.
Wherein step 207 specifically comprises:
the obtaining of the repeatability detection result of the hplc flowmeters 10 according to the arithmetic mean of the measured values comprises:
repeatability detection result S of high performance liquid phase transfer liquid flowmeternIn order to realize the purpose,
wherein,
calculating a numerical average for said measured values;
Viis the measured value obtained at the ith time.
In this embodiment, after the arithmetic mean of the measurement points is calculated, the repeatability detection structure of the hplc flowmeters 10 is obtained by the method of calculating the repeatability detection results.
In the embodiment of the invention, the measuring range of the high-efficiency liquid phase transfer liquid flowmeter 10 is 50 ul-25 ml.
In this embodiment, the high efficiency liquid phase dispense fluid flow meter 10 may also be other measurement ranges.
In the present example, the number of measurement points was 4, and was 0.5ml, 1ml, 10ml and 20ml, respectively.
In this embodiment, the number of the measurement points may be other numbers, 6, 10, etc. The more the number is, the more accurate the calibration is, the other points can be selected as the measuring points, as long as the method is suitable for testing.
In the embodiment of the invention, a plurality of measuring points are selected in the measuring range of the high-efficiency liquid-phase transfer liquid flowmeter, the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point, the quality of liquid passing through each measuring point and the time required for each measuring point to pass are obtained, the indication value error of the high-efficiency liquid-phase transfer liquid flowmeter is obtained according to the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point and the quality of liquid passing through each measuring point in a certain time, then the repeatability detection result of the high-efficiency liquid-phase transfer liquid flowmeter is obtained according to the indication value error of the high-efficiency liquid-phase transfer liquid flowmeter, and finally the high-efficiency liquid-phase transfer liquid flowmeter is calibrated according to the indication value error and the repeatability detection result. The calibration method of the high performance liquid chromatography liquid flowmeter provided by the invention can calibrate the high performance liquid chromatography liquid flowmeter which has small flow and high precision and is used for measuring the liquid flow rate of a carrier flow system in a high performance liquid chromatography system and the liquid flow control of a precision flow control branch system.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A calibration method for a high-efficiency liquid-phase to liquid-phase transfer flowmeter is characterized by comprising the following steps:
selecting a plurality of measuring points in the measuring range of the high-efficiency liquid-phase transfer liquid flowmeter, and acquiring the measured value of the high-efficiency liquid-phase transfer liquid flowmeter of each measuring point, the quality of liquid flowing through each measuring point and the elapsed time of each measuring point;
obtaining an indication error of the high-efficiency liquid-phase transfer liquid flowmeter according to the measured value of the high-efficiency liquid-phase transfer liquid flowmeter, the mass of liquid flowing through each measuring point and the time elapsed by each measuring point;
obtaining a repeatability detection result of the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error;
and calibrating the high-efficiency liquid-phase transfer liquid flowmeter according to the indicating value error and the repeatability detection result.
2. The method of calibrating a hplc flowmeter of claim 1, wherein said deriving a value error of said hplc flowmeter from each measured value of said hplc flowmeter, a mass of liquid flowing through each measurement point, and an elapsed time at each measurement point comprises:
obtaining the standard instantaneous volume flow of each measuring point according to the mass of the liquid flowing through each measuring point and the time elapsed by each measuring point;
obtaining the indicating value error corresponding to each measuring point according to the standard instantaneous volume flow of each measuring point and the measured value of each measuring point;
and selecting the indicating value error of the high-efficiency liquid-phase transfer liquid flowmeter from the indicating value errors of the plurality of measuring points.
3. The method of calibrating a high efficiency liquid phase dispense fluid flow meter according to claim 2, wherein said deriving a standard instantaneous volumetric flow rate for each measurement point from the mass of liquid flowing through each measurement point and the elapsed time for each measurement point comprises:
determining the density of the liquid according to the liquid calibration temperature;
obtaining the calculated volume of each measuring point according to the ratio of the mass of the liquid flowing through the measuring point to the density of the liquid at the liquid calibration temperature;
and obtaining the standard instantaneous volume flow of each measuring point according to the ratio of the calculated volume of each measuring point to the elapsed time of each measuring point.
4. The method of calibrating a hplc flowmeter of claim 2, wherein said obtaining an indication error for each measurement point from said standard instantaneous volumetric flow rate for each measurement point and said measured value for each measurement point comprises:
the indication error is deltai，
Wherein, ViThe measured value of the ith measuring point is the measured value of the ith measuring point;
Vi0is the standard instantaneous volume flow at the ith measurement point.
5. The method of calibrating a hplc flowmeter of claim 1, wherein said obtaining a repeatability measurement of said hplc flowmeter based on said error in the readings of each measurement point comprises:
selecting a measuring point with the largest indication value error, and obtaining the measured value of the measuring point for multiple times;
obtaining an arithmetic mean value of the measured values according to the measured values obtained for multiple times;
and obtaining a repeatability detection result of the high-efficiency liquid phase transfer liquid flowmeter according to the arithmetic mean value of the measured values.
6. The method of calibrating a high efficiency liquid phase dispense fluid flow meter according to claim 5, wherein said obtaining an arithmetic mean of said measured values from said measured values obtained a plurality of times comprises:
the arithmetic mean of the measured values is
Wherein, ViThe measured value obtained for the ith time;
n is the number of times the measured value is obtained.
7. The method of calibrating a hplc flowmeter of claim 5, wherein said obtaining a repeatability test of said hplc flowmeter based on an arithmetic mean of said measured values comprises:
repeatability detection result S of high performance liquid phase transfer liquid flowmeternIn order to realize the purpose,
wherein,
calculating a numerical average for said measured values;
Viis the measured value obtained at the ith time.
8. The method of calibrating a high efficiency liquid phase dispense fluid flow meter according to claim 2, wherein said selecting an indication error of said high efficiency liquid phase dispense fluid flow meter from said indication errors of said plurality of measurement points comprises:
and selecting the indicating error with the largest error value from the indicating errors of the plurality of measuring points as the indicating error of the high-efficiency liquid phase transfer liquid flowmeter.
9. The method of calibrating a high efficiency liquid phase dispense fluid flow meter according to claim 1,
the measuring range of the high-efficiency liquid phase transfer liquid flowmeter is 50 ul-25 ml.
10. The method of calibrating a high efficiency liquid phase dispense fluid flow meter according to claim 9,
the number of measurement points was 4, 0.5ml, 1ml, 10ml and 20ml, respectively.
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| CN112426585A (en) * | 2020-11-20 | 2021-03-02 | 南京信息职业技术学院 | Insulin pump metering calibration method |
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