CN110057417A - A kind of micrometeor and ultra micro flow rate-measuring device and method - Google Patents

A kind of micrometeor and ultra micro flow rate-measuring device and method Download PDF

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Publication number
CN110057417A
CN110057417A CN201910270785.7A CN201910270785A CN110057417A CN 110057417 A CN110057417 A CN 110057417A CN 201910270785 A CN201910270785 A CN 201910270785A CN 110057417 A CN110057417 A CN 110057417A
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CN
China
Prior art keywords
micrometeor
ultra micro
flow rate
micro flow
measuring device
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201910270785.7A
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Chinese (zh)
Inventor
李明
马昱
卢俊锋
陈才
陈锦峰
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SHANGHAI WUFENG SCIENTIFIC INSTRUMENTS CO Ltd
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SHANGHAI WUFENG SCIENTIFIC INSTRUMENTS CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by SHANGHAI WUFENG SCIENTIFIC INSTRUMENTS CO Ltd filed Critical SHANGHAI WUFENG SCIENTIFIC INSTRUMENTS CO Ltd
Priority to CN201910270785.7A priority Critical patent/CN110057417A/en
Publication of CN110057417A publication Critical patent/CN110057417A/en
Priority to CN201910821672.1A priority patent/CN110455364B/en
Priority to CN201921440467.2U priority patent/CN210719297U/en
Pending legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01FMEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F11/00Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it
    • G01F11/006Details or accessories
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01FMEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F11/00Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it
    • G01F11/28Apparatus requiring external operation adapted at each repeated and identical operation to measure and separate a predetermined volume of fluid or fluent solid material from a supply or container, without regard to weight, and to deliver it with stationary measuring chambers having constant volume during measurement

Abstract

The invention discloses a kind of micrometeor and ultra micro flow rate-measuring devices, comprising: vacuum degassing machine, tested infusion pump, pressure sensor and damper tube;High-voltage electric switching valve, high-voltage electric switching valve are connected to damper tube, high-accuracy timer, waste liquid bottle and precise injection needle respectively;Precise injection needle gos deep into weighing bottle;Weighing bottle is placed in precision electronic balance, inside hold fluid to be measured (pure water), and sealed with atoleine;Precision electronic balance is placed on high stable and weighs on platform.The present invention solves the problems, such as micrometeor and ultra micro flow measurement accuracy and precision, introduce the means of the exclusion bubble of vacuum degassing machine and damper tube, switch Vavle switching flow path by the switch control high-voltage electric of high-accuracy timer, calculating to deduct influences since liquid level rises, buoyancy variation is brought, so as to Accurate Determining flow.Measurement device of the present invention has many advantages, such as that measurement is simple and fast, and measurement result is accurate and reliable.

Description

A kind of micrometeor and ultra micro flow rate-measuring device and method
Technical field
The present invention relates to liquid micro-flow and ultra micro flow measurement technical fields, especially suitable for ultra micro flow output equipment Performance detection.
Background technique
Currently, the detection for micrometeor and ultra micro flow output equipment, mainly uses mass method or flowmeter method.Matter Amount method is the quality of liquid output equipment output pure water in the unit of account time using pure water as liquid medium.Flowmeter method is logical Overcurrent meter directly detects the performance of liquid output equipment, but flowmeter used itself be also required to by mass method into Row calibration.
Currently, the mode still imperfect for the test of liquid micro-flow and ultra micro flow.There are one for mass method measurement Fixed problem, for example do not account for since liquid increase causes liquid level to be raised and then causes the variation of injection needle buoyancy in weighing bottle Problem, therefore, when carrying out micrometeor especially ultra micro flow measurement, the accuracy of existing mass method cannot be met the requirements; In existing flowmeter method due to flowmeter be calibrated by mass method, and ultra micro flowmeter precision it is difficult to ensure that, flow The range of measurement is relatively narrow, thus flowmeter method is not able to satisfy the requirement of ultra micro flow measurement.In addition, traditional flowmeter can only be Micrometeor or small flow are measured in the case where having pressure difference, is not able to satisfy the requirement of ultra micro flow measurement.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of more perfect measurement micrometeor output equipments The scheme of performance proposes a kind of micrometeor and ultra micro flow rate-measuring device, comprising:
Vacuum degassing machine, tested infusion pump, pressure sensor and damper tube;High-voltage electric switching valve, the high-voltage electric Switching valve is connected to the damper tube, high-accuracy timer, waste liquid bottle and precise injection needle respectively;The precise injection needle gos deep into In weighing bottle;The weighing bottle is placed in precision electronic balance, inside hold fluid to be measured, the surface of the fluid to be measured It is sealed with atoleine, to prevent the fluid to be measured from volatilizing in air;The precision electronic balance is placed on high stable and claims It measures on platform.
In the present invention, the vacuum degassing machine is connected to the input terminal of tested infusion pump.
In the present invention, the pressure sensor is connected to the outlet end of tested infusion pump, connects damper tube thereafter.
In the present invention, one end damper tube outlet end of the high-voltage electric switching valve, is powered and the position of power-off connects respectively It is connected to measurement pipeline and waste-solution line, and waste-solution line and measurement length of pipe are consistent.
The energization and power-off switching of heretofore described high-accuracy Timer Controlling high-voltage electric switching valve.
In the present invention, in the present invention, the precision electronic balance is placed on the weighing platform of high stable.
In the present invention, precise injection needle and measurement pipeline is fixed in the perspex frame.
In the present invention, the inner section product size of the weighing bottle is consistent.
In the present invention, the outer cross section product size of precise injection needle is consistent.
In the present invention, fluid to be measured (pure water) is sealed using atoleine.
Different degassing methods is introduced in the present invention, is sufficiently deaerated to test solution, keeps flow more stable, is improved Accuracy when micrometeor and ultra micro flow rate test.
The present invention substitutes manual control using micro computer control, more accurate for time control, and repeatability is higher, improves Method accuracy, precision.
The continuous mode of the measurement device has fully considered the influence of precise injection needle buoyancy, to ensure flow measurement Accuracy.The measurement device sufficiently combines the method and micro computer control of exhaust bubble, to improve the accuracy of flow measurement And precision.The present invention realized flow conveying include micrometeor to ultra micro flow measurement, from 1 μ L/min-5mL/min across Multiple orders of magnitude have been got over, the accurate of micro updating flow and conveying need to be studied;The shadow that flow is conveyed for pressure and temperature simultaneously It rings, influence of each parameter of comprehensive study to flow delivery precision, repeatability, precision.
The technical scheme is that weight method (executing standard: China Testing & Analysis Association's YQ00202016 standard) On the basis of, it sufficiently deaerates to fluid to be measured (pure water), fluid to be measured is through the bubble in time suction evacuation syringe pump.Using accurate fixed When high-voltage electric switching valve control fluid to be measured acquisition time, and with perspex frame fix liquid liquid-transport pipe-line, Injection needle.By calculating, the incrementss of the volume of precise injection needle are deducted.Meanwhile guaranteeing environmental condition: temperature is (15~30) DEG C, and indoor temperature fluctuation is not more than ± 2 DEG C, relative humidity is (40-60) %, and is made a record.
The invention also provides a kind of micrometeor and ultra micro flow determining methods, comprising the following steps:
(1) micro-bubble of liquid and pipeline is excluded by vacuum degassing machine and damper tube.
(2) pressure is detected by pressure sensor, guarantees the measurement for carrying out flow under a certain pressure.
(3) after pressure stabilisation, high-voltage electric is controlled by split-second timer and switches Vavle switching, is acquired.
(4) finally by calculating, influence of the buoyancy variation for measurement result is deducted.In fluid flow continuous mode, Liquid level is gradually increasing in weighing bottle.Since precise injection needle is fixed on perspex frame, and immersed in liquid level hereinafter, with Liquid level rises, and liquid buoyancy suffered by precise injection needle gradually increases, and the active force which results in injection needle to balance also gradually increases Add.Therefore, it is increased to should be precision electronic balance registration incrementss deduction injection needle buoyancy for the increased quality of practical fluid to be measured Equivalent.The rising value of fluid to be measured liquid level is calculated by quality incrementss and sectional area, and then calculates buoyancy incrementss.
Compared with prior art, the beneficial effects of the present invention are: fully considering that dissolved gas ties measurement in fluid to be measured The method that vacuum degassing machine and damper tube etc. exclude bubble is introduced the continuous mode of mass method, improves measurement by the influence of fruit Accuracy;Vavle switching is switched using high-accuracy Timer Controlling high-voltage electric to substitute manual control switching, improves measurement Accuracy and precision;It fully considers in measurement discharge process, since liquid level rising causes brought by the variation of injection needle buoyancy It influences, so that measurement result has higher accuracy.
Detailed description of the invention
Fig. 1 show the structural schematic diagram of micrometeor and ultra micro flow rate-measuring device of the present invention.
Fig. 2 is the inner section product A of weighing bottle and the outer cross section product B schematic diagram of injection needle.
Specific embodiment
In conjunction with following specific embodiments and attached drawing, the present invention is described in further detail.Implement process of the invention, Condition, experimental method etc. are among the general principles and common general knowledge in the art, this hair in addition to what is specifically mentioned below It is bright that there are no special restrictions to content.
In Fig. 1-Fig. 2,1- vacuum degassing machine, 2- is tested infusion pump, 3- pressure sensor, 4- damper tube, 5- high-voltage electric Switching valve, the high-accuracy timer of 6-, 7- waste liquid bottle, 8- high stable weigh platform, 9- precision electronic balance, 10- perspex frame Frame, 11- weighing bottle, 12- precise injection needle, 13- atoleine.
In the present invention, micrometeor and ultra micro flow rate-measuring device include 1- vacuum degassing machine, molten in liquid for excluding Solve gas.At normal temperature, gas has certain solubility in a liquid, if being not excluded for the gas in liquid, it will cause realities There are certain deviations for the amount of infusion of survey liquid quality and infusion pump.In micrometeor and ultra micro flow measurement, because of fluid course Small, influence of the viscosity for flow increases, and fine bubble, which easily gathers in piping flow process, in liquid becomes larger, when making measurement Instruction is unstable, accuracy decline.Meanwhile in measurement process, with the operation of infusion pump, gas may be escaped from liquid, from And influence the performance of infusion pump.
In the presence of no pressure, with the operation of infusion pump, remaining gas may adhere to pipe in liquid In road or infusion pump, to influence the accuracy of flow measurement.In the present invention, micrometeor and ultra micro flow rate-measuring device include 4- damper tube, damper tube can provide certain pressure in the process in infusion, in favor of excluding in infusion pump housing and pipeline Bubble.Micrometeor and ultra micro flow rate-measuring device 3- pressure sensor are used to detect pressure size in the present invention, it is ensured that certain Pressure under carry out flow measurement.
In the present invention, micrometeor and ultra micro flow rate-measuring device include 5- high-voltage electric switching valve and the high-accuracy timer of 6- (being controlled with computer), high-accuracy timer, which is equipped with, starts countdown button, timing start to terminate to respectively correspond with timing energization and Power-off switching, and then control the state switching of high-voltage electric switching valve, realize waste-solution line and measure the switching of pipeline.Wherein, The scale division value of high-accuracy timer is not more than 1ms;High-voltage electric switching valve has the function of electric control, and delay time is not more than 10ms.Traditional manual control method is to move flowpath conduit directly by operator to control switching, while using manual time-keeping Device records the time.When being switched to timer from flow path, the measurement result of manual control method is all operated by personnel horizontal Limitation, while measurement result accuracy and precision not can guarantee yet.Assuming that the total time of flow measurement is 5min, operation The reaction time of personnel is 0.15s (reaction time of normal person is 0.15-0.4s), then the accuracy error of manual control is 0.05%, and computer control accuracy error is less than 0.0033%, and repeatability is higher.In addition, high-voltage electric switching valve is cut Change that channel volume is small as far as possible, to guarantee the accuracy of measurement result.In the present invention, by having the function of electric control high pressure Dynamoelectric switching valve, what is utilized is that computer reacts fast, has the characteristics that high duplication.
In the present invention, waste-solution line and measurement length of pipe are consistent, to reduce the pressure drop in flow path handoff procedure Variation, guarantee stability of flow, improve precision of measurement, but have no related request before.
In the present invention, micrometeor and ultra micro flow rate-measuring device include that 8- high stable weighs platform, steady for placing 9- high Fixed precision electronic balance, to guarantee the stability of precision electronic balance registration.The weighing platform of high stable is independent, it is necessary to It is isolated with infusion pump, prevents infusion pump vibration from causing balance measurement error.The class of accuracy of precision electronic balance is not less than II Grade, scale division value are not more than 0.01mg.Suitable load is selected according to uninterrupted in actual use, tests quality as far as possible in balance 60% or so of load.
In the present invention, micrometeor and ultra micro flow rate-measuring device include 10- perspex frame, and perspex frame is used to Fixed liquid liquid-transport pipe-line and 11- precise injection needle, and make infusion pipeline vacantly on frame, while windproof and dustproof.
In the present invention, micrometeor and ultra micro flow rate-measuring device include 11- precise injection needle and 12- weighing bottle, precision note The outer cross section size for penetrating needle is consistent, and the inner section size of weighing bottle is also required to unanimously.Current existing technology is for precise injection Needle and weighing bottle dimensions and no requirement (NR).If will be unable to guarantee accurately to calculate liquid in flow measurement without the restriction Face rise volume, and then influence the accuracy of method.So to fully consider injection needle buoyancy for the shadow of balance weighing result It rings, fluid flow is corrected.During flow measurement, since liquid level rises in weighing bottle, the weighing value of balance is The summation of the quality of weight value and injection needle the buoyancy conversion of actual liquid, as shown in formula (1).Thus, the rising of liquid level Height and practical transfusion fluid integral are not calculated according to formula (2), formula (3).
M=mIt is real+mIt is floating=ρ * VIt is real+ρ*VIt is floating
=ρ * (A-B) * Δ H+ ρ * B* Δ H=ρ * A* Δ H (1)
In formula:
mIt is real--- practical injection quality, mg
mIt is floating--- quality value added, mg caused by injection needle buoyancy changes
VIt is floating--- precise injection needle immerses volume value added, mL
VIt is real--- practical infusion volume, mL
Δ H --- since infusion leads to liquid level lifting height in weighing bottle, cm
ρ --- the density of pure water, mg/mL under test temperature
M --- balance measured value, mg
The inner section product of A --- weighing bottle, cm2
B --- precise injection needle outer cross section product, cm2
K --- constants are worth for (A-B)/A
The inner section product A of weighing bottle and the outer cross section product B of precise injection needle are as shown in Figure 2.
In the present invention, 13- atoleine, density is about that 0.9g/mL (20 DEG C) for sealing prevents fluid to be measured (pure Water) volatilization.Dimethicone used in the YQ00202016 standard that the prior art uses, its density is about 1g/mL at 20 DEG C, It is close with pure water density, it will lead to certain mixing for sealing pure water, the effect of sealing cannot be played.And atoleine conduct The substance of common sealing pure water, is different from other sealing substances, and low volatility, density feature are more suitable for measurement dress It sets.Atoleine in the present invention is the density of common atoleine, guarantees that its density is significantly less than the density of pure water.
The present invention carries out concrete operations process:
1) it in addition to fixed bracket, is successively attached according to 1 schematic diagram of attached drawing;
2) using pure water as liquid medium, high-voltage electric switching valve 5 is switched to output pipe, starts tested infusion pump 2, opens Vacuum degassing machine 1, the bubble in multiple suction evacuation flow output equipment are moved, abundant rinse-system to pressure is stablized.To pressure After stabilization, high-voltage electric switching valve 5 is switched to waste-solution line;
3) a small amount of pure water is injected in weighing bottle in advance, and is sealed with atoleine 13, precision electronic balance 9 is put into In, it is fixed with perspex frame 10, precise injection needle 12 is inserted into 13 liquid level of atoleine hereinafter, initial mass is denoted as m0, And accurate recording environment temperature T (laboratory temperature);
4) high-accuracy timer 6 input suitable time t (change depending on specific flow rate test point, precision electronic balance Mass change is not less than the precision of 10 × electronic balance), it clicks high-accuracy timer and starts countdown, start to measure, Replication 11 times, precision electronic balance data are read, are recorded as m respectively1、m2、m3….m11
5) data processing is finally carried out, flow is calculated.
Flow of the invention is calculated by following calculating process:
Actual test bulking value are as follows: balance weighing value is converted to bulking value and subtracts injection needle volume value added;
It can be obtained after being derived according to formula (3), the average flow rate of liquid can be calculated according to formula (4), (5)
Fn=K* (mn-mn-1)/ρ/t (4)
F?=∑ Fn/n (5)
In formula (4), (5):
ρ --- the density of pure water, mg/ml under test temperature
K --- constants are worth for (A-B)/A
Fn --- n-th flow actual measured value, mL/min
mn--- n-th measurement terminates quality, mg
mn-1--- n-th measurement starts quality, mg
T --- time of measuring, min
N --- pendulous frequency
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with appended claims be protect Protect range.

Claims (10)

1. a kind of micrometeor and ultra micro flow rate-measuring device characterized by comprising
Vacuum degassing machine (1), tested infusion pump (2), pressure sensor (3) and damper tube (4);
High-voltage electric switching valve (5), the high-voltage electric switching valve (5) respectively with the damper tube (4), high-accuracy timer (6), waste liquid bottle (7) is connected to precise injection needle (12);
The precise injection needle (12) probes into weighing bottle (11);
The weighing bottle (11) is placed on precision electronic balance (9), inside hold fluid to be measured, the table of the fluid to be measured Face is sealed with atoleine (13), to prevent the fluid to be measured from volatilizing in air;
The precision electronic balance (9) is placed on high stable and weighs on platform (8).
2. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the vacuum degassing machine (1) It is connected to the input terminal of tested infusion pump (2).
3. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the pressure sensor (3) It is connected to the outlet end of tested infusion pump (2), connects damper tube (4) thereafter.
4. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the high-accuracy timer (6) energization and power-off for controlling high-voltage electric switching valve (5) switch and access measurement system, the high-voltage electric switching valve (5) Output end pass through piping connection respectively to the precise injection needle (12) and the waste liquid bottle (7).
5. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the high-voltage electric switching valve (5) two length of pipe of output end are consistent, to guarantee the consistency of pressure drop.
6. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the weighing bottle (11) it is interior Cross-sectional dimension is consistent.
7. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the precise injection needle (12) Outer cross section product size be consistent.
8. micrometeor as described in claim 1 and ultra micro flow rate-measuring device, which is characterized in that the high stable weighs platform (8) perspex frame (10) are equipped with.
9. micrometeor as claimed in claim 8 and ultra micro flow rate-measuring device, which is characterized in that the perspex frame (10) precise injection needle (12) and pipeline are fixed.
10. a kind of micrometeor and ultra micro flow rate-measuring device measuring method, which is characterized in that using appointing such as claim 1-9 Micrometeor described in one and ultra micro flow rate-measuring device, comprising the following steps:
The micro-bubble of liquid and pipeline is excluded by vacuum degassing machine and damper tube;
Pressure is detected by pressure sensor, guarantees the measurement for carrying out flow under a certain pressure;
It is after pressure stabilisation, Vavle switching is switched by high-accuracy Timer Controlling high-voltage electric, is acquired;
By calculating, influence of the buoyancy variation for measurement result is deducted.
CN201910270785.7A 2019-04-04 2019-04-04 A kind of micrometeor and ultra micro flow rate-measuring device and method Pending CN110057417A (en)

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CN201910270785.7A CN110057417A (en) 2019-04-04 2019-04-04 A kind of micrometeor and ultra micro flow rate-measuring device and method
CN201910821672.1A CN110455364B (en) 2019-04-04 2019-09-02 Micro-flow and ultra-micro-flow measuring device and method
CN201921440467.2U CN210719297U (en) 2019-04-04 2019-09-02 Micro-flow and ultramicro-flow measuring device

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CN113390626A (en) * 2021-06-08 2021-09-14 苏州原位芯片科技有限责任公司 Micro flow control pump valve device test system and test method
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CN115077643A (en) * 2022-07-26 2022-09-20 中国测试技术研究院流量研究所 Flow detection device and detection method for micro-flow liquid

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