CN105044272B - A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability - Google Patents
A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability Download PDFInfo
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- CN105044272B CN105044272B CN201510362522.0A CN201510362522A CN105044272B CN 105044272 B CN105044272 B CN 105044272B CN 201510362522 A CN201510362522 A CN 201510362522A CN 105044272 B CN105044272 B CN 105044272B
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- pressure gauge
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Abstract
A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability.The invention belongs to chromatography of ions field, come to provide the ion chromatograph of mobility and the field of relevant apparatus to mobile phase pressurization especially with pump, cushioning liquid holding vessel passes through pipeline and pump, injector, flow damper, guard column, pressure gauge, chromatogram column fixer, go out sample detector, waste liquid tank is sequentially connected, the chromatogram column fixer is used to place ion chromatographic column to be measured, it is set to be connected with front and rear pipeline, wherein pump, pressure gauge, going out sample detector has data wire to be connected with the terminal, injector adds the mixture of several standard determinands of suitable concentration, the present invention can efficiently learn the most huge pillar pressure that chromatographic column can bear, improve efficiency, and it ensure that chromatographic column will not be damaged simultaneously.
Description
Technical field
The invention belongs to chromatography of ions field, and to pressurize to mobile phase especially with pump provides the chromatography of ions of mobility
The field of instrument and relevant apparatus.
Background technology
High pressure pump is one of most important part of ion chromatograph, and it is acted on sample and mobile phase mainly with steady
Fixed flow velocity imports chromatographic column, suppressor and subsequent ion chromatographic system.Because the tolerance of ion chromatographic column is weaker, work as pump
Pressure improves to a certain extent, irreversibility will be caused to destroy ion chromatographic column, so the voltage endurance capability of high-pressure pump is ion
One important indicator of chromatogram.At present, the pressure-resistant evaluation method of existing pump has two：First, the pressure with instrument autogamy
Sensor determines pump pressure, does not possess traceability and fairness；Second, pressure rise is made by the method for blocking pump discharge, with
The increase of pumping liquid, pump pressure can continue to raise, and can not the constant time (5min) for keeping requiring；It is if stifled by adjusting
Head tightness makes pressure constant, is very difficult to regulation again and arrives target pressure value.And this method and flow in actual use
Increase makes pump pressure rise inconsistent, it is impossible to really investigates the pressure-resistant situation of pump in actual use.It is resistance to that the present invention devises a kind of pump
The test device of pressure, ion chromatograph pump pressure elevation process is simulated, and by this device, it is pressure-resistant to invent a kind of pump
Pressure detection method, so as to it is true, scientifically ion chromatograph is investigated with the pressure-resistant situation of pump, filled up domestic blank.
The content of the invention
Rarely has the device for being specifically used to quick measurement chromatographic column voltage endurance capability in the prior art, in order to fill in actually measuring
Divide the service life for taking chromatographic column into account, if the most huge pillar pressure that chromatographic column can bear can efficiently be learnt, can be designed that
Faster separation method, efficiency is improved, and ensure that chromatographic column will not be damaged simultaneously, the present invention is exactly to solve the skill
Art problem and this device is provided.
The device that the present invention is used for quick measurement chromatography of ions voltage endurance capability is included with lower part：Cushioning liquid holding vessel,
Pump, pressure gauge, flow damper, injector, chromatogram column fixer, pipeline, guard column, waste liquid pool, go out sample detector, injector,
Controller, terminal, the data circuit with data processing and display function, wherein cushioning liquid holding vessel by pipeline and pump,
Injector, flow damper, guard column, pressure gauge, chromatogram column fixer, go out sample detector, waste liquid tank is sequentially connected, the chromatogram
Column fixer be used for place ion chromatographic column to be measured, it connect with front and rear pipeline, wherein pump, pressure gauge, go out sample detect
Device has data wire to be connected with the terminal.
Flow damper in said apparatus causes the mobile phase under high pressure by producing soft resistance, can make its fast transition
For gentle but still holding certain flow rate mobile phase, " pulse " symptom that pump is brought is greatly reduced.It is well known that chromatography of ions
Pump can bring the uneven flow velocity of " pulsed " due to its working method to the mobile phase of chromatographic column, can typically use certain means
By its tranquilization, this process is similar to the wave filter in alternating current, and the application then realizes this purpose using flow damper, and
The flow damper that the application uses also has preferably unhurried current ability, can be with the arteries and veins for just improving more pause and transition in rhythm or melody by distance of very little
Formula mobile phase is rushed, so as to provide the apparatus and method of the measure voltage endurance capability of efficient quick.
Above-mentioned flow damper is made up of the outer wall being tightly bonded and notched internals, the groove and inside outer wall surface
Composition is available for the lumen that mobile phase (liquid phase) flows, and mobile phase flows therethrough.The shape at the center of each differential cross-section of groove
Shape with minor function by being determined:The function is cylindrical coordinates minor function, and a is to turn over unit angle
When groove on the distance that projects to coordinate system center of the point on coordinate system center and plane with vertical axis z-axis is crossed, r represents to turn
Cross point that unit angle projects on coordinate system center and plane with vertical axis z-axis is crossed to the movement at coordinate system center away from
From b represents to turn over the distance that unit angle moves in z-axis.It can be needed to carry out selection span, each f according to actual conditions
Position of the point in cylindrical-coordinate system in (r, φ, z) respective slot.A, b unit are mm/ °, represent often to rotate 1 degree
When polar diameter increase (or reduce) amount), their numerical value can be adjusting grooves and center in cylindrical coordinate with identical or different
Distance, the parameter of distance between groove.
The shape of above-mentioned groove does not account for the cross-sectional area of groove, and above-mentioned function value is the central point of cross section
Description, the cross section of the groove can need to determine as the case may be, circle that typically can be using value as 0.1-1mm internal diameters
Tee section.
During using the device, injector adds the mixture of several standard determinands of suitable concentration, and pump is then adjusted first
Compression pump to general remark book suggestion enters mobile phase, and the peak of the peak shape of standard can be now seen from detector.Then by electricity
Brain terminal control pump pressurizes, and observes the shape at peak, because pressure, flow velocity increase, becomes by the time of chromatographic column fixed phase
Change, if the excessive flow velocity of pressure is too fast, resolution ratio is deteriorated between causing peak, now understands that the pressure is too high, according to
The required resolution ratio of separation can learn pressure-resistant situation.
Beneficial effects of the present invention：Flow damper used in the present invention is not isometrical helical groove, and mobile phase enters flow damper
When, " annulus " (being not the section of groove) that groove is formed has larger diameter, and as mobile phase flows into, the diameter constantly becomes
It is small, to export when the groove enclosed annulus decline be cross section, it is such the advantages of be with larger pressure, flow velocity enter flowing
Mutually reduce flow velocity soon " around great circle " first, subsequent institute's pitch of the laps was originally smaller, causes flow velocity to become more steady, reduces
Chromatographic column is washed away, serves good " rectification " effect.
Brief description of the drawings：
Fig. 1 is each part connection figure, and solid line is liquid line, and dotted line is data wire, and 1 is buffer storage NaOH solution tank NaOH, and 2 are
Pump, 3 be sampling device, and 4 be flow damper, and 5 be guard column, and 6 be pressure gauge, and 7 be chromatogram column fixer, and 8 be sample detector,
9 be waste liquid tank, and 10 be the terminal with data processing and display function.
Fig. 2 is the schematic shapes of flow damper further groove, and design upper end is liquid feeding end, and lower end is outlet end.
Embodiment
Cushioning liquid holding vessel 1 is solid by pipeline and pump 2, injector 3, flow damper 4, guard column 5, pressure gauge 6, chromatographic column
Determine device 7, go out sample detector 8, waste liquid tank 9 is sequentially connected, the chromatogram column fixer 7 be used for place chromatography of ions to be measured
Post, it is connected with front and rear pipeline, wherein pump 2, pressure gauge 6, go out sample detector 8 and there is data wire to be connected with the terminal 10.
Above-mentioned flow damper 4 is made up of the outer wall being tightly bonded and notched internals, the groove and inside outer wall table
Face forms the lumen for being available for mobile phase (liquid phase) to flow, and mobile phase flows therethrough.The center of each differential cross-section of groove
Shape with minor function by being determinedThe function is cylindrical coordinates minor function, and a is to turn over unit angle
The distance that projects to coordinate system center of the point on coordinate system center excessively and the plane with vertical axis z-axis, r are represented on groove when spending
Turn over point that unit angle projects on coordinate system center and plane with vertical axis z-axis is crossed to the movement at coordinate system center away from
From b represents to turn over the distance that unit angle moves in z-axis.It can be needed to carry out selection span according to actual conditions, eachPosition of the point in cylindrical-coordinate system in respective slot.A, b unit are mm/ °, when representing often to rotate 1 degree
Increase (or reduce) amount of polar diameter), their numerical value can with identical or different, be adjusting grooves with cylindrical coordinate center away from
From the parameter of distance between groove.
Each part and chromatographic column are connected according to connected mode of the present invention, now flow damper groove uses size
For the size of flow damper 4 used is length=5cm, and liquid feeding end groove maximum annulus is 1cm radiuses；Now cross section is 0.2mm
The circle of internal diameter.Material therefor outer wall is stainless steel or polytetrafluoroethylene (PTFE), and it is polytetrafluoroethylene (PTFE) to have reeded internal materials, should
Flow damper can customize to obtain to the manufacturer of production plastics.Now a=1.38x10^-4mm/ degree, b=6.94x10^-4mm/ degree,Degree.
Gradually rise is pumped after connecting, and boosting all adds biased sample and simultaneously observes chromatogram every time, until discovery is differentiated
Rate is undesirable, and it is 26.3MPa that now determination experiment chromatographic column is pressure-resistant.
In summary, the present invention preferably resolves the technical problem of quick measurement chromatographic column voltage endurance capability, and provides
A kind of flow damper well brings good " rectification " effect to " pulse " formula pump pressure.
Claims (2)
1. a kind of device of quick measurement ion chromatographic column voltage endurance capability, it is characterised in that described device contains such as lower component：It is slow
Rush solution storage tanks, pump, pressure gauge, flow damper, injector, chromatogram column fixer, pipeline, guard column, waste liquid tank, go out sample inspection
Survey device, controller, terminal, the data wire with data processing and display function, wherein cushioning liquid holding vessel by pipeline with
Pump, injector, flow damper, guard column, pressure gauge, chromatogram column fixer, go out sample detector, waste liquid tank is sequentially connected, described
Chromatogram column fixer be used for place ion chromatographic column to be measured, it is connected with front and rear pipeline, wherein pump, pressure gauge, go out sample
Detector has data wire to be connected with the terminal；
The flow damper is made up of the outer wall being tightly bonded and notched internals, and the groove is formed with inside outer wall surface
The lumen for being available for mobile phase to flow, the shape at the center of each differential cross-section of groove with minor function by being determined：F (r, φ, z)=f
(r=φ * a, φ, z=φ * b), the function are cylindrical coordinates minor function, and a is crossing coordinate for point on groove when turning over unit angle
It is center and represents to turn over unit angle in coordinate system with the distance for projecting to coordinate system center in the plane of z-axis, b
The distance moved along in z-axis, the cross section of the groove are the circular cross-section of value 0.1-1mm internal diameters；
The flow damper is generally taper or internals and set for taper, and the maximum radius upper limit is 5cm, length 2-50cm.
2. claim 1 described device is used for the method for measuring ion chromatographic column voltage endurance capability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510362522.0A CN105044272B (en) | 2015-06-26 | 2015-06-26 | A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510362522.0A CN105044272B (en) | 2015-06-26 | 2015-06-26 | A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability |
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| Publication Number | Publication Date |
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| CN105044272A CN105044272A (en) | 2015-11-11 |
| CN105044272B true CN105044272B (en) | 2017-12-26 |
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| CN201510362522.0A Expired - Fee Related CN105044272B (en) | 2015-06-26 | 2015-06-26 | A kind of apparatus and method of quick measurement chromatography of ions voltage endurance capability |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511256A (en) * | 2001-06-07 | 2004-07-07 | 纳诺斯特利姆有限公司 | Microfluidic separation devices with on-column sample injection |
| CN203474680U (en) * | 2013-09-01 | 2014-03-12 | 嘉施利（眉山）化肥有限公司 | Coating oil tank for production of nitrate-chloride-based slow release compound fertilizer |
| CN204855471U (en) * | 2015-06-26 | 2015-12-09 | 山东省计量科学研究院 | Rapid survey ion chromatogram seal pressure's device |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2250521Y (en) * | 1995-12-11 | 1997-03-26 | 顾好粮 | Pneumatic constant current liquid phase chromatography infusion device |
| CN2484564Y (en) * | 2001-06-06 | 2002-04-03 | 浙江大学 | Chromatographic apparatus of analog moving bed with open loop structure |
| CN2685606Y (en) * | 2004-03-18 | 2005-03-16 | 东台市燕山仪表总厂 | Acumulator damper for high-speed liquid phase chromatographic pump |
| CN202083678U (en) * | 2011-04-29 | 2011-12-21 | 上海伍丰科学仪器有限公司 | High-pressure constant-current pump ripple damper with full-peak contact surface |
| JP5677649B1 (en) * | 2013-04-22 | 2015-02-25 | 積水メディカル株式会社 | Switching valve for flow analyzer |
-
2015
- 2015-06-26 CN CN201510362522.0A patent/CN105044272B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511256A (en) * | 2001-06-07 | 2004-07-07 | 纳诺斯特利姆有限公司 | Microfluidic separation devices with on-column sample injection |
| CN203474680U (en) * | 2013-09-01 | 2014-03-12 | 嘉施利（眉山）化肥有限公司 | Coating oil tank for production of nitrate-chloride-based slow release compound fertilizer |
| CN204855471U (en) * | 2015-06-26 | 2015-12-09 | 山东省计量科学研究院 | Rapid survey ion chromatogram seal pressure's device |
Non-Patent Citations (1)
| Title |
|---|
| 高效、快速液相色谱系统的构建及评价;李笃信;《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》;20080115(第01期);第35页"3.2.1. 实验设备"，第36页"3.2.3. 系统流程图"，第37页"3.3.1.耐压测试" * |
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| CN105044272A (en) | 2015-11-11 |
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Granted publication date: 20171226 Termination date: 20180626 |