CN105044228B - Device and method for measuring column capacity of chromatographic column - Google Patents
Device and method for measuring column capacity of chromatographic column Download PDFInfo
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- CN105044228B CN105044228B CN201510362401.6A CN201510362401A CN105044228B CN 105044228 B CN105044228 B CN 105044228B CN 201510362401 A CN201510362401 A CN 201510362401A CN 105044228 B CN105044228 B CN 105044228B
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Abstract
The invention relates to a device and method for quickly measuring column capacity of a chromatographic column, wherein a special flow slowing device and matched components are used to achieve the purpose of quick and convenient measurement; the device is sequentially connected with a buffer solution storage tank, a pump, the flow slowing device, a sample introduction injector, a guard column, a to-be-measured chromatographic column, a detector and a liquid waste gathering tank through a liquid flow-through pipeline; the pump, the sample introduction injector and the detector are connected with a terminal through data lines, the sample introduction injector enters a mobile phase, the mobile phase enters the flow slowing device through the thrust of the pump to remove the pulse brought by the pump, enters the chromatographic column and is detected by the detector after coming out, and then a chromatogram map is drawn through calculation; if sample amount is not excessive during entering, the peak shape should be relatively symmetric, and sampling concentration can be increased at this time; if the peak shape is obviously tailed, the column capacity is achieved or exceeded, the chromatographic column can be washed at this time, and the sampling concentration can be gradually decreased to be closed to the column capacity.
Description
Technical field
The invention belongs to chromatography of ions field, especially needs to judge the highest sample size that specific chromatographic column can bear
Technical field.
Background technology
Column capacity, is also column load, refers to the maximum sample size allowed in the case where post separation efficiency is not affected.It is any
The amount of the sample that chromatographic column can bear is limited, when the amount of sample has exceeded certain limit, chromatograph column overload, chromatographic peak
Broaden, or even gross distortion, the column efficiency of chromatographic column declines rapidly with the increase of sample size.Therefore, column capacity is to represent color
One important parameter of spectrum post characteristic.At present, ion chromatographic column column capacity method of testing has two kinds, and one kind is to refer to ion exchange
The method of testing of resin exchange capacity, the method have ignored the ion remained in resin space, and be by titration method
Carry out quantitatively, operating process is more complicated.Method of another kind of change for passing through peak shape to determine column capacity, i.e., progressively increase into
Sample amount, column capacity is determined by the change of spectrogram, and the method is affected larger by environmental condition, instrument state, and due to
Pressure tolerance power is estimated and is difficult to accomplish accurately judgement, and provide the pump of flow velocity because it has pulse feature, this pulse pressure
The suddenly change of power easily causes too high and pressure oscillation the problem of pressurization to fixing phase, even results in the damage of fixing phase.
So, need a kind of accurate, method of science badly and ion chromatographic column column capacity is measured.
The content of the invention
The present invention fast determines for convenience a certain chromatographic column and treats analyte sample highest sample size ability to bear, there is provided
A kind of device voluntarily researched and developed and supporting method.
The device of the present invention contains with lower component：Buffer solution holding vessel, pump, flow damper, sampling injector, guard column,
Chromatographic column to be measured, detector, waste collection tank, fluid communication lines, data wire, with data processing and control and display work(
The terminal of energy；Described device is sequentially connected with lower component by fluid communication lines：It is buffer solution holding vessel, pump, slow
Stream device, sampling injector, guard column, chromatographic column to be measured, detector, waste collection tank；Pump, sampling injector, detector pass through
Data wire is connected with the terminal.
Sample determinand is held in the sampling injector, by terminal controlled motor sample introduction.The sample introduction injection
The preferred technical scheme of device one is that using multiple syringe samplings, sample concentration height is different in each syringe, by calculating
And the syringe of terminal control variable concentrations sample introduction successively.
Flow damper in said apparatus causes the mobile phase under high pressure through producing soft resistance, can make its fast transition
For mobile phase that is gentle but still keeping certain flow rate, " pulse " symptom that pump brings 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 adopt certain means
By its tranquilization, similar to the wave filter in alternating current, the application then realizes this purpose to this process using flow damper, and
Compared to existing technology middle same device also has preferably unhurried current ability to the flow damper that the application is adopted, can be with the process of very little
Distance just improves the pulsatile flow phase of more pause and transition in rhythm or melody, so as to provide device and the side of the measure voltage endurance capability of efficient quick
Method.
Above-mentioned flow damper is made up of the outer wall tightly fitted and notched internals, the groove and inside outer wall surface
Composition is available for the chamber that mobile phase (liquid phase) flows, mobile phase to flow therethrough.The shape at the center of each differential cross-section of the groove
By being determined with minor function:The function is cylindrical coordinatess minor function, and a is for when turning over unit angle
The point that projects on coordinate system center and plane with vertical axises z-axis is crossed is put on groove to the distance at coordinate system center, r is represented turn
Cross point that unit angle projects on coordinate system center and plane with vertical axises z-axis is crossed to the movement at coordinate system center away from
From b is represented and turned over the distance that unit angle is moved in z-axis.Can be needed to carry out selection span according to practical situation, eachPosition of the point in respective slot in cylindrical-coordinate system.The unit of a, b is mm/ °, when expression often rotates 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.
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-sectional area
Description, the cross-sectional area of the groove can need to determine as the case may be, typically can be with value as 0.1-1mm internal diameters
Circular cross-section.
When in use, sample Jing syringes enter into mobile phase to the present invention, and mobile phase enters flow damper by thrust of pump, by pump
The pulse that brings is removed, into chromatographic column and out after Jing detectors detect, then by calculating and plotting chromatogram, if entering fashionable sample
Without excessively, then peak shape should be more symmetrical, can now increase sample introduction concentration for product amount.In an optimal technical scheme, make
With the sample of another higher concentration by syringe sampling, rising sample introduction is continued if still compound-split is required if peak shape dense
Degree, if hangover substantially occurs in peak shape, means column capacity to reach or exceed, and now can first clean chromatographic column, then by
Step reduces sample introduction concentration, approaches column capacity.
The application is due to having used special flow damper, pulse pump pressure quilt " filtering ", under the premise of maintaining overall pressure
The fluctuation of pressure is reduced, such that it is able to reduce " impact " to fixing phase, technological deficiency of the prior art is overcome so that
Pulse voltage supply to pump serves mitigation.
Description of the drawings
Fig. 1 is apparatus of the present invention connection figure, and in figure, 1 is buffer solution holding vessel, and 2 is pump, 3 flow dampers, and 4 is sample introduction note
Emitter, 5 is guard column, and 6 is chromatographic column, and 7 is detector, and 8 is waste collection tank, and 9 is terminal；Solid line represents liquid flow
Stylet, dotted line is data wire；
Fig. 2 is the schematic diagram of flow damper shape；In figure, upper end is liquid feeding end, and lower end is liquid outlet.
Specific embodiment
The present invention is further described with reference to specific embodiment, such as accompanying drawing 1, shown in 2.
A kind of device of measurement chromatographic column column capacity, containing with lower component：Buffer solution holding vessel 1, pump 2, flow damper 3,
Sampling injector 4, guard column 5, chromatographic column to be measured 6, detector 7, waste collection tank 8, fluid communication lines, data wire has
Data processing and the terminal 9 of control and display function；Institute's fluid communication lines are sequentially connected with lower component：Buffering is molten
Liquid holding vessel 1, pump 2, flow damper 3, sampling injector 4, guard column 5, chromatographic column to be measured 7, detector 7, waste collection tank 8；And
And, pump 2, sampling injector 6, detector 7 are connected by data wire with the terminal 9.
The flow damper 3 is made up of the outer wall tightly fitted and notched internals, the groove and inside outer wall table
Face constitutes the chamber for being available for mobile phase (liquid phase) to flow, and mobile phase is flowed therethrough.The shape at the center of each differential cross-section of the groove
Shape with minor function by being determined:The function is cylindrical coordinatess minor function, and a is to turn over unit angle
When groove on put the point that projects on coordinate system center and plane with vertical axises z-axis is crossed to the distance at coordinate system center, r is represented
Turn over point that unit angle projects on coordinate system center and plane with vertical axises z-axis is crossed to the movement at coordinate system center away from
From b is represented and turned over the distance that unit angle is moved in z-axis.Can be needed to carry out selection span according to practical situation, eachPosition of the point in respective slot in cylindrical-coordinate system.The unit of a, b is mm/ °, when expression often rotates 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.The shape of above-mentioned groove does not account for the cross-sectional area of groove, and above-mentioned function value is horizontal stroke
The description of the central point of sectional area, the cross-sectional area of the groove can need to determine as the case may be, typically can take
It is worth for the circular cross-section of 0.1-1mm internal diameters.
Sample determinand is held in the sampling injector 4, by the controlled motor sample introduction of terminal 9.The sample introduction note
Emitter 4 for multiple, by calculate and terminal control variable concentrations syringe sample introduction successively.Buffer solution is prepared, mark is prepared successively
Quasi- solution：1mg/L, 5mg/L, 15mg/L, 25mg/L, 50ml/L, 100mg/L, 200mg/L, 400mg/L, 800mg/L,
The chloride ion standard sample of 1000mg/L, 1200mg/L, 1500mg/L, 2000mg/L, sample concentration height in each syringe 4
Difference, sample Jing syringes enter into mobile phase, and mobile phase enters flow damper by thrust of pump, and the pulse that pump is brought is removed, and is entered
Enter chromatographic column and out after Jing conductivity detectors detection, then by calculating and plotting chromatogram.Through entering that concentration rises successively
Sample loading mode, when finding 1500mg/L concentration sample introductions, peak occurs in that slight conditions of streaking, and 2000mg/L is even more serious, and 1200mg/
Do not occur substantially hangover during L sample introductions, now determine that the chromatographic column should not be added higher than 1300-1400mg/L concentration determinands.
Claims (2)
1. it is a kind of measurement ion chromatographic column column capacity device, it is characterised in that containing with lower component：Buffer solution holding vessel,
Pump, flow damper, sampling injector, guard column, ion chromatographic column to be measured, detector, waste collection tank, fluid communication lines, number
According to line, the terminal with data processing and control and display function；Described device passes through fluid communication lines successively
Connection is with lower component：Buffer solution holding vessel, pump, flow damper, sampling injector, guard column, ion chromatographic column to be measured, detection
Device, waste collection tank；Also, pump, sampling injector, detector are connected by data wire with the terminal；
Sample determinand is held in the sampling injector, by terminal controlled motor sample introduction；
The sampling injector is multiple, and sample concentration is different in each syringe, and by terminal variable concentrations are controlled
Syringe sample introduction successively；
The flow damper is made up of the outer wall tightly fitted and notched internals, and the groove is constituted with inside outer wall surface
The chamber for being available for mobile phase to flow, mobile phase flows therethrough, and the shape at the center of the channel section with minor function by being determined:
The function be cylindrical coordinatess minor function, a for turn over unit angle when groove on put cross coordinate system center and with vertical axises z
The distance for projecting to coordinate system center in the plane of axle, r represent turn over unit angle cross coordinate system center and with vertical axises z
In the plane of axle project point to the movement at coordinate system center distance, b represent when turning over unit angle z-axis move away from
From eachPosition of the point in respective slot in cylindrical-coordinate system.
2. claim 1 described device is used to measure ion chromatographic column column capacity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510362401.6A CN105044228B (en) | 2015-06-26 | 2015-06-26 | Device and method for measuring column capacity of chromatographic column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510362401.6A CN105044228B (en) | 2015-06-26 | 2015-06-26 | Device and method for measuring column capacity of chromatographic column |
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| Publication Number | Publication Date |
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| CN105044228A CN105044228A (en) | 2015-11-11 |
| CN105044228B true CN105044228B (en) | 2017-04-12 |
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| CN201510362401.6A Expired - Fee Related CN105044228B (en) | 2015-06-26 | 2015-06-26 | Device and method for measuring column capacity of chromatographic column |
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Citations (4)
| 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 |
| CN102539590A (en) * | 2011-12-31 | 2012-07-04 | 聚光科技(杭州)股份有限公司 | Chromatographic analysis system and chromatographic analysis method |
| WO2014175251A1 (en) * | 2013-04-22 | 2014-10-30 | 積水メディカル株式会社 | Switching valve for flow-type analysis device |
| CN204855463U (en) * | 2015-06-26 | 2015-12-09 | 山东省计量科学研究院 | Measure device of chromatographic column column capacity |
-
2015
- 2015-06-26 CN CN201510362401.6A patent/CN105044228B/en not_active Expired - Fee Related
Patent Citations (4)
| 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 |
| CN102539590A (en) * | 2011-12-31 | 2012-07-04 | 聚光科技(杭州)股份有限公司 | Chromatographic analysis system and chromatographic analysis method |
| WO2014175251A1 (en) * | 2013-04-22 | 2014-10-30 | 積水メディカル株式会社 | Switching valve for flow-type analysis device |
| CN204855463U (en) * | 2015-06-26 | 2015-12-09 | 山东省计量科学研究院 | Measure device of chromatographic column column capacity |
Non-Patent Citations (1)
| Title |
|---|
| 超效液相色谱系统构建及其色谱性能;沈从华;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140715(第07期);第2.1、2.2.2、2.3.2小节，图2.1 * |
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| CN105044228A (en) | 2015-11-11 |
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