CN104508478B - Liquid chromatograph and liquid feeding device - Google Patents
Liquid chromatograph and liquid feeding device Download PDFInfo
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- CN104508478B CN104508478B CN201380041151.5A CN201380041151A CN104508478B CN 104508478 B CN104508478 B CN 104508478B CN 201380041151 A CN201380041151 A CN 201380041151A CN 104508478 B CN104508478 B CN 104508478B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/24—Automatic injection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/326—Control of physical parameters of the fluid carrier of pressure or speed pumps
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- Control Of Positive-Displacement Pumps (AREA)
- Reciprocating Pumps (AREA)
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Abstract
The present invention provides a kind of liquid feeding device and liquid chromatograph, and it has, and the kind with eluent, temperature, mixing ratio, liquor charging pressure is the most accurate and high-precision low pressure gradient mode.Possessing: pumping section, it possesses: have the suction inlet of eluent and the cylinder of ejiction opening and the piston of back and forth movement in above-mentioned cylinder, has suction inlet and the cylinder of ejiction opening and the piston of back and forth movement in above-mentioned cylinder, carries out the absorption of above-mentioned eluent, ejection；Valve cell, it switches the kind of multiple eluents that above-mentioned pumping section is drawn by on-off action；Pressure transducer, the pressure of the eluent that its detection sprays from the ejiction opening of above-mentioned pumping section；Control portion, it controls the on-off action of above-mentioned valve cell, wherein, above-mentioned control portion obtains and starts the actual actual absorption interval being drawn of above-mentioned eluent after the ejection pressure of sucking action starts the interval and above-mentioned decompression interval of decompression being drawn to above-mentioned eluent from the above-mentioned piston when drawing the plurality of eluent, is controlled such that the on-off action carrying out above-mentioned valve cell in the actual absorption interval that this is obtained.
Description
Technical field
The present invention relates to a kind of liquid chromatograph and liquid feeding device.
Background technology
Liquid chromatograph is following device, i.e. adds to by the solvent (eluent) of liquid feeding device liquor charging
Analyzing object samples, the composition being carried out sample by detached dowel is separated, and is existed by detector detections such as spectroscopes
Each composition of different time conveying, determines the composition of sample.
An example as the liquid feeding device of liquid chromatograph, it is known that by the work of back and forth movement in cylinder
Fill in the mode of the liquor charging of row eluent.
In using the liquor charging of liquid chromatograph of device as described above, there is following such gradient liquor charging
System, i.e. uses multiple eluent to change the composition liquor charging of eluent, it is possible to improve and analyzes
Object samples separating degree in detached dowel, seeks to shorten analysis time.
In the present system, there is the air at the upstream side from the cylinder carrying out liquor charging be pressed onto under lower pressure and change
Become the liquor charging mode of the low pressure gradient mode that is referred to as of the composition of multiple eluent.In low pressure gradient mode,
When liquid feeding device starts to draw, it is arranged on the mechanism of the composition changing eluent of liquid feeding device upstream side
(typically adjusting the opening/closing time of the open and close valve being connected with each eluent) washes drawing to change during the time
The composition of de-liquid, makes liquid feeding device draw multiple eluents, thus realizes.
So, in low pressure gradient mode liquid feeding device upstream side change eluent composition, therefore have
Time along with liquor charging pressure uprise and the mixed performance of eluent reduce.
Its reason is when the piston finished in the cylinder of ejection of eluent starts sucking action, to circle
The pressure in Tong period to atmospheric pressure, eluent is not drawn in cylinder, thus changes mixed
The time of the composition of composition and division in a proportion and actual absorption time produce difference.The precision pair of the mixing ratio of such eluent
Final analysis result also produces impact.
In patent documentation 1, it is proposed that based on prediction calculate from liquor charging pressure to atmospheric pressure till time
Between and revise the method for time of the composition changing mixing ratio.
Prior art literature
Patent documentation
Patent documentation 1: No. 3172429 publication of patent
Summary of the invention
The problem that invention is to be solved
The kind wanting the eluent of liquor charging has varied, and for physics values such as volume modulus, each is washed
De-liquid has different values.It addition, affected by such various conditions such as temperature of eluent, these
Factor changes sometimes.
But, in the method disclosed in patent documentation 1, only carry out mixing ratio according to the information of liquor charging pressure
Correction, therefore entirely without in view of the kind of handled eluent and character thereof.Therefore, we
In method, in kind, mixing ratio and other situations due to eluent, the characteristics such as its volume modulus are sent out
Cannot tackle in the case of having given birth to change.
It is an object of the invention to: provide a kind of have with eluent kind, temperature, the composition of mixing ratio,
Liquor charging pressure is the most accurate and the device of high-precision low pressure gradient mode and employ this device
Method.
Means for solving the above
As a form for achieving the object above, it is provided that a kind of device, it possesses: pumping section, its tool
Get everything ready the suction inlet of eluent and the cylinder of ejiction opening, the piston of back and forth movement in above-mentioned cylinder, carry out
The absorption of above-mentioned eluent, ejection；Valve cell, it switches above-mentioned pumping section by on-off action and is drawn many
The kind of individual eluent；Pressure transducer, the pressure of the eluent that its detection sprays from the ejiction opening of above-mentioned pumping section
Power；Control portion, it controls the on-off action of above-mentioned valve cell, it is characterised in that above-mentioned control portion obtains
The absorption stated after piston starts the sucking action of the plurality of eluent to above-mentioned eluent start decompression
Behind decompression interval interval, above-mentioned, the actual actual absorption interval being drawn of above-mentioned eluent, is controlled such that
The on-off action of above-mentioned valve cell is carried out in the actual absorption interval that this is obtained.
Invention effect
According to said one form, it is possible to realize with the kind of eluent, its temperature, mixing ratio composition with
And liquor charging pressure etc. is the most accurate and the liquor charging of high-precision low pressure gradient mode.
Accompanying drawing explanation
Fig. 1 is the figure of the summary of the structure representing liquid chromatograph.
Fig. 2 is the figure of an example of the structure representing the liquid feeding device being arranged in liquid chromatograph.
Fig. 3 is the chart of the example drawing interval pressure change representing liquid feeding device.
Fig. 4 is the structure of the control unit (data processing equipment) 22 representing embodiments of the present invention
The figure of a part.
Fig. 5 is the flow chart of the step of the liquor charging representing embodiments of the present invention.
Fig. 6 is the operating procedure representing embodiments of the present invention and the data processing equipment 110 accompanied therewith
The flow chart of process.
Fig. 7 is synoptic diagram and the cylinder of the pressure change of the first cylinder representing embodiments of the present invention
Liquor charging state and check-valves, the figure of state of open and close valve.
Fig. 8 is the figure of the configuration example representing the liquid feeding device different from the embodiment shown in Fig. 2.
Fig. 9 is the figure of the configuration example representing the liquid feeding device different from the embodiment shown in Fig. 2, Fig. 8.
Detailed description of the invention
Embodiment 1
Fig. 1 represents the summary of the structure of the liquid chromatograph being carried out liquor charging by low pressure gradient mode.
In this device, select to be contained in multiple container by the switching device 2 with multiple open and close valve
Multiple eluent in 1a～1d, is attracted by liquid feeding device 3, is sprayed.Spray to switching device 2 liquor charging
Eluent.
Switching device 2 is by optionally switching the eluent of container 1a～1d, it is possible to change from liquid feeding device
The mixing ratio of the eluent of 3 liquor chargings, changes the ratio of components of eluent.
The stream of the sample injection unit 4 eluent after being switched device 2 switching injects as analyzing object
Liquid sample.
Separate the liquid sample injected according to each composition in detached dowel 5.Due to molecular weight, hydrophobicity,
The difference of electric charge etc., each composition is different from the time that detached dowel 5 is sent.
Constant in order to temperature is remained, the most sometimes detached dowel 5 is arranged on column oven (column
Oven) in.
Each composition that detector 6 detection produces time difference and sends from detached dowel 5.
Fig. 2 represents an example of the structure of the liquid feeding device 3 shown in Fig. 1.
In this configuration, be made up of piston and cylinder 2 pump units are connected in series, use series connection
The liquor charging of mode.
In each pump unit, by cam, the rotary motion of motor is transformed to the back and forth movement of piston.
The spinning movement of motor 21 being transmitted to camshaft 17 by belt 18, first piston 13 passes through
First cam 15 carries out coming and going action, and the second piston 14 carries out coming and going action by the second cam 16.
The rotating speed of camshaft 17 is identified by control unit 22.
A various method is had for this knowledge method for distinguishing, but the such as circle of slit in camshaft 17 installation settings
Plate 19, with the sensor 20 method detection slit by optics, electrostatic capacitance, the magnetic line of force etc., it is possible to inspection
Survey the rotating speed of camshaft 17.
Pipe arrangement in the downstream of the second cylinder 11 arranges the pressure transducer 12 of the pressure measured in pipe arrangement, will
It is sent to control unit 22 by the value of the pressure in the pipe arrangement of this pressure transducer 12 metering.
The value of the pressure in control unit 22 and this pipe arrangement controls the rotating speed of motor 21 accordingly, by upper
It is sent to control unit 22 after stating the rotating speed of sensor 20 dosing cam axle 17, adjusts turning of motor 21
Speed.
In the low pressure gradient mode making the mixing ratio of multiple eluent gradually change over time, at the first circle
In the interval that entrance side check-valves 8 in the sucking action interval of cylinder 9 is open, it is arranged on switching device 2
In multiple open and close valve 7a～7d carry out on-off action.
Control unit 22 by adjust open and close valve 7a～7d corresponding with corresponding eluent opening/closing time and
Timing changes mixing ratio so that realize the proportion of composing of various eluent.
Fig. 4 is the one of the structure chart of the control unit (data processing equipment) 22 of embodiments of the present invention
Part.Additionally, in addition in structure illustrated herein, data processing equipment 22 possesses as holding
The calculation processing apparatus (such as CPU) of the computing unit of the various programs of row, conduct are for storing with this journey
Sequence is the storage device of the memory element of the various data of representative, for the data carried out to each device with refer to
The input and output calculation processing apparatus that the input and output shown etc. control.
In the diagram, data processing equipment 22 possesses input unit 24, calculating part 25, storage part 26, send
Hydraulic control portion 27, output unit 28.
Input unit 24 be from outside input relevant with the control of liquid feeding device 3 impose a condition (such as flow,
Mixing ratio, time etc.) and umber of pulse S interval in order to obtain decompression in calculating part 25offset, real
Interval umber of pulse S is drawn on borderRRequired various information (the such as volume of piston displacement l, cylinder
VALL, the diameter d of piston, draw interval umber of pulse SS, liquor charging pressure) part.
Here, draw interval to refer to that first piston 13 carries out the interval overall of sucking action, decompression interval is
Entrance side is only to the liquor charging pressure in cylinder to atmospheric pressure to refer to start sucking action from first piston 13
Going back to the interval till valve 8 opens, actual interval of drawing refers to the actual interval being drawn of eluent.
As above-mentioned input method, such as in addition to the input carried out by input equipment 24, also warp
The input that carried out by the storage medium storing these information, communicate via network and other computers
Input method etc..
Calculating part 25, according to the information inputted from input unit 24, is counted respectively according to computing formula described later
Calculate.Specifically, by umber of pulse S in decompression intervaloffsetObtaining section obtains the umber of pulse that decompression is interval
Soffset, draw interval umber of pulse S by realityRObtaining section obtains umber of pulse S that actual absorption is intervalR。
Storage part 26 is to store the information via input unit 24 input and obtained by calculating part 25
Umber of pulse S that decompression is intervaloffset, actual draw interval umber of pulse SRPart.
Liquor charging control portion 27 is umber of pulse S interval according to the decompression being stored in storage part 26offset, real
Interval umber of pulse S is drawn on borderRCarry out the part of the control of liquid feeding device 3.Specifically, instruction is sent
Make to control pumping section 23, the action of open and close valve 7.
Output device 28 controls letter according to the instruction obtained from liquor charging control portion 27 to liquid feeding device 3 output
Number.
Fig. 3 is the example drawing interval pressure change in the liquor charging operation representing liquid feeding device
Chart.Transverse axis represents the umber of pulse (n) of the motor 21 required for the action of piston, and the longitudinal axis represents pressure
The value (MPa) of the pressure that sensor 12 detects.
Here, Ss represents the umber of pulse drawn in interval, SoffsetRepresent the umber of pulse in decompression interval, SR
Represent that reality draws the umber of pulse in interval.
Fig. 5 is the motion flow of the liquid feeding device 3 of embodiments of the present invention.
Fig. 7 represent the first cylinder 9 pressure change synoptic diagram and liquor charging operation in absorption side check-valves,
Spray an example of the operating state of side check-valves, open and close valve.It addition, in the figure 7, it is also represented by publishing picture
One example of the opening and closing timing drawing interval pressure change and open and close valve now shown in 3.With
The sucking action of one piston 13 starts the open and close controlling of open and close valve while starting in the case of, due to first
Cylinder 9 is not depressurized to atmospheric pressure, does not the most draw and becomes open with in the decompression interval of the first cylinder 9
The solvent that the open and close valve of state connects.
Illustrate that according to Fig. 3, Fig. 5 and Fig. 7 the liquor charging of present embodiment controls.
First, if the sucking action of first piston 13 starts (S501), then with this place by first
The liquor charging pressure of cylinder 9 is to atmospheric pressure (S502), and entrance side check-valves 8 is open (S503).
Thus, the actual absorption (S504) starting eluent.
If by the sucking action of first piston 13, being eluted liquid in the first cylinder 9 and fill up, fill knot
Bundle (S505), the most then starts the press-in action (S506) of first piston 13.
If the motion (changing with pressure) along with the fluid produced by the press-in action of first piston 13
And entrance side check-valves 8 closes (S507), then the eluent in the first cylinder 9 is compressed and the first cylinder
In 9 pressurized (S508).
If the pressure in the first cylinder 9 reaches the pressure of the eluent from the second cylinder 11 ejection, then spray
Go out side check-valves 10 to open (S509), the second piston 14 of the second cylinder 11 and the pressure of first piston 13
Entering action and synchronously carry out sucking action, eluent fills up in the second cylinder 11 (S510).
If being eluted liquid in the second cylinder 11 to fill up, end-of-fill (S511), the most then start second
The press-in action (S512) of piston 14.
If by the flowing of the fluid that the press-in action of the second piston 14 produces, thus ejection side check-valves
10 Guan Bis (S513), then spray the eluent (S514) of the inside of the second cylinder 11.
Here, Fig. 6 is to represent that the operating procedure of embodiments of the present invention and the most adjoint data process dress
Put the flow chart of the process of 110.
First, in the liquor charging operation started after the absorption operation shown in Fig. 5 terminates, metering enters from (1)
Mouth side check-valves 8 closes (S503), and (2) start the press-in action (S506) of first piston 13,
Pressure in (3) first cylinders 9 reaches the pressure P (S508) of the eluent from the second cylinder 11 ejection,
(4) displacement lc of the first piston 13 that ejection side check-valves 10 is required till opening (S509)
(S601)。
Displacement l at this moment is measured by the input unit 24 of data processing equipment 22c, such as, using step
In the case of entering motor, obtain according to umber of pulse.Alternatively, it is also possible to use rotary encoders etc. are according to electricity
The rotating speed of motivation obtains the piston displacement of compression section.
Here, use the cylinder volume V drawn when starting0, the ejection volume V of cylinder 1d, cylinder 1
Compression volume dVC, the increase of volume when being depressurized to atmospheric pressure when obtaining and draw according to formula (1) and start
Amount dV.
If here, displacement l of the piston 13 till using decompressionoffset, the piston 13 of compression section
Displacement lC, displacement l of piston 13 of liquor charging operationdDisplacement dV, Vd、dVC, then public affairs are obtained
Formula (2).
If using above-mentioned formula and umber of pulse conversion coefficient k, then represent S with following formulaoffset。
Then, according to umber of pulse S obtained based on above-mentioned formula (2)offsetWith the umber of pulse drawn in interval
SS, obtain umber of pulse S in actual absorption interval by following formulaR。
SR=SS-Soffset... formula (4)
Above-mentioned control unit 22 carries out above-mentioned calculating, the umber of pulse in the actual absorption interval obtained herein
SRIn, adjust opening/closing time and the timing (S605) of open and close valve 7a～7d, it is possible to realize the most also
And high-precision mixing ratio.
In the structure of the liquid feeding device 3 shown in Fig. 2, by being passed by the pressure being connected with the second cylinder 11
The pressure that sensor 12 measures is controlled.
As other forms, it is also possible to be applied between entrance side check-valves 8 and ejection side check-valves 10
Add in the liquid feeding device of pressure transducer.In this embodiment, it is possible to by additional pressure transducer
Directly measure the pressure in the first cylinder 9, therefore by more correctly being compressed from atmospheric pressure by the first cylinder 9
To the pressure of the second cylinder 11 liquor charging, it is possible to carry out the liquor charging that pressure fluctuation is little.
In the synoptic diagram of the liquid feeding device 3 of the present embodiment shown in Fig. 2, there is shown be connected in series 2
Tandem (series) liquid feeding device of individual cylinder gained, but it is being connected in parallel 2 cylinder gained also
Line liquid feeding device, the liquid feeding device driving piston to be characterized independently so that each cylinder is respectively provided with motor
In, unrelated with the type of drive of liquid feeding device, it is also possible to be applied to low pressure gradient liquor charging mode.Following description
These embodiments.
Embodiment 2
Fig. 8 represents an example of liquid feeding device, and they are different from the embodiment shown in Fig. 2, it is characterised in that:
Each cylinder has independent drive division and motor, drives piston independently.In this example embodiment, by with electricity
The rotary motion of motor is transformed to linear motion and drives piston by the direct acting drive division that motivation connects.
The rotary motion of motor 42,43 is passed to direct acting drive division 38,39, and piston 34,35 leads to
Cross the back and forth movement of direct acting drive division and back and forth movement.As this direct acting drive division, such as, can enumerate ball
Leading screw.
Direction of rotation according to the motor connected determines the moving direction of each piston, according to the rotating speed of motor
Identify the displacement of piston.Especially in the case of employing stepping motor, can be by the movement of piston
Distance is counted as umber of pulse.
Use be arranged on direct acting drive division 38,39 detection plate 36,37 and by optics, electrostatic capacitance,
The methods such as the magnetic line of force carry out the sensor 40,41 detected, and identify piston 34,35 by control unit 44
Position.Can also be different from detection method shown in the present embodiment, by using rotary encoder etc.
Identify the position of piston, displacement.
Pipe arrangement in the downstream of the second cylinder 32 arranges the pressure transducer 33 of the pressure in metering pipe arrangement, will
It is sent to control unit 44 by the value of the pressure in the pipe arrangement of this pressure transducer 33 metering.
Control unit 44, corresponding to the value of pressure in this pipe arrangement, liquor charging flow, controls turning of each motor
Speed, adjusts displacement and the translational speed of piston.
In the low pressure gradient mode of the liquid feeding device shown in Fig. 8, be arranged in switching device 2 multiple opens
The interval that valve closing 7a～the 7d also entrance side check-valves in the sucking action interval of the first cylinder is open is entered
Row on-off action.About the manner, it is also contemplated that by the application present invention and improves mixing ratio precision.
Embodiment 3
Fig. 9 represents an example of liquid feeding device, and they are different from the embodiment shown in Fig. 2, it is characterised in that
Each cylinder has been connected in parallel.
In the case of applying low pressure gradient in the liquid feeding device shown in Fig. 9, need to have switching valve
The switching device 2 of 7a～7d is arranged on the branch point 45 to first cylinder the 47, second cylinder 50 donor solvent
Upstream side.
In the liquid feeding device connecting each cylinder in (side by side) mode in parallel, it is characterised in that: connected
Each cylinder has the absorption of solvent, compresses, sprays operation.
Compression section from the solvent uptake of the first cylinder 47 to the solvent drawn terminates, the second cylinder
50 carry out system ejection downstream, individually from the solvent uptake of the second cylinder 50 to the solvent drawn
Till compression section terminates, the first cylinder 47 carries out system ejection downstream individually.
In the absorption operation of the first cylinder 47, by the suction action of first piston 53 by the first cylinder
Pressure in 47 is to atmospheric pressure, the filling that simultaneously start solvent open with entrance side check-valves 46.
In the interval that entrance side check-valves 46 is open, control unit 62 is by adjusting the opening and closing of relief valve 7a～7d
Time and timing make mixing ratio change, and change the ratio of components of eluent.
After being filled with solvent in the first cylinder 47, the press-in action of first piston 53 starts, entrance side
Check-valves 46 closes due to the flowing of produced fluid, and the eluent in the first cylinder 47 is compressed.
If the pressure in the first cylinder 47 be compressed to by pressure transducer 52 detect by the second cylinder
The pressure of 50 liquor chargings, then ejection side check-valves 48 is open, starts the liquor charging of the first cylinder 47.
It addition, the second cylinder 50 continuing liquor charging compensates the ejection of the first cylinder 47 while slowing down, make
Obtain liquor charging flow to fix and do not produce pressure oscillation.
At this moment, metering is closed in the first cylinder 47 from entrance side check-valves 46 and is compressed to the second cylinder
The pressure of the ejection of 50 and spray side check-valves 48 open till displacement l of first piston 531, root
Umber of pulse S in the decompression interval of the first cylinder 47 is calculated according to above-mentioned formula (1), formula (2)1offset
Umber of pulse S in interval is drawn with reality1R。
Use the S calculated1R、S1offset, the next absorption at the first cylinder 47 adjusts opening and closing in operation
The on-off action of valve 7a～7d.
If the second piston 54 of the second cylinder 50 stops, then the ejection side check-valves 51 of the second cylinder 50
The fluid produced due to the ejection from the first cylinder 47 flows and closes, and transfers to the list of the first cylinder 47
Solely ejection.In the ejection interval of the first cylinder 47, the second cylinder 50 carries out the suction of the solvent of sucking action
Compression till the liquor charging pressure of the solvent take, drawn.
If the pressure in the second cylinder 50 is compressed to by pressure transducer 52 detect by the first cylinder
The pressure of 47 liquor chargings, then ejection side check-valves 51 is open, starts the liquor charging of the second cylinder 50.
It addition, the first cylinder 47 continuing liquor charging compensates the ejection of the second cylinder 50 while slowing down, make
Obtain liquor charging constant flow and do not produce pressure oscillation.
At this moment, in the same manner as the first cylinder, calculate compression ratio V of the second cylinder 502P。
Metering is closed into the ejection pressure being compressed to the first cylinder in the second cylinder 50 from entrance side check-valves 49
Power and spray side check-valves 51 open till displacement l of the second piston 542, according to above-mentioned formula
(1) umber of pulse S during, (2) calculate the decompression interval of the second cylinder 502offsetInterval is drawn with reality
In umber of pulse S2R。
Use compression ratio V calculated2P, the S that calculates according to formula (2) and (3)2R、S2offset,
Next at the second cylinder 50 draws the on-off action of adjustment open and close valve 7a～7d in operation.
In the liquid feeding device being connected in parallel each cylinder, circulate by repeating above-mentioned driving, realize
The liquor charging that pressure oscillation is little.
According to piston displacement l calculated by control unit in the compression section of each cylinder, according to piston
Interval and the actual absorption interval of the decompression that displacement l calculates, adjusts the switching during absorption operation of each cylinder
The switching time of valve, it is possible to apply the present invention.
Additionally, in the above-described embodiment, illustrate to use absorption interval, decompression absorption district interval, actual
Between each interval in the umber of pulse of piston carry out the situation of control of open and close valve, but the application of the present invention is right
As being not limited to this, such as, it is also contemplated that the translational speed of piston, carry out on the basis of the time (sec)
Control.
Description of reference numerals
1: container (eluent)；2: switching device；3: liquid feeding device；4: sample injection unit；5:
Detached dowel；6: detector；7: open and close valve；8,29,46,49: entrance side check-valves；9,30,47:
First cylinder；10,31,48,51: ejection side check-valves；11,32,50: the second cylinder；12、33、
52: pressure transducer；13,34,53: first piston；14,35,54: the second piston；15,55:
First cam；16,56: the second cam；17,57: camshaft；18,58: belt；19,59: circle
Plate；20,60: sensor；21,61: motor；22,44,62: (data process dress to control unit
Put)；23: pumping section；24: input unit；25: calculating part；26: storage part；27: liquor charging control portion；
28: output unit；36,37: detection plate；38: the first direct acting drive divisions；39: the second direct acting drive divisions；
40: first sensor；41: the second sensors；42: the first motor；43: the second motor；45:
Branch.
Claims (14)
1. a liquid chromatograph, it possesses:
Liquid-feeding pump, its first pump unit connected in series or in parallel and second pump unit, carry out eluent absorption,
Ejection, wherein, this first pump unit and this second pump unit possess the suction inlet with above-mentioned eluent respectively
With the cylinder of ejiction opening, in above-mentioned cylinder the piston of back and forth movement；
Valve cell, it switches the kind of multiple eluents that above-mentioned liquid-feeding pump is drawn by on-off action；
Pressure transducer, the pressure of the eluent that its detection sprays from the ejiction opening of above-mentioned liquid-feeding pump；
Automatic sampling machine, in the stream of its eluent that liquid sample is injected into this ejection；
Detached dowel, it separates the liquid sample of this injection according to composition；
Detector, it detects each composition after this separation according to composition；
Control portion, the on-off action of its above-mentioned valve cell of control, this liquid chromatograph is characterised by,
The compression of the above-mentioned eluent that above-mentioned control portion is carried out according to the first piston in above-mentioned first pump unit
The displacement obtained in operation and ejection operation, obtains above-mentioned first piston and starts the suction of the plurality of eluent
Above-mentioned eluting behind decompression decompression interval interval, above-mentioned absorption to above-mentioned eluent starts after taking action
The actual actual absorption interval being drawn of liquid, is controlled such that and carries out in the actual absorption interval that this is obtained
The on-off action of above-mentioned valve cell.
Liquid chromatograph the most according to claim 1, it is characterised in that
Possess the motor driving above-mentioned piston,
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned electronic
Machine in above-mentioned decompression interval umber of pulse required for the action of above-mentioned first piston, actual draw district above-mentioned
Umber of pulse required for the action of above-mentioned first piston between.
Liquid chromatograph the most according to claim 1, it is characterised in that
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned first
The distance of piston movement in above-mentioned decompression interval and actual draw the distance of movement in interval above-mentioned.
Liquid chromatograph the most according to claim 1, it is characterised in that
Above-mentioned control portion controls the on-off action of above-mentioned valve cell in above-mentioned actual absorption is interval so that this suction
The mixing ratio change of the eluent taken.
Liquid chromatograph the most according to claim 1, it is characterised in that
It is also equipped with: detect the pressure transducer of pressure in above-mentioned cylinder,
Above-mentioned control portion is according to the first pressure by the pressure transducer detection of the pressure detected in above-mentioned cylinder
Value, the second pressure detected from the pressure transducer of the pressure of the eluent of the ejiction opening ejection of said pump by detection
Force value, controls the liquor charging of this eluent.
Liquid chromatograph the most according to claim 5, it is characterised in that
Possess the motor driving above-mentioned piston,
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned electronic
Machine in above-mentioned decompression interval umber of pulse required for the action of above-mentioned first piston, actual draw district above-mentioned
Umber of pulse required for the action of above-mentioned first piston between.
Liquid chromatograph the most according to claim 5, it is characterised in that
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned first
Distance that piston moves in above-mentioned decompression interval and in the above-mentioned actual distance drawing interval movement.
8. a liquid feeding device, it possesses:
Pumping section, its first pump unit connected in series or in parallel and second pump unit, carry out eluent absorption,
Ejection, wherein, this first pump unit and this second pump unit possess the suction inlet with above-mentioned eluent respectively
With the cylinder of ejiction opening, in above-mentioned cylinder the piston of back and forth movement；
Valve cell, it switches the kind of multiple eluents that above-mentioned pumping section is drawn by on-off action；
Pressure transducer, the pressure of the eluent that its detection sprays from the ejiction opening of above-mentioned pumping section；
Control portion, the on-off action of its above-mentioned valve cell of control, this liquid feeding device is characterised by,
The compression of the above-mentioned eluent that above-mentioned control portion is carried out according to the first piston in above-mentioned first pump unit
The displacement obtained in operation and ejection operation, obtains above-mentioned first piston and starts the suction of the plurality of eluent
Above-mentioned eluting behind decompression decompression interval interval, above-mentioned absorption to above-mentioned eluent starts after taking action
The actual actual absorption interval being drawn of liquid, is controlled such that and carries out in the actual absorption interval that this is obtained
The on-off action of above-mentioned valve cell.
Liquid feeding device the most according to claim 8, it is characterised in that
Possess the motor driving above-mentioned piston,
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned electronic
Machine in above-mentioned decompression interval umber of pulse required for the action of above-mentioned first piston, actual draw district above-mentioned
Umber of pulse required for the action of above-mentioned first piston between.
Liquid feeding device the most according to claim 8, it is characterised in that
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned first
Distance that piston moves in above-mentioned decompression interval and in the above-mentioned actual distance drawing interval movement.
11. liquid feeding devices according to claim 8, it is characterised in that
Above-mentioned control portion controls the on-off action of above-mentioned valve cell in above-mentioned actual absorption is interval so that this suction
The mixing ratio change of the eluent taken.
12. liquid feeding devices according to claim 8, it is characterised in that
It is also equipped with: detect the pressure transducer of pressure in above-mentioned cylinder,
Above-mentioned control portion is according to the first pressure by the pressure transducer detection of the pressure detected in above-mentioned cylinder
Value, second detected from the pressure transducer of the pressure of the eluent of the ejiction opening ejection of above-mentioned pumping section by detection
Force value, controls the liquor charging of this eluent.
13. liquid feeding devices according to claim 12, it is characterised in that
Possess the motor driving above-mentioned piston,
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned electronic
Machine in above-mentioned decompression interval umber of pulse required for the action of above-mentioned first piston, actual draw district above-mentioned
Umber of pulse required for the action of above-mentioned first piston between.
14. liquid feeding devices according to claim 12, it is characterised in that
Movement in the compression section of the above-mentioned eluent that above-mentioned control portion is carried out according to above-mentioned first piston away from
Displacement in the liquor charging operation of the above-mentioned eluent carried out from, above-mentioned first piston, obtains above-mentioned first
Distance that piston moves in above-mentioned decompression interval and in the above-mentioned actual distance drawing interval movement.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012183738 | 2012-08-23 | ||
| JP2012-183738 | 2012-08-23 | ||
| PCT/JP2013/070407 WO2014030498A1 (en) | 2012-08-23 | 2013-07-29 | Liquid chromatography device and liquid delivery device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104508478A CN104508478A (en) | 2015-04-08 |
| CN104508478B true CN104508478B (en) | 2016-08-24 |
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ID=50149808
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380041151.5A Active CN104508478B (en) | 2012-08-23 | 2013-07-29 | Liquid chromatograph and liquid feeding device |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP5887412B2 (en) |
| CN (1) | CN104508478B (en) |
| DE (1) | DE112013003747T5 (en) |
| WO (1) | WO2014030498A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7011921B2 (en) * | 2017-10-31 | 2022-02-10 | アークレイ株式会社 | Liquid feeding method |
| CN107632057B (en) * | 2017-10-31 | 2024-06-21 | 湖南三码头食品有限公司 | Quick continuous detection device for food |
| CN108217913A (en) * | 2018-02-05 | 2018-06-29 | 苏州思上环保科技有限公司 | A kind of sewage bactericidal unit |
| JP7186113B2 (en) * | 2019-03-01 | 2022-12-08 | 株式会社日立ハイテク | liquid transfer pump, liquid chromatograph |
| CN115190942A (en) * | 2020-03-24 | 2022-10-14 | 株式会社日立高新技术 | Liquid feeding device and liquid feeding method |
| CN115166119B (en) * | 2022-06-30 | 2024-06-14 | 华谱科仪(北京)科技有限公司 | High-precision low-pressure gradient method of high-performance liquid chromatograph |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0260760A2 (en) * | 1986-09-17 | 1988-03-23 | Philips Electronics Uk Limited | Liquid chromatograph |
| EP0840010A2 (en) * | 1996-10-29 | 1998-05-06 | Shimadzu Corporation | Plunger pump |
| US5852231A (en) * | 1996-03-29 | 1998-12-22 | Hitachi, Ltd. | Elution liquid control for a liquid chromatograph |
| EP2107241A2 (en) * | 2008-04-02 | 2009-10-07 | Thermo Fischer Scientific | A Piston Pump Having a Force Sensor and a Method for Controlling Said Pump |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2195473B (en) * | 1986-09-17 | 1990-08-15 | Philips Electronic Associated | Liquid chromatograph |
| JP2636699B2 (en) * | 1993-09-07 | 1997-07-30 | 株式会社島津製作所 | Liquid chromatograph |
| JP3849301B2 (en) * | 1998-06-01 | 2006-11-22 | 株式会社島津製作所 | Liquid chromatograph |
| JP5049808B2 (en) * | 2008-01-31 | 2012-10-17 | 株式会社日立ハイテクノロジーズ | Liquid feeding device and analyzer having the same |
-
2013
- 2013-07-29 CN CN201380041151.5A patent/CN104508478B/en active Active
- 2013-07-29 WO PCT/JP2013/070407 patent/WO2014030498A1/en active Application Filing
- 2013-07-29 DE DE112013003747.5T patent/DE112013003747T5/en active Pending
- 2013-07-29 JP JP2014531560A patent/JP5887412B2/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0260760A2 (en) * | 1986-09-17 | 1988-03-23 | Philips Electronics Uk Limited | Liquid chromatograph |
| US5852231A (en) * | 1996-03-29 | 1998-12-22 | Hitachi, Ltd. | Elution liquid control for a liquid chromatograph |
| EP0840010A2 (en) * | 1996-10-29 | 1998-05-06 | Shimadzu Corporation | Plunger pump |
| EP2107241A2 (en) * | 2008-04-02 | 2009-10-07 | Thermo Fischer Scientific | A Piston Pump Having a Force Sensor and a Method for Controlling Said Pump |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5887412B2 (en) | 2016-03-16 |
| JPWO2014030498A1 (en) | 2016-07-28 |
| CN104508478A (en) | 2015-04-08 |
| WO2014030498A1 (en) | 2014-02-27 |
| DE112013003747T5 (en) | 2015-08-20 |
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