CN106018637B - Have both low pressure ion chromatography and the instrument and application method of low pressure Flow Injection Analysis - Google Patents

Have both low pressure ion chromatography and the instrument and application method of low pressure Flow Injection Analysis Download PDF

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Publication number
CN106018637B
CN106018637B CN201610393222.3A CN201610393222A CN106018637B CN 106018637 B CN106018637 B CN 106018637B CN 201610393222 A CN201610393222 A CN 201610393222A CN 106018637 B CN106018637 B CN 106018637B
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analysis
liang
low
electromagnetic valve
way electromagnetic
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CN106018637A (en
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张新申
高昊东
马玉洁
靳皓琛
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Sichuan University
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Sichuan University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/06Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • G01N2030/201Injection using a sampling valve multiport valves, i.e. having more than two ports

Abstract

Have both low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis, including feed liquor flow path, analyze flow path, flow cell, detector and the computer processing system being connected with detector, the feed liquor flow path is by three-way magnetic valve, first low-lift pump, second low-lift pump, six-way injection valve, injection annulus and liquid delivery tube assemble, the analysis flow path includes the Flow Injection Analysis flow path suitable for optical detection, anion analysis flow path, cation analysis flow path and the Flow Injection Analysis flow path suitable for Conductivity detection, the flow cell is made of conductance flow cell and optical flow cell, the detector is made of electric conductivity detector and fluorescence detector.Using the instrument, the Flow Injection Analysis of optical detection, low pressure ion chromatography anion analysis, low pressure ion chromatography cation analysis can not only be carried out, moreover it is possible to carry out the Flow Injection Analysis of Conductivity detection.

Description

Have both low pressure ion chromatography and the instrument and application method of low pressure Flow Injection Analysis
Technical field
The invention belongs to detection and analysis fields during environment water analysis, more particularly to low pressure ion chromatography and flow injection The instrument of analysis.
Background technology
The chromatography of ions (IC) is by, by measured ion, being connected in ion exchange resin column separation liquid phase with electric conductivity detector The method of the ion of continuous detection chromatographic isolation, can also grasp in the high pressing operation of high pressure system under low pressure system low pressure Make.Flow injection analysis is to be examined by flow path with fluorescence detector or conductance with certain flow velocity by fluid to be measured and reagent Device is surveyed to be detected to form the method that spectrogram realizes measured matter analysis.Therefore, they are both needed to corresponding analytical instrument.Existing point It is single to analyse instrumental function, i.e., only there is the ion-chromatographic analyzer of ion chromatography or the stream of Flow Injection Analysis function Dynamic Injection Analysis instrument, when need to carry out Flow Injection Analysis when not only needing progress ion chromatography, need to purchase two alanysis instrument Device not only increases original equipment cost, but also increases the placement space of equipment.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide have both low pressure ion chromatography and low pressure flow injection The instrument and application method of analysis, to possess the need that an instrument can meet ion chromatography and Flow Injection Analysis It will.
The instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis, including feed liquor flow path, analysis Flow path, flow cell, detector and the computer processing system being connected with detector, the feed liquor flow path is by three-way magnetic valve, One low-lift pump, the second low-lift pump, six-way injection valve, injection annulus and liquid delivery tube assemble, and liquid delivery tube includes sample Or standard specimen delivery pipe, promote liquid delivery pipe, eluent delivery pipe, first share take over, developing solution delivery pipe and second is shared and connect Pipe;The analysis flow path includes the Flow Injection Analysis flow path suitable for optical detection, anion analysis flow path and cation point Analyse flow path;The flow cell is made of conductance flow cell and optical flow cell, and the detector is examined by electric conductivity detector and optics Survey device composition;Sample or standard specimen delivery pipe are connected with an inlet of the first low-lift pump and six-way injection valve, promote liquid conveying Pipe, eluent delivery pipe different from three-way magnetic valve inlets connection respectively, first shares to take over and goes out with three-way magnetic valve The inlet connection of liquid mouth, the first low-lift pump and six-way injection valve, second shares to take over and goes out with one of six-way injection valve Liquid mouth connects, and one end of injection annulus is connected by an inlet of pipe fitting and six-way injection valve, the other end by pipe fitting with The liquid outlet connection of six-way injection valve;Suitable for optical detection Flow Injection Analysis flow path by first liang of three-way electromagnetic valve, Mixer, reactor are connected in sequence by pipe fitting, and the inlet of first liang of three-way electromagnetic valve is common by pipe fitting and second With connection is taken over, the liquid outlet of the reactor is connected by pipe fitting with optical flow cell, the developing solution delivery pipe and second Low-lift pump is connected with mixer;Anion analysis flow path is passed through by second liang of three-way electromagnetic valve, low pressure anion separation column, suppressed column Pipe fitting is connected in sequence, and the inlet of second liang of three-way electromagnetic valve shares to take over by pipe fitting with second to be connected, the suppression The liquid outlet of column processed is connected by pipe fitting with conductance flow cell;Cation analysis flow path by the 3rd liang of three-way electromagnetic valve and low pressure sun from Sub- splitter is formed by connecting by pipe fitting, and the inlet of the 3rd liang of three-way electromagnetic valve shares the company of taking over by pipe fitting and second It connects, the liquid outlet of the low pressure cation separation column is connected by pipe fitting with conductance flow cell.
In above-mentioned instrument, analysis flow path can also increase the Flow Injection Analysis flow path suitable for Conductivity detection, this is suitable for The Flow Injection Analysis flow path of Conductivity detection is formed by connecting by the 4th liang of three-way electromagnetic valve and buffer by pipe fitting, described 4th liang The inlet of three-way electromagnetic valve is shared to take over and is connected by pipe fitting with second, and the liquid outlet of the buffer passes through pipe fitting and conductance stream Logical pond connection.
The instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis, when analysis flow path be suitable for When the Flow Injection Analysis flow path of optical detection, anion analysis flow path and cation analysis flow path, optical detection can be carried out Flow Injection Analysis, low pressure ion chromatography anion analysis and low pressure ion chromatography cation analysis;When analysis flow path is applicable In the Flow Injection Analysis flow path of optical detection, anion analysis flow path, cation analysis flow path and suitable for Conductivity detection During Flow Injection Analysis flow path, can carry out the Flow Injection Analysis of optical detection, low pressure ion chromatography anion analysis, low pressure from The Flow Injection Analysis of sub- chromatography cation analysis and Conductivity detection.
The instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis is the first low-lift pump, second low The pressure of press pump is not higher than 2 × 105Pa~3 × 105Pa, flow are 0.5mL/min~2.0mL/min.
The instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis, low-lift pump, threeway electromagnetism Valve, two three-way electromagnetic valves, conductance flow cell, electric conductivity detector, optical flow cell, fluorescence detector buffer and suppressed column can lead to Cross market purchase;Six-way injection valve can both be bought by market, also can as disclosed in CN 02244841.1 structure fabrication;Low pressure Anion separation column and low pressure cation separation column are selected according to analyzed ion, can both be bought, and can also refer to by market Column packing production method disclosed in CN 201410098759.8, CN 201210201081.2 makes.
Low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis are had both described in of the present invention, application method is as follows:
1st, low pressure ion chromatography anion analysis is carried out
1. when analysis flow path is the Flow Injection Analysis flow path, anion analysis flow path and cation suitable for optical detection When analyzing flow path, the inlet of three-way magnetic valve connection eluent delivery pipe is made to open and be communicated with liquid outlet, be connected promotion liquid The inlet of delivery pipe is closed, and second liang of three-way electromagnetic valve is made to be in opening, makes the 3rd liang of three-way electromagnetic valve, first liang of energization magnetic Valve is closed, and is closed the second low-lift pump, the first low-lift pump is in opening;
When analysis flow path is suitable for the Flow Injection Analysis flow path of optical detection, anion analysis flow path, cation point When analysing flow path and the Flow Injection Analysis flow path suitable for Conductivity detection, make the feed liquor of three-way magnetic valve connection eluent delivery pipe Mouth is opened and communicated with liquid outlet, is connected the inlet closing for promoting liquid delivery pipe, and second liang of three-way electromagnetic valve is made to be in opening state State is closed the 3rd liang of three-way electromagnetic valve, first liang of three-way electromagnetic valve, the 4th liang of three-way electromagnetic valve, makes at the second low-lift pump Opening is in closed state, the first low-lift pump;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction shape State makes standard specimen S2 or sample S1 be full of injection annulus by the driving of the first low-lift pump, then analytical instrument is converted to analysis shape State carries out the mapping of standard specimen or sample chromatogram.
2nd, low pressure ion chromatography cation analysis is carried out
1. when analysis flow path is the Flow Injection Analysis flow path, anion analysis flow path and cation suitable for optical detection When analyzing flow path, the inlet of three-way magnetic valve connection eluent delivery pipe is made to open and be communicated with liquid outlet, be connected promotion liquid The inlet of delivery pipe is closed, and the 3rd liang of three-way electromagnetic valve is made to be in opening, makes second liang of three-way electromagnetic valve, first liang of energization magnetic Valve is closed, and is closed the second low-lift pump, the first low-lift pump is in opening;
When analysis flow path is suitable for the Flow Injection Analysis flow path of optical detection, anion analysis flow path, cation point When analysing flow path and the Flow Injection Analysis flow path suitable for Conductivity detection, make the feed liquor of three-way magnetic valve connection eluent delivery pipe Mouth is opened and communicated with liquid outlet, is connected the inlet closing for promoting liquid delivery pipe, and the 3rd liang of three-way electromagnetic valve is made to be in opening state State is closed second liang of three-way electromagnetic valve, first liang of three-way electromagnetic valve, the 4th liang of three-way electromagnetic valve, makes at the second low-lift pump Opening is in closed state, the first low-lift pump;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction shape State makes standard specimen S2 or sample S1 be full of injection annulus by the driving of the first low-lift pump, then analytical instrument is converted to analysis shape State carries out the mapping of standard specimen or sample chromatogram.
3rd, optical detection Flow Injection Analysis is carried out
1. when analysis flow path is the Flow Injection Analysis flow path, anion analysis flow path and cation suitable for optical detection When analyzing flow path, the inlet that three-way magnetic valve connection promotes liquid delivery pipe is made to open and be communicated with liquid outlet, be connected eluent The inlet of delivery pipe is closed, and first liang of three-way electromagnetic valve is made to be in opening, makes second liang of three-way electromagnetic valve, the 3rd liang of energization magnetic Valve is closed, and the second low-lift pump, the first low-lift pump is made to be in opening;
When analysis flow path is suitable for the Flow Injection Analysis flow path of optical detection, anion analysis flow path, cation point When analysing flow path and the Flow Injection Analysis flow path suitable for Conductivity detection, three-way magnetic valve connection is made to promote the feed liquor of liquid delivery pipe Mouth is opened and the inlet closing of eluent delivery pipe is communicated, be connected with liquid outlet, and first liang of three-way electromagnetic valve is made to be in opening state State is closed second liang of three-way electromagnetic valve, the 3rd liang of three-way electromagnetic valve, the 4th liang of three-way electromagnetic valve, makes the second low-lift pump, One low-lift pump is in opening;
2. analyzer is arranged on analysis state carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump makes standard specimen S2 or sample S1 be full of injection annulus, then analytical instrument is converted to analysis state, into The mapping of rower sample or sample spectrogram.
4th, Conductivity detection Flow Injection Analysis is carried out
1. it is suitable for the Flow Injection Analysis flow path of optical detection, anion analysis flow path, cation point to analyze flow path Flow path and the Flow Injection Analysis flow path suitable for Conductivity detection are analysed, three-way magnetic valve connection is made to promote the inlet of liquid delivery pipe The inlet opened and eluent delivery pipe is communicated, be connected with liquid outlet is closed, and the 4th liang of three-way electromagnetic valve is made to be in opening, First liang of three-way electromagnetic valve, second liang of three-way electromagnetic valve, the 3rd liang of three-way electromagnetic valve are closed, the first low-lift pump is in and opens State is opened, the second low-lift pump is closed;
2. analyzer is arranged on analysis state carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump makes standard specimen S2 or sample S1 be full of injection annulus, then analytical instrument is converted to analysis state, into The mapping of rower sample or sample spectrogram.
Compared with prior art, the invention has the advantages that:
1st, the instrument provided by the invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis is new multi-functional Analytical instrument can not only carry out the Flow Injection Analysis of optical detection, low pressure ion chromatography anion analysis, low pressure ion chromatography Cation analysis, moreover it is possible to carry out the Flow Injection Analysis of Conductivity detection.
2nd, since the instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis is multifunctional analysis Therefore instrument, possesses the needs that such instrument can meet ion chromatography and Flow Injection Analysis.
3rd, due to possessing an instrument of the present invention with regard to the needs of ion chromatography and Flow Injection Analysis can be met, Therefore for a user, original equipment cost can be not only reduced using instrument of the present invention, but also the placement that can reduce equipment is empty Between, be conducive to the application and popularization of low pressure ion chromatography and Flow Injection Analysis Method.
4th, instrument of the present invention is easy to use, and the opening and closing of control valve and low-lift pump is only needed to achieve that optics is examined The Flow Injection Analysis of survey, low pressure ion chromatography anion analysis, the stream of low pressure ion chromatography cation analysis or Conductivity detection Dynamic Injection Analysis.
5th, carrying out low pressure ion chromatography analysis and low pressure Flow Injection Analysis using instrument of the present invention can obtain very Good effect.
Description of the drawings
Fig. 1 is that the first structure of the instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis is shown It is intended to, instrument is in analysis state;
Fig. 2 is low pressure ion chromatography to be had both described in Fig. 1 and the instrument of low pressure Flow Injection Analysis is in showing for sample introduction state It is intended to;
Fig. 3 is that second of structure of the instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis is shown It is intended to, instrument is in analysis state;
Fig. 4 is low pressure ion chromatography to be had both described in Fig. 3 and the instrument of low pressure Flow Injection Analysis is in showing for sample introduction state It is intended to.
In figure, 1-three-way magnetic valve, the 2-the first low-lift pump, the 3-the second low-lift pump, 4-six-way injection valve, 5-sample introduction Ring, 6-1-sample or standard specimen delivery pipe, 6-2-promotion liquid delivery pipe, 6-3-eluent delivery pipe, 6-4-the first share and connect Pipe, 6-5-developing solution delivery pipe, 6-6-the second share take over, 7-the first liang of three-way electromagnetic valve, 8-the second liang of three-way electromagnetic valve, 9-the three liang of three-way electromagnetic valve, 10-mixer, 11-low pressure anion separation column, 12-suppressed column, 13-low pressure cation point From column, 14-conductance flow cell, 15-electric conductivity detector, 16-reactor, 17-optical flow cell, 18-fluorescence detector, 19-computer processing system, 20-the four liang of three-way electromagnetic valve, 21-buffer, S1-sample, S2-standard specimen, C-promotion liquid, R-developing solution, E-eluent.
Specific embodiment
Below by embodiment to the instrument of the present invention for having both low pressure ion chromatography and low pressure Flow Injection Analysis and Its application method is described further.
In following embodiments, when analytical instrument is arranged to analysis state, the inlet c and liquid outlet d of six-way injection valve 6 Conducting, inlet a is turned on liquid outlet b, inlet e is turned on liquid outlet f;When analytical instrument is arranged to sample introduction state, six The inlet c of logical sampling valve 6 is turned on liquid outlet b, inlet a is turned on liquid outlet f, inlet e is turned on liquid outlet d.
Embodiment 1
In the present embodiment, the instrument of low pressure ion chromatography and low pressure Flow Injection Analysis is had both as shown in Figure 1 and Figure 2, including Feed liquor flow path, analysis flow path, flow cell, detector and the computer processing system 19 being connected with detector, the feed liquor flow path By the assembling of three-way magnetic valve 1, the first low-lift pump 2, the second low-lift pump 3, six-way injection valve 4, injection annulus 5 and liquid delivery tube Into liquid delivery tube includes sample or standard specimen delivery pipe 6-1, liquid delivery pipe 6-2, eluent delivery pipe 6-3, first is promoted to share Take over 6-4, developing solution delivery pipe 6-5 and second share take over 6-6;The analysis flow path includes the flowing suitable for optical detection Injection Analysis flow path, anion analysis flow path and cation analysis flow path;The flow cell is by conductance flow cell 14 and optical flow Logical pond 17 forms, and the detector is made of electric conductivity detector 15 and fluorescence detector 18;
Sample or standard specimen delivery pipe 6-1 are connected with an inlet of the first low-lift pump 2 and six-way injection valve 4, promote liquid Delivery pipe 6-2, eluent delivery pipe 6-3 different from three-way magnetic valve 1 inlets connection respectively, first share take over 6-4 with The inlet connection of the liquid outlet of three-way magnetic valve 1, the first low-lift pump 2 and six-way injection valve 4, second shares take over 6-6 It is connected with a liquid outlet of six-way injection valve 4, one end of injection annulus 5 passes through pipe fitting and an inlet of six-way injection valve 4 Connection, the other end are connected by pipe fitting with a liquid outlet of six-way injection valve 4;
Led to suitable for the Flow Injection Analysis flow path of optical detection by first liang of three-way electromagnetic valve 7, mixer 10, reactor 16 Pipe fitting to be crossed to be connected in sequence, the inlet of first liang of three-way electromagnetic valve 7 shares take over 6-6 with second by pipe fitting and is connected, The liquid outlet of the reactor 16 is connected by pipe fitting with optical flow cell 17, the developing solution delivery pipe 6-5 and the second low pressure Pump 3 and mixer 10 connect;Anion analysis flow path is by second liang of three-way electromagnetic valve 8, low pressure anion separation column 11, suppressed column 12 It is connected in sequence by pipe fitting, the inlet of second liang of three-way electromagnetic valve 8 shares take over 6-6 by pipe fitting and second and connects It connects, the liquid outlet of the suppressed column 12 is connected by pipe fitting with conductance flow cell 14;Cation analysis flow path is by the 3rd liang of energization Magnet valve 9 and low pressure cation separation column 13 are formed by connecting by pipe fitting, and the inlet of the 3rd liang of three-way electromagnetic valve 9 passes through pipe fitting Take over 6-6 is shared with second to be connected, the liquid outlet of the low pressure cation separation column 13 is connected by pipe fitting and conductance flow cell 14 It connects.
Low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis are had both described in the present embodiment, low-voltage ion color can be carried out It is as follows to compose anion analysis, low pressure ion chromatography cation analysis and optical detection Flow Injection Analysis, application method:
I carries out low pressure ion chromatography anion analysis
1. the inlet that three-way magnetic valve 1 connects eluent delivery pipe 6-3 is made to open and be communicated with liquid outlet, be connected promotion The inlet of liquid delivery pipe 6-2 is closed, and second liang of three-way electromagnetic valve 8 is made to be in opening, makes the 3rd liang of three-way electromagnetic valve 9, first Two three-way electromagnetic valves 7 are closed, and are closed the second low-lift pump 3, the first low-lift pump 2 is in opening;
2. analyzer is arranged on analysis state, under the driving of the first low-lift pump 2, eluent E is through eluent delivery pipe 6-3, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4, injection annulus 5, six-way injection valve 4, second and share and take over 6-6, second liang of three-way electromagnetic valve 8, low pressure anion separation column 11, suppressed column 12 enter conductance flow cell 14, through electric conductivity detector 15, which transmit a signal to computer processing system 19, is handled, and obtains baseline;
3. converting analytical instrument to sample introduction state, under the driving of the first low-lift pump 2, sample S1 or standard specimen S2 are through first Injection annulus into injection annulus 5 and are full of by low-lift pump 2, six-way injection valve 4;
4. again converting analytical instrument to analysis state, under the driving of the first low-lift pump 2, eluent E is defeated through eluent Pipe 6-3, three-way magnetic valve 1, first is sent to share take over 6-4, six-way injection valve 4 into injection annulus 5, by the sample S1 in injection annulus Or standard specimen S2 push-in low pressure anion separation column 11, in sample S1 or standard specimen S2 by measured ion in low pressure anion separation column 11 In be separated from each other after exit into suppressed column 12 respectively, in suppressed column eliminate eluent background conductance interference after enter conductance Flow cell 14 transmits a signal to computer processing system 19 through electric conductivity detector 15 and handles, and obtains the chromatography of sample or standard specimen Figure;
5. using a series of standard specimen of various concentrations, the chromatogram and drawing curve of a series of standard specimens are obtained, is passed through The regression equation of working curve can be calculated in sample by the concentration of measured ion.
II carries out low pressure ion chromatography cation analysis
1. the inlet that three-way magnetic valve 1 connects eluent delivery pipe 6-3 is made to open and be communicated with liquid outlet, be connected promotion The inlet of liquid delivery pipe 6-2 is closed, and the 3rd liang of three-way electromagnetic valve 9 is made to be in opening, makes second liang of three-way electromagnetic valve 8, first Two three-way electromagnetic valves 7 are closed, and are closed the second low-lift pump 3, the first low-lift pump 2 is in opening;
2. analyzer is arranged on analysis state (see Fig. 1), under the driving of the first low-lift pump 2, eluent E is through eluent Delivery pipe 6-3, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4, injection annulus 5, six-way injection valve 4, second and are total to Enter conductance flow cell 14 with take over 6-6, the 3rd liang of three-way electromagnetic valve 9, low pressure cation separation column 13, it will through electric conductivity detector 15 Signal transmission is handled to computer processing system 19, obtains baseline;
3. analytical instrument is converted to sample introduction state (see Fig. 2), under the driving of the first low-lift pump 2, sample S1 or standard specimen Injection annulus into injection annulus 5 and are full of by S2 through the first low-lift pump 2, six-way injection valve 4;
4. again converting analytical instrument to analysis state (see Fig. 1), under the driving of the first low-lift pump 2, eluent E is through washing De- liquid delivery pipe 6-3, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4 enters injection annulus 5, will be in injection annulus 5 Sample S1 or standard specimen S2 push-in low pressure cation separation column 13, in sample S1 or standard specimen S2 by measured ion in low pressure cation Conductance flow cell 14 is exited into after being separated from each other in splitter 13 respectively, computer is transmitted a signal to through electric conductivity detector 15 Processing system 19 is handled, and obtains the chromatogram of sample or standard specimen;
5. using a series of standard specimen of various concentrations, the chromatogram and drawing curve of a series of standard specimens are obtained, is passed through The regression equation of working curve can be calculated in sample by the concentration of measured ion;
III optical detection Flow Injection Analysis
1. the inlet that the connection of three-way magnetic valve 1 promotes liquid delivery pipe 6-2 is made to open and be communicated with liquid outlet, be connected elution The inlet of liquid delivery pipe 6-3 is closed, and first liang of three-way electromagnetic valve 7 is made to be in opening, makes second liang of three-way electromagnetic valve the 8, the 3rd Two three-way electromagnetic valves 9 are closed, and the second low-lift pump 3, the first low-lift pump 2 is made to be in opening;
2. analyzer is arranged on analysis state (see Fig. 1), under the driving of the first low-lift pump 2, liquid C is promoted through promoting liquid Delivery pipe 6-2, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4, injection annulus 5, six-way injection valve 4, second and are total to Enter mixer 10 with take over 6-6, the first solenoid valve 7, under the driving of the second low-lift pump 3, developing solution R is through developing solution delivery pipe 6-5 enters mixer 10 with liquid C is promoted to be mixed to form mixed liquor, and the reacted device 16 of mixed liquor enters optical flow cell 17, Computer processing system 19 is transmitted a signal to through fluorescence detector 18 to handle, and obtains baseline;
3. analytical instrument is converted to sample introduction state (see Fig. 2), under the driving of the first low-lift pump 2, sample S1 or standard specimen Injection annulus into injection annulus 5 and are full of by S2 through the first low-lift pump 2, six-way injection valve 4;
4. again converting analytical instrument to analysis state (see Fig. 1), under the driving of the first low-lift pump 2, liquid C is promoted through pushing away Hydrodynamic delivery pipe 6-2, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4 enters injection annulus 5, promote sample S1 or Standard specimen S2 is pushed into mixer 10, and under the driving of the second low-lift pump 3, developing solution R enters mixer 10 through developing solution delivery pipe 6-5 Colored complex is generated into reactor 16 after being mixed with sample S1 or standard specimen S2, the liquid containing colored complex enters optical flow Logical pond 17, transmits a signal to computer processing system 19 through fluorescence detector 18 and handles, obtain sample or standard specimen spectrogram;
5. using a series of standard specimen of various concentrations, the spectrogram and drawing curve of a series of standard specimens are obtained, passes through work The concentration of measured matter in sample can be calculated by making the regression equation of curve.
Embodiment 2
In the present embodiment, the instrument of low pressure ion chromatography and low pressure Flow Injection Analysis is had both as shown in Figure 3, Figure 4, including Feed liquor flow path, analysis flow path, flow cell, detector and the computer processing system 19 being connected with detector.It is different from embodiment 1 Part is to analyze flow path to add Flow Injection Analysis flow path suitable for Conductivity detection, should be noted suitable for flowing of Conductivity detection Analysis flow path is penetrated to be formed by connecting by pipe fitting by the 4th liang of three-way electromagnetic valve 20 and buffer 21, the 4th liang of three-way electromagnetic valve 20 Inlet shares take over 6-6 with second by pipe fitting and is connected, and the liquid outlet of the buffer 21 passes through pipe fitting and conductance flow cell 14 connections.
Low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis are had both described in the present embodiment, optical detection can be carried out Flow Injection Analysis, low pressure ion chromatography anion analysis, the flowing of low pressure ion chromatography cation analysis and Conductivity detection are noted Penetrate analysis.The Flow Injection Analysis of the optical detection, low pressure ion chromatography anion analysis, low pressure ion chromatography cation point The application method of analysis is a difference in that with embodiment 1:4th liang of three-way electromagnetic valve 20 should be at closed state.Except above-mentioned difference Place is outer, and other operations are same as Example 1.The Flow Injection Analysis of the Conductivity detection, application method are as follows:
1. the inlet that the connection of three-way magnetic valve 1 promotes liquid delivery pipe 6-2 is made to open and be communicated with liquid outlet, be connected elution The inlet of liquid delivery pipe 6-3 is closed, and the 4th liang of three-way electromagnetic valve 20 is made to be in opening, makes first liang of three-way electromagnetic valve 7, second Two three-way electromagnetic valves 8, the 3rd liang of three-way electromagnetic valve 9 are closed, and the first low-lift pump 2 is made to be in opening, the second low-lift pump 3 It is closed;
2. analyzer is arranged on analysis state (see Fig. 3), under the driving of the first low-lift pump 2, liquid C is promoted through promoting liquid Delivery pipe 6-2, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4, injection annulus 5, six-way injection valve 4, second and are total to Enter conductance flow cell 14 with take over 6-6, the 4th liang of three-way electromagnetic valve 20, buffer 21, through electric conductivity detector 15 by signal transmission It is handled to computer processing system 19, obtains baseline;
3. analytical instrument is converted to sample introduction state (see Fig. 4), under the driving of the first low-lift pump 2, sample S1 or standard specimen Injection annulus into injection annulus 5 and are full of by S2 through the first low-lift pump 2, six-way injection valve 4;
4. again converting analytical instrument to analysis state (see Fig. 3), under the driving of the first low-lift pump 2, liquid C is promoted through pushing away Hydrodynamic delivery pipe 6-2, three-way magnetic valve 1, first share take over 6-4, six-way injection valve 4 into injection annulus 5 promote sample S1 or Standard specimen S2 enters conductance flow cell 14 through the 4th liang of three-way electromagnetic valve 20, buffer 21, is transmitted a signal to through electric conductivity detector 15 Computer processing system 19 is handled, and obtains sample or standard specimen spectrogram;
5. using a series of standard specimen of various concentrations, the spectrogram and drawing curve of a series of standard specimens are obtained, passes through work Make curve and sample spectrogram it can be learnt that measured matter electric conductivity value in sample.

Claims (4)

1. have both low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis, including feed liquor flow path, analysis flow path, flow cell, Detector and the computer processing system (19) being connected with detector, it is characterised in that the feed liquor flow path is by three-way magnetic valve (1), the first low-lift pump (2), the second low-lift pump (3), six-way injection valve (4), injection annulus (5) and liquid delivery tube assemble, Liquid delivery tube includes sample or standard specimen delivery pipe (6-1), promotes liquid delivery pipe (6-2), eluent delivery pipe (6-3), first It shares and takes over (6-4), developing solution delivery pipe (6-5) and second shared is taken over (6-6);The analysis flow path includes being suitable for optics Flow Injection Analysis flow path, anion analysis flow path and the cation analysis flow path of detection;The flow cell is by conductance flow cell (14) it is made of with optical flow cell (17) composition, the detector electric conductivity detector (15) and fluorescence detector (18);First Low-lift pump, the pressure of the second low-lift pump are not higher than 2 × 105Pa~3 × 105Pa, flow are 0.5mL/min~2.0mL/min;
Sample or standard specimen delivery pipe (6-1) are connected with an inlet of the first low-lift pump (2) and six-way injection valve (4), are promoted Liquid delivery pipe (6-2), eluent delivery pipe (6-3) respectively from the different inlets of three-way magnetic valve (1) connect, first share connect Pipe (6-4) and the liquid outlet of three-way magnetic valve (1), an inlet of the first low-lift pump (2) and six-way injection valve (4) are connected, Second shares and takes over (6-6) and be connected with a liquid outlet of six-way injection valve (4), and one end of injection annulus (5) passes through pipe fitting and six The inlet connection of logical sampling valve (4), the other end are connected by pipe fitting with a liquid outlet of six-way injection valve (4);
Suitable for optical detection Flow Injection Analysis flow path by first liang of three-way electromagnetic valve (7), mixer (10), reactor (16) It is connected in sequence by pipe fitting, the inlet of first liang of three-way electromagnetic valve (7) is shared by pipe fitting and second to be taken over (6-6) Connection, the liquid outlet of the reactor (16) are connected by pipe fitting with optical flow cell (17), the developing solution delivery pipe (6-5) It is connected with the second low-lift pump (3) and mixer (10);
Anion analysis flow path passes through pipe fitting by second liang of three-way electromagnetic valve (8), low pressure anion separation column (11), suppressed column (12) It is connected in sequence, the inlet of second liang of three-way electromagnetic valve (8) is shared by pipe fitting with second to be taken over (6-6) and be connected, institute The liquid outlet for stating suppressed column (12) is connected by pipe fitting with conductance flow cell (14);
Cation analysis flow path is formed by connecting by the 3rd liang of three-way electromagnetic valve (9) and low pressure cation separation column (13) by pipe fitting, The inlet of the 3rd liang of three-way electromagnetic valve (9) is shared with second by pipe fitting and takes over (6-6) and be connected, and the low pressure cation divides Liquid outlet from column (13) is connected by pipe fitting with conductance flow cell (14).
2. low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis are had both according to claim 1, it is characterised in that point Analysing flow path includes the Flow Injection Analysis flow path for being suitable for Conductivity detection, should be suitable for the Flow Injection Analysis flow path of Conductivity detection It is formed by connecting by the 4th liang of three-way electromagnetic valve (20) and buffer (21) by pipe fitting, the feed liquor of the 4th liang of three-way electromagnetic valve (20) Mouthful by pipe fitting with second it is shared take over (6-6) and be connected, the liquid outlet of the buffer (21) passes through pipe fitting and conductance flow cell (14) connect.
3. the application method of low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis, feature are had both described in claim 1 It is:
Carry out low pressure ion chromatography anion analysis
1. the inlet of three-way magnetic valve (1) connection elution liquid pipe (6-3) is made to open and be communicated with liquid outlet, is connected promotion liquid pipe The inlet of (6-2) is closed, and second liang of three-way electromagnetic valve (8) is made to be in opening, make the 3rd liang of three-way electromagnetic valve (9), first liang Three-way electromagnetic valve (7) is closed, and is closed the second low-lift pump (3), the first low-lift pump (2) is in opening state State;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus, then analytical instrument is converted to analysis State carries out the mapping of standard specimen or sample chromatogram;
Or carry out low pressure ion chromatography cation analysis
1. the inlet of three-way magnetic valve (1) connection elution liquid pipe (6-3) is made to open and be communicated with liquid outlet, is connected promotion liquid pipe The inlet of (6-2) is closed, and the 3rd liang of three-way electromagnetic valve (9) is made to be in opening, make second liang of three-way electromagnetic valve (8), first liang Three-way electromagnetic valve (7) is closed, and is closed the second low-lift pump (3), the first low-lift pump (2) is in opening state State;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus (5), then by analytical instrument convert to point Analysis state carries out the mapping of standard specimen or sample chromatogram;
Or carry out optical detection Flow Injection Analysis
1. make three-way magnetic valve (1) connection that the inlet of liquid pipe (6-2) be promoted to open and communicated with liquid outlet, be connected elution liquid pipe The inlet of (6-3) is closed, and first liang of three-way electromagnetic valve (7) is made to be in opening, make second liang of three-way electromagnetic valve (8), the 3rd liang Three-way electromagnetic valve (9) is closed, and the second low-lift pump (3), the first low-lift pump (2) is made to be in opening;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus, then analytical instrument is converted to analysis State carries out the mapping of standard specimen or sample spectrogram.
4. the application method of low pressure ion chromatography and the instrument of low pressure Flow Injection Analysis, feature are had both described in claim 2 It is that workflow is as follows:
Carry out low pressure ion chromatography anion analysis
1. the inlet of three-way magnetic valve (1) connection elution liquid pipe (6-3) is made to open and be communicated with liquid outlet, is connected promotion liquid pipe The inlet of (6-2) is closed, and second liang of three-way electromagnetic valve (8) is made to be in opening, make the 3rd liang of three-way electromagnetic valve (9), first liang Three-way electromagnetic valve (7), the 4th liang of three-way electromagnetic valve (20) are closed, and are closed the second low-lift pump (3), are first low Press pump (2) is in opening;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus, then analytical instrument is converted to analysis State carries out the mapping of standard specimen or sample chromatogram;
Or carry out low pressure ion chromatography cation analysis
1. the inlet of three-way magnetic valve (1) connection elution liquid pipe (6-3) is made to open and be communicated with liquid outlet, is connected promotion liquid pipe The inlet of (6-2) is closed, and the 3rd liang of three-way electromagnetic valve (9) is made to be in opening, make second liang of three-way electromagnetic valve (8), first liang Three-way electromagnetic valve (7), the 4th liang of three-way electromagnetic valve (20) are closed, and are closed the second low-lift pump (3), are first low Press pump (2) is in opening;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus (5), then by analytical instrument convert to point Analysis state carries out the mapping of standard specimen or sample chromatogram;
Or carry out optical detection Flow Injection Analysis
1. make three-way magnetic valve (1) connection that the inlet of liquid pipe (6-2) be promoted to open and communicated with liquid outlet, be connected elution liquid pipe The inlet of (6-3) is closed, and first liang of three-way electromagnetic valve (7) is made to be in opening, make second liang of three-way electromagnetic valve (8), the 3rd liang Three-way electromagnetic valve (9), the 4th liang of three-way electromagnetic valve (20) are closed, and the second low-lift pump (3), the first low-lift pump (2) is made to locate In opening;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus, then analytical instrument is converted to analysis State carries out the mapping of standard specimen or sample spectrogram;
Or carry out Conductivity detection Flow Injection Analysis
1. make three-way magnetic valve (1) connection that the inlet of liquid pipe (6-2) be promoted to open and communicated with liquid outlet, be connected elution liquid pipe The inlet of (6-3) is closed, and the 4th liang of three-way electromagnetic valve (20) is made to be in opening, make first liang of three-way electromagnetic valve (7), second liang Three-way electromagnetic valve (8), the 3rd liang of three-way electromagnetic valve (9) are closed, and the first low-lift pump (2) are made to be in opening, second is low Press pump (3) is closed;
2. analyzer is arranged on analysis state first carries out baseline mapping, then analytical instrument is converted to sample introduction state, is led to Crossing the driving of the first low-lift pump (2) makes standard specimen (S2) or sample (S1) be full of injection annulus, then analytical instrument is converted to analysis State carries out the mapping of standard specimen or sample spectrogram.
CN201610393222.3A 2016-06-03 2016-06-03 Have both low pressure ion chromatography and the instrument and application method of low pressure Flow Injection Analysis Expired - Fee Related CN106018637B (en)

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