CN209264621U - A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring - Google Patents
A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring Download PDFInfo
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- CN209264621U CN209264621U CN201821906549.7U CN201821906549U CN209264621U CN 209264621 U CN209264621 U CN 209264621U CN 201821906549 U CN201821906549 U CN 201821906549U CN 209264621 U CN209264621 U CN 209264621U
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Abstract
A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring, including the first miniature peristaltic pump, second miniature peristaltic pump, third miniature peristaltic pump, 4th miniature peristaltic pump, first check valve, second one-way valve, metal tube, high-voltage end electrophoretic buffer liquid storage bottle, waste liquid bottle, two-way normally open solenoid valve, cross four-way buffer fluid reservoir, hybrid reaction coil pipe, capillary, photometry detector, three-way connection, a pole of the high voltage power supply of the external micromation of electrophoresis high voltage interface as electrophoretic separation process, another pole of the metal tube as electrophoretic separation process, anode and cathode relationship is formed between the two poles of the earth, constitute a complete electrophoresis circuit, analyze to metal complex solution in electrophoresis circuit the type and its concentration in the solution of determining heavy metal by photometry detector.The utility model detected value corresponding standard value's deviation is smaller, and detection data accuracy, reliability and stability are preferable, and have it is at low cost, be convenient for carrying, flexibly easy-to-use, highly sensitive advantage.
Description
Technical field
The present invention relates to water sample pollutant monitoring technical fields more particularly to a kind of for water sample heavy metal in-situ monitoring
Capillary electrophoresis.
Background technique
With the continuous quickening of industrialization and urbanization process, what the pollution of heavy metal became in environment water is particularly acute,
The health of people is seriously endangered.Mine, mine are located at remote districts mostly, and the influence to local water environment is not allowed to neglect
Depending on however since remote districts have inconvenient traffic, the great challenge of pollutant monitoring in environment water is realized and regular manually adopted
Sample is all more difficult.Analyte easily causes the loss or pollution of detection target during storing, being transported to laboratory.
Therefore, portable field monitoring instrument is researched and developed, by the great quality for improving field monitoring data, reduces the labor of monitoring personnel
Dynamic burden, while also more timely environmental pollution event can make Emergency decision.More innings of currently used on-site test means
It is limited to using traditional electrochemical sensor, cost is all very high, and is only measured to simple parameters such as conductance, pH value；
Although the electrochemical sensor for having detection content of beary metal comes out, its data reliability and long-time stability are poor, difficult
To meet the requirement of long term monitoring from far-off regions.
Summary of the invention
In view of the deficiencies of the prior art, technical problem solved by the invention is to provide that a kind of cost is low, portability
Good and data monitoring high reliablity water sample monitoring device.
In order to solve the above technical problems, the technical solution adopted by the present invention is that a kind of for water sample heavy metal in-situ monitoring
Capillary electrophoresis, including the first miniature peristaltic pump, the second miniature peristaltic pump, third miniature peristaltic pump, the 4th miniature peristaltic pump,
First check valve, second one-way valve, metal tube, high-voltage end electrophoretic buffer liquid storage bottle, waste liquid bottle, two-way normally open solenoid valve, ten
Word four-way buffer fluid reservoir, hybrid reaction coil pipe, capillary, photometry detector, three-way connection, second minitype creepage
Pump, second one-way valve, three-way connection first interface and second interface, hybrid reaction coil pipe, cross four-way buffer fluid reservoir
First interface and second interface, capillary, photometry detector, high-voltage end electrophoretic buffer liquid storage bottle are sequentially connected and connect, described
First miniature peristaltic pump, the first check valve, the third interface of cross four-way buffer fluid reservoir and the 4th interface four, metal tube,
Two-way normally open solenoid valve, waste liquid bottle, which are sequentially connected, to be connect, the third interface of the three-way connection and the third miniature peristaltic pump phase
Even, the interface of the high-voltage end electrophoretic buffer liquid storage bottle lower part is connect with the 4th miniature peristaltic pump, the high-voltage end electricity
The overflow port that swimming buffer liquid storage bottle is arranged by top is connected with the second waste fluid bag and has electrophoresis high voltage interface, institute on top
It states metal tube to be connected by the ground terminal being equipped with the earth, the overflow port and the first waste fluid bag that the waste liquid bottle is equipped with by top
It is connected, a pole of the high voltage power supply of the external micromation of electrophoresis high voltage interface as electrophoretic separation process, the metal tube is made
For another pole that process is separated by electrophoresis, anode and cathode relationship is formed between the two poles of the earth, a complete electrophoresis circuit is constituted, by described
Photometry detector analyze to metal complex solution in electrophoresis circuit the type and its in the solution of determining heavy metal
Concentration.
The photometry detector includes light emitting diode, photoelectric detector and capillary detection optical interface, the hair
Tubule detection optical interface both ends are separately connected capillary and high-voltage end electrophoretic buffer liquid storage bottle, and the light emitting diode is institute
It states photometry detector and light source is provided, the photoelectric detector is responsible for that real-time data acquisition, analysis and processing work is rapidly completed
Make.
The capillary is the vitreous silica capillary that the internal diameter connecting with cross four-way buffer fluid reservoir is 10-100 μm
Pipe, junction portion outer casing internal diameter are the PEEK casing of 0.4mm；
The hybrid reaction coil pipe is teflon pipe, a length of 30cm, internal diameter 0.5mm；
The high tension voltage of the high voltage interface connection is 3-30kV, by high-pressure mini conversion module by laptop
USB port power supply conversion generates, and the polarity of high tension voltage can be converted by software control；
The high-voltage end electrophoretic buffer liquid storage bottle, waste liquid bottle keep the one of the two liquid level by the overflow port that top is arranged
It causes, guarantees that liquid level differential pressure is not present in electrophoresis circuit and generates dynamical elevation to capillary both ends and then influences to measure
Precision.
First miniature peristaltic pump is used to input supplement and provides the running buffer solution of certain ionic strength, maintains electrophoresis
The conducting of process electric current, buffer solution also maintains the pH value of electrophoresis solution while providing stable ionic strength, to protect
It is constant to hold the migration rate of each component to be measured in the solution, while electrophoretic buffer is also used to rinse cross four-way buffer liquid storage
Indoor remaining mixing sample and reagent；Second miniature peristaltic pump is for inputting complex reaction reagent；The third is miniature
Peristaltic pump is used for input sample solution or standard solution；4th miniature peristaltic pump is for inputting to high-voltage end electrophoretic buffer
The supplement of the electrophoretic buffer for each detection circulation that liquid storage bottle carries out guarantees in order to which system waits next detection circulation
Subsequent analytic process is not influenced.
The working principle of the invention:
Most metal ions are weaker to the absorption of light in water sample, it is difficult to directly be tested with portable optical detection method.
Such as want spectrophotometric determination of gold category ion, it is necessary to react with some complexometric reagents and generate coloring matter, coloring matter can be inhaled
The light for receiving specific wavelength, can be detected with spectrophotometry.But the selectivity of such methods is poor, various metals ion
It can react with this kind of complexometric reagent, the concentration of single metal is difficult to differentiate between by spectrophotometry.
The present invention, which reacts the metal in water sample with complexometric reagent, generates colored complex, after capillary electrophoresis separation,
Spectrophotometry is carried out again, can measure various metals concentration in water sample simultaneously.Select 4- (2- pyridylazo) resorcinol
(PAR) metal ions such as cobalt, nickel, copper, zinc, cadmium, iron or in the complexometric reagents such as 1- (2- pyridylazo)-beta naphthal (PAN) and water
It reacts, generates colored complex.Apply electric field after colored complex is injected quartz capillary, metal complex is in high pressure
Migration rate in electric field is different, therefore the time for reaching photometry detector is different.Pass through what is obtained with metal master solution
Absorbance signal comparison, the time that can use the signal arrival detector under high voltage electric field determine the type of metal, absorbance
The intensity of peak-to-peak signal determines the concentration of metal.
Operating process and technique of the invention, comprising the following steps:
(1) by each means initialization.
(2) start the second miniature peristaltic pump to input complex reaction reagent, the second one-way valve through opening reaches three and connects
Head；Start third miniature peristaltic pump with input sample solution or standard solution arrive three-way connection, sample solution or standard solution and
Complex reaction reagent mixes in three-way connection and reaction enters cross four after generating metal complex in hybrid reaction coil pipe
Logical buffer fluid reservoir.
(3) after complex compound is completely filled with cross four-way buffer fluid reservoir, the power-off of the second miniature peristaltic pump stops working,
The power-off of third miniature peristaltic pump stops working, and complex solution is stood.
(4) third miniature peristaltic pump input sample solution or standard solution are restarted, is applied to the by software supervision
The voltage of three miniature peristaltic pumps, the position of the voltage signal instruction pump rotor of acquisition, to accurately control third minitype creepage
The turnning circle of pump.
(5) it triggers the energization of two-way normally open solenoid valve after two rotation periods to close, third miniature peristaltic pump works on
The pressure injected for sample solution or standard solution is generated, by the indoor sample solution of cross four-way buffer liquid storage or standard
Solution is pressed into capillary.
(6) stop the rotation of third miniature peristaltic pump, complex solution stands waiting in systems.
(7) start the first miniature peristaltic pump to input electrophoretic buffer, through the first check valve to cross four-way running buffer
Liquid fluid reservoir, metal tube are rinsed.
(8) stop the rotation of the first miniature peristaltic pump, complex solution stands waiting in systems.
(9) by high-pressure mini electric power starting, high-pressure mini electricity is applied to high-voltage end electrophoretic buffer by high voltage interface
Within liquid storage bottle, electrophoresis circuit, the electrophoresis point of sample solution or standard solution are established by the ground terminal of capillary and metal tube
Leave the beginning.When sample solution separates, the output of record photometry detector and height under conditions of data acquiring frequency is 20Hz
Voltage source current signal.The voltage signal exported from photometry detector can calculate absorbance A.By absorbance signal A to the time
Mapping, obtains Capillary Electrophoresis spectrogram.On Capillary Electrophoresis spectrogram, each signal peak corresponds to corresponding metal complex.
By contrast standard solution, it is assured that it is which kind of heavy metal according to each signal peak corresponding time (transit time), it is right
Peak height and peak area than sample solution and standard solution determine mass percentage content of the metal ion in water sample.
(10) the first miniature peristaltic pump is opened, two-way normally open solenoid valve is also at channel status, again with electrophoretic buffer
Rinse cross four-way buffer fluid reservoir.
(11) the first miniature peristaltic pump is kept to run well, two-way normally open solenoid valve is powered closure to buffer in cross four-way
Liquid fluid reservoir generates certain pressure.
(12) stop the operating of the first miniature peristaltic pump, two-way normally open solenoid valve continues to remain powered on closure holding pressure, will
Electrophoretic buffer is pressed into capillary in cross four-way buffer fluid reservoir, is rinsed to it.
(13) it opens the 4th miniature peristaltic pump and suitably supplements high-voltage end electrophoretic buffer liquid storage bottle to input electrophoretic buffer,
In order to which system waits next detection circulation.
(14) system returns to initial conditions, is ready for next detection circulation.
It is smaller using detected value corresponding standard value deviation of the present invention, detection data accuracy, reliability and stability compared with
It is good, it is provided simultaneously at low cost, the advantages that being convenient for carrying, is flexibly easy-to-use, highly sensitive.
Detailed description of the invention
Fig. 1 is present system structural schematic diagram；
Fig. 2 is the electrophoresis signal spectrogram of cobalt, copper, zinc ion in present invention separation water sample.
Specific embodiment
A specific embodiment of the invention is further described with reference to the accompanying drawings and examples, but is not to this hair
Bright restriction.
Fig. 1 shows a kind of capillary electrophoresis for water sample heavy metal in-situ monitoring, including the first miniature peristaltic pump
1, the second miniature peristaltic pump 2, third miniature peristaltic pump 3, the 4th miniature peristaltic pump 4, the first check valve 5, second one-way valve 6, gold
Belong to pipe 11, high-voltage end electrophoretic buffer liquid storage bottle 12, waste liquid bottle 13, two-way normally open solenoid valve 14, cross four-way buffer liquid storage
Room 16, hybrid reaction coil pipe 17, capillary 18, photometry detector, three-way connection 25, second miniature peristaltic pump 2,
Two check valves 6,25 first interface of three-way connection and second interface, hybrid reaction coil pipe 17, cross four-way buffer fluid reservoir 16
First interface and second interface, capillary 18, photometry detector, high-voltage end electrophoretic buffer liquid storage bottle 12 be sequentially connected
Connect, first miniature peristaltic pump 1, the first check valve 5, cross four-way buffer fluid reservoir 16 third interface and the 4th interface
Four, metal tube 11, two-way normally open solenoid valve 14, waste liquid bottle 13 are sequentially connected and connect, the third interface of the three-way connection 25 and institute
It states third miniature peristaltic pump 3 to be connected, the interface of 12 lower part of high-voltage end electrophoretic buffer liquid storage bottle and the described 4th miniature compacted
Dynamic 4 connection of pump, the high-voltage end electrophoretic buffer liquid storage bottle 12 are connected simultaneously by the overflow port that top is arranged with the second waste fluid bag 8
There is electrophoresis high voltage interface 22 on top, the metal tube 11 passes through the ground terminal 15 being equipped with and is connected with the earth, the waste liquid bottle
13 overflow ports being equipped with by top are connected with the first waste fluid bag 7, the high-voltage electricity of the external micromation of the electrophoresis high voltage interface 22
A pole of the source as electrophoretic separation process, another pole of the metal tube 11 as electrophoretic separation process form yin between the two poles of the earth
Anode relationship constitutes a complete electrophoresis circuit, molten to metal complex in electrophoresis circuit by the photometry detector
Liquid analyze the type and its concentration in the solution of determining heavy metal.
The photometry detector includes light emitting diode 19, photoelectric detector 20 and capillary detection optical interface 21,
21 both ends of capillary detection optical interface are separately connected capillary 18 and high-voltage end electrophoretic buffer liquid storage bottle 12, the hair
Optical diode 19 provides light source for the photometry detector, and the photoelectric detector 20, which is responsible for real-time data are rapidly completed, to be adopted
Collection, analysis and processing work.
The capillary 18 is the vitreous silica hair that the internal diameter connecting with cross four-way buffer fluid reservoir is 10-100 μm
Tubule, junction portion outer casing internal diameter are the PEEK casing of 0.4mm；
The hybrid reaction coil pipe 17 is teflon pipe, a length of 30cm, internal diameter 0.5mm；
The high tension voltage that the high voltage interface 22 connects is 3-30kV, by high-pressure mini converter by laptop
USB port power supply conversion generates, and the polarity of high tension voltage can be converted by software control；
The high-voltage end electrophoretic buffer liquid storage bottle 12, waste liquid bottle 13 keep the two liquid level by the overflow port that top is arranged
It is consistent, guarantee to be not present liquid level pressure difference in electrophoresis circuit and generate dynamical elevation to capillary both ends and then influence
Measurement accuracy.
First miniature peristaltic pump 1 is used to input supplement and provides the running buffer solution 9 of certain ionic strength, maintains electricity
The conducting of swimming process electric current, buffer solution also maintain the pH value of electrophoresis solution while providing stable ionic strength, thus
Keep the migration rate of each component to be measured in the solution constant, while electrophoretic buffer is also used to rinse the storage of cross four-way buffer
Remaining mixing sample and reagent in liquid chamber；Second miniature peristaltic pump 2 is for inputting complex reaction reagent 23；The third
Miniature peristaltic pump 3 is used for input sample solution or standard solution 24；4th miniature peristaltic pump 4 is for inputting to high-voltage end electricity
The supplement of the electrophoretic buffer for each detection circulation that buffer liquid storage bottle 12 of swimming carries out, in order to which system waits next detection
Circulation, guarantee do not influence subsequent analytic process.
The working principle of the invention:
Most metal ions are weaker to the absorption of light in water sample, it is difficult to directly be tested with portable optical detection method.
Such as want spectrophotometric determination of gold category ion, it is necessary to react with some complexometric reagents and generate coloring matter, coloring matter can be inhaled
The light for receiving specific wavelength, can be detected with spectrophotometry.But the selectivity of such methods is poor, various metals ion
It can react with this kind of complexometric reagent, the concentration of single metal is difficult to differentiate between by spectrophotometry.
The present invention, which reacts the metal in water sample with complexometric reagent, generates colored complex, after capillary electrophoresis separation,
Spectrophotometry is carried out again, can measure various metals concentration in water sample simultaneously.Select 4- (2- pyridylazo) resorcinol
(PAR) metal ions such as cobalt, nickel, copper, zinc, cadmium, iron or in the complexometric reagents such as 1- (2- pyridylazo)-beta naphthal (PAN) and water
It reacts, generates colored complex.Apply electric field after colored complex is injected quartz capillary, metal complex is in high pressure
Migration rate in electric field is different, therefore the time for reaching photometry detector is different.Pass through what is obtained with metal master solution
Absorbance signal comparison, the time that can use the signal arrival detector under high voltage electric field determine the type of metal, absorbance
The intensity of peak-to-peak signal determines the concentration of metal.
Embodiment 1:
Experiment agents useful for same is to analyze the pure or above purity, prepares all solution using ultrapure water.Back-ground electolyte packet
Include Na2B4O7, N- tri- (methylol) methyl-3-aminopropanesulfonicacid acid (TAPS), three (methylol) aminomethanes) and/N- cyclohexyl -2-
Tarine (TRIS/CHES) etc. is adjusted to required pH with 1mol/L NaOH.Respectively by nitrate, chloride or sulfate
The metallic salt of form is dissolved in 0.01mol/L HNO3The stock solution of metal ion, used time are prepared in (trace meter is pure)
It is diluted to required concentration step by step.
System needs configured electrophoretic buffer, complexometric reagent, sample to be tested accessing corresponding pipeline position before use
It sets, and be full of pipeline and waste liquid bottle 13, high-voltage end electrophoretic buffer liquid storage bottle 12 by opening corresponding miniature peristaltic pump.
Capillary 18 successively uses 1mol/L NaOH, 1mol/L HCl and ultrapure water carry out it before being connected to system
Cleaning.By in 18 access system of capillary after the completion of cleaning, then by opening the first miniature peristaltic pump 1, being powered and close two usually
Open electromagnetic valve 14 will clean in electrophoretic buffer ramming system.System readiness after the completion of cleaning can carry out sample survey
Examination.Typical sample test process is as shown in table 1 below.
Table 1
The parameter of the table can be input in the host computer procedure that LABVIEW writes, each step is by host computer procedure
Progressive scan program executes content and is controlled, and is acquired by the operation of each component of computer controlled automatic control system, data
And interpretation of result."ON", which represents, in table is in energization open state；"Off", which represents, is in energization closed state；At "-" expression
In off-position.
Existing 1 pair of the table of comparisons operating process and technique of the invention are specifically described, comprising the following steps:
(1) by each means initialization, the duration about 3 seconds.
(2) the second miniature peristaltic pump 2 of starting inputs complex reaction reagent to input liquid velocity as the speed of 0.2mL/min
23, the second one-way valve 6 opened that is powered reaches three-way connection 25；Starting third miniature peristaltic pump 3 to input liquid velocity is
The speed input sample solution or standard solution 24 of 0.2mL/min arrives three-way connection 25, sample solution or standard solution 24 and network
Reaction reagent 23 is closed to mix in three-way connection 25 and enter ten after reaction generation metal complex in hybrid reaction coil pipe 17
Word four-way buffer fluid reservoir 16, process duration about 40 seconds.
(3) after complex compound is completely filled with cross four-way buffer fluid reservoir 16, the power-off of the second miniature peristaltic pump 2 stops work
Make, 6 power-failure close of second one-way valve, the power-off of third miniature peristaltic pump 3 stops working.Complex solution is stood, time of repose 3
Second.
(4) restarting third miniature peristaltic pump 3 is to input the speed input sample solution that liquid velocity is 50 μ L/min
Or standard solution 24, the voltage of third miniature peristaltic pump 3 is applied to by software supervision, the voltage signal of acquisition indicates pump rotor
Position, thus accurately control third miniature peristaltic pump 3 turnning circle.One rotation period of third miniature peristaltic pump 3
About 3 seconds, 2 circle of the rotation of third miniature peristaltic pump 3, the duration 6 seconds.
(5) at two, triggering two-way normally open solenoid valve 14 is powered and closes after rotation period 6 seconds, third miniature peristaltic pump 3 after
Continuous work generates the pressure injected for sample solution or standard solution, and the sample in cross four-way buffer fluid reservoir 16 is molten
In liquid or standard solution indentation capillary 18, the duration is injected in 10000 milliseconds.
(6) stop third miniature peristaltic pump 3 to rotate, complex solution stands waiting in systems, and time of repose is 3 seconds.
(7) the first miniature peristaltic pump 1 of starting inputs electrophoretic buffer 9 to input liquid velocity as the speed of 0.3mL/min,
Cross four-way electrophoretic buffer fluid reservoir 16, metal tube 11 are rinsed through the first check valve 5, rinsing is 60 seconds.
(8) stop the rotation of the first miniature peristaltic pump 1, complex solution stands waiting in systems, and time of repose is 3 seconds.
(9) by high-pressure mini electric power starting, high-pressure mini electricity is applied to high-voltage end running buffer by high voltage interface 22
Within liquid liquid storage bottle 12, electrophoresis circuit is established by the ground terminal 15 of capillary 18 and metal tube 11, sample solution or standard are molten
The electrophoretic separation of liquid 24 starts, and the electrophoresis duration was up to 40 minutes.It is 20Hz in data acquiring frequency when sample solution separates
Under conditions of record photometry detector output and high voltage power supply current signal.The voltage signal exported from photometry detector can
Calculate absorbance A.Absorbance signal A is plotted against time, Capillary Electrophoresis spectrogram is obtained.On Capillary Electrophoresis spectrogram, often
A signal peak all corresponds to corresponding metal complex.By contrast standard solution, according to (the migration of each signal peak corresponding time
Time) it is assured that be which kind of heavy metal, the peak height and peak area of contrast sample solution and standard solution determine metal ion
Mass percentage content in water sample.
(10) the first miniature peristaltic pump 1 is opened, two-way normally open solenoid valve 14 is also at channel status, with electrophoretic buffer 9
Cross four-way buffer fluid reservoir 16 is rinsed again, and washing time is 10 seconds.
(11) the first miniature peristaltic pump 1 is kept to run well, two-way normally open solenoid valve 14 is powered closure in cross four-way
Buffer fluid reservoir 16 generates certain pressure, holds time 8 seconds.
(12) stop the operating of the first miniature peristaltic pump 1, two-way normally open solenoid valve 14, which continues to remain powered on closure 60 seconds, to be kept
Electrophoretic buffer in cross four-way buffer fluid reservoir 16 is pressed into capillary 18, is rinsed to it by pressure.
(13) the 4th miniature peristaltic pump 4 is opened to input liquid velocity as the speed of 0.3mL/min and input electrophoretic buffer
10 appropriate supplement high-voltage end electrophoretic buffer liquid storage bottles 12, in order to which system waits next detection circulation, the 4th minitype creepage
Pump is kept for rotation time 2 seconds.
(14) system returns to initial conditions, the used time about 1 second, is ready for next detection circulation.
Embodiment 2:
Continuous operation investigates stability of the invention in laboratory, while to Co (II), Cu (II) and Zn (II) metal
The detection of Ar ion mixing standard solution, the electrophoresis signal spectrogram for separating cobalt, copper, zinc ion in water sample of detection is as shown in Fig. 2, wherein
Heavy metal concentration is all 80 μm of ol/L, and abscissa is the time of electrophoresis, and ordinate is signal strength.The corresponding gold of each signal peak
Belong to as For the illustrated example, signal peak heights and sample concentration are positively correlated.
The main performance index of detection is as shown in table 2 below:
2 Main Analysis performance indicator of table
Continuous operation was more than 3 months in the lab by the present invention, wherein carrying out continuous 945 to Cu (II) and Zn (II) ion
Secondary detection, 2 kinds of Ion transfer time RSD are respectively 1.6% and 1.7%, and the RSD of peak height is respectively 5.4% and 4.5%.It proves
Stability of the invention is good.
Embodiment 3:
The content of Zn (II) in the river of on-site measurement somewhere has in this area river a large amount of mine wastewaters to inject, wherein
Institute's metal ion may cause to seriously affect to local resident and ecological environment.Using the inductively coupled plasma of the prior art
Constitution spectrometer (ICP-MS) is used for contrast verification.Measurement result of the present invention see the table below 3:
3 water sample on-site test of table and substrate mark-on result
Measurement result shows the rate of recovery of substrate mark-on at the scene of the invention between 90~113%, and the present invention measures
As a result reach consistent with the icp ms of the prior art (ICP-MS) acceptable level.Demonstrate this hair
The bright feasibility to heavy metal field monitoring in water sample.Cost of the present invention is about 6000 yuans, far below other on the market
Capillary electrophoresis price (mostly in terms of hundreds of thousands of members), good portability (length, width and height: 21cm*10cm*7cm) can be by micro-
Type high-voltage converter is converted is powered by the USB port of laptop, convenient and practical.
In conclusion detection data deviation of the present invention is smaller, accuracy, reliability and stability are preferable, are provided simultaneously with
It is at low cost, be convenient for carrying, flexibly it is easy-to-use, highly sensitive the advantages that.
Detailed description is made that embodiments of the present invention in conjunction with attached drawing above, but the present invention be not limited to it is described
Embodiment.To those skilled in the art, without departing from the principles and spirit of the present invention, to these implementations
Mode carries out various change, modification, replacement and variant are still fallen in protection scope of the present invention.
Claims (7)
1. a kind of capillary electrophoresis for water sample heavy metal in-situ monitoring, which is characterized in that including the first miniature peristaltic pump
(1), the second miniature peristaltic pump (2), third miniature peristaltic pump (3), the 4th miniature peristaltic pump (4), the first check valve (5), second
Check valve (6), metal tube (11), high-voltage end electrophoretic buffer liquid storage bottle (12), waste liquid bottle (13), two-way normally open solenoid valve
(14), cross four-way buffer fluid reservoir (16), hybrid reaction coil pipe (17), capillary (18), photometry detector, three connect
Head (25), second miniature peristaltic pump (2), second one-way valve (6), three-way connection (25) first interface and second interface are mixed
Close the first interface and second interface, capillary (18), photometry of reaction coil pipe (17), cross four-way buffer fluid reservoir (16)
Detector, high-voltage end electrophoretic buffer liquid storage bottle (12) are sequentially connected and connect, first miniature peristaltic pump (1), the first check valve
(5), the third interface of cross four-way buffer fluid reservoir (16) and the 4th interface four, metal tube (11), two-way normally open solenoid valve
(14), waste liquid bottle (13), which is sequentially connected, connects, the third interface of the three-way connection (25) and third miniature peristaltic pump (3) phase
Even, the interface of high-voltage end electrophoretic buffer liquid storage bottle (12) lower part is connect with the 4th miniature peristaltic pump (4), the height
The overflow port that pressure side electrophoretic buffer liquid storage bottle (12) is arranged by top is connected with the second waste fluid bag (8) and has electricity on top
It swims high voltage interface (22), the metal tube (11) passes through the ground terminal (15) being equipped with and is connected with the earth, and the waste liquid bottle (13) is logical
It crosses the overflow port that top is equipped with to be connected with the first waste fluid bag (7), the high-voltage electricity of the external micromation of the electrophoresis high voltage interface (22)
A pole of the source as electrophoretic separation process, another pole of the metal tube (11) as electrophoretic separation process are formed between the two poles of the earth
Anode and cathode relationship constitutes a complete electrophoresis circuit, by the photometry detector to metal complex in electrophoresis circuit
Solution analyze the type and its concentration in the solution of determining heavy metal.
2. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as described in claim 1, which is characterized in that the light
Degree method detector includes light emitting diode (19), photoelectric detector (20) and capillary detection optical interface (21), the capillary
Pipe detection optical interface (21) both ends are separately connected capillary (18) and high-voltage end electrophoretic buffer liquid storage bottle (12), described to shine
Diode (19) provides light source for the photometry detector, and the photoelectric detector (20) is responsible for that real-time data are rapidly completed
Acquisition, analysis and processing work.
3. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as claimed in claim 1 or 2, which is characterized in that institute
Stating capillary (18) is the vitreous silica capillary that the internal diameter connecting with cross four-way buffer fluid reservoir (16) is 10-100 μm
Pipe, junction portion outer casing internal diameter are the PEEK casing of 0.4 mm.
4. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as claimed in claim 1 or 2, which is characterized in that institute
Stating hybrid reaction coil pipe (17) is teflon pipe, a length of 30 cm, 0.5 mm of internal diameter.
5. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as claimed in claim 1 or 2, which is characterized in that institute
The high tension voltage for stating high voltage interface (22) connection is 3-30 kV, can pass through software control reverse.
6. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as claimed in claim 1 or 2, which is characterized in that institute
It states high-voltage end electrophoretic buffer liquid storage bottle (12), waste liquid bottle (13) and keeps the one of the two liquid level by the overflow port that top is arranged
It causes.
7. being used for the capillary electrophoresis of water sample heavy metal in-situ monitoring as claimed in claim 1 or 2, which is characterized in that institute
It states the first miniature peristaltic pump (1) and provides the running buffer solution (9) of certain ionic strength for inputting supplement, described second is miniature
Peristaltic pump (2) is for inputting complex reaction reagent (23)；The third miniature peristaltic pump (3) is used for input sample solution or standard
Solution (24)；4th miniature peristaltic pump (4) is used to input to each of high-voltage end electrophoretic buffer liquid storage bottle (12) progress
Detect the supplement of the electrophoretic buffer of circulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821906549.7U CN209264621U (en) | 2018-11-20 | 2018-11-20 | A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821906549.7U CN209264621U (en) | 2018-11-20 | 2018-11-20 | A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring |
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| Publication Number | Publication Date |
|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109406607A (en) * | 2018-11-20 | 2019-03-01 | 桂林电子科技大学 | A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109406607A (en) * | 2018-11-20 | 2019-03-01 | 桂林电子科技大学 | A kind of capillary electrophoresis for water sample heavy metal in-situ monitoring |
| CN109406607B (en) * | 2018-11-20 | 2023-10-10 | 桂林电子科技大学 | Capillary electrophoresis apparatus for in-situ monitoring of heavy metals in water sample |
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