CN107084981A - The high-precision pH sensors of acid-base indicator photometry are sustained based on nano material - Google Patents
The high-precision pH sensors of acid-base indicator photometry are sustained based on nano material Download PDFInfo
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- CN107084981A CN107084981A CN201710473122.6A CN201710473122A CN107084981A CN 107084981 A CN107084981 A CN 107084981A CN 201710473122 A CN201710473122 A CN 201710473122A CN 107084981 A CN107084981 A CN 107084981A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract
The present invention relates to Environmental Chemistry monitoring technical field, and in particular to a kind of high-precision pH sensors that acid-base indicator photometry is sustained based on nano material, including filter element, constant pressure current stabilization pump, constant temperature sustained release unit, detection unit and waste liquid pool.The high-precision pH sensors that acid-base indicator photometry is sustained based on nano material of the present invention, by setting indicator to be sustained post in the sensor, replacing the fluid filling pump of sensor in the prior art and indicator storage device, it is to avoid frequent replacing storing reagent, cumbersome property is reduced.The pH sensors of the present invention, accuracy is high, and stability is good, can long working, it is convenient to use.
Description
Technical field
The present invention relates to Environmental Chemistry monitoring technical field, and in particular to one kind is sustained acid-base indicator based on nano material
The high-precision pH sensors of photometry.
Background technology
Nearest Ocean acidification increasingly paid attention to by oceanographer, carbonate eqrilibrium in seawater pH reacting conditions ocean
The change of system, directly affects marine ecology diversity.Current oceanographic survey generally uses Electrode potential logging to determine pH, should
Method is based on Nernst equation design, by determining the potential difference between indicator electrode and reference electrode under the conditions of zero current
To carry out analysis measure.This method is ripe, easy to operate, and equipment is simple, cheap, but because drift electrode causes this method
It is difficult to accurate measurements pH fine change, and needs frequently to be calibrated using standard buffer solution to ensure the accurate of measurement
Property.Dickson assess this method accuracy think its in laboratory conditions precision be difficult to more than 0.01pH, home position sensing
Even more there was only ± 0.1pH.Then, Tapp, Yao et al. are proposed according to acid-base indicator in succession is issued to solution in condition of different pH
The indicator molecules of different molecular form have absorption maximum in specific wavelength during from balance, by calculating pH and absorbance relation
On-line measurement pH theory is realized, and is proposed with phenol red as indicator, detection comes pair in 439nm and 577nm absorbance changes
PH is accurately measured.This method has the reachable ± 0.001pH of accuracy of detection height, it is not necessary to the advantage of frequent calibration, but makees
For sensor using need that fluid filling pump and indicator storage device is separately configured, it is necessary to often change reagent bag, it is cumbersome.
The content of the invention
It is an object of the invention to provide a kind of high-precision pH biographies that acid-base indicator photometry is sustained based on nano material
Sensor, the pH sensors accuracy is high, and stability is good, convenient and swift, simple to operate, can long working, it is not necessary to individually match somebody with somebody
Put fluid filling pump and indicator storage device, it is not necessary to often change reagent bag.
To achieve these goals, the present invention is adopted the following technical scheme that：One kind is indicated based on nano material sustained release soda acid
The high-precision pH sensors of agent photometry, including filter element, constant pressure current stabilization pump, constant temperature sustained release unit, detection unit and waste liquid
Pond；
It is provided with the constant temperature sustained release unit in path I, path II, heating module and temperature controller module, the path I
It is connected with indicator sustained release post, the path II and is provided with conductivity sensor, the heating module is arranged on the path I
With the underface of the path II, the temperature controller module is electrically connected with the heating module；
Indicator sustained release post include in shell, the shell filled with can Absorption quantity desorption indicator absorption fill out
Indicator is adsorbed with material, adsorption stuffing；
Flow cell I is provided with the detection unit and flow cell II, the flow cell I and the flow cell II are used
Z-type flow cell, the flow cell I and the flow cell II side are provided with light source, and opposite side is provided with photoelectric receiving system,
The optical fiber of the light source and the photoelectric receiving system respectively with Z-type flow cell both sides is connected；
The outlet of the filter element is connected with the inlet of the constant pressure current stabilization pump, and the constant pressure current stabilization pumps out liquid
Mouth is connected with the path I and the path II respectively by knockout, and the path I is connected with the flow cell I, institute
State path II with the flow cell II to be connected, the flow cell I and the flow cell II are connected with the waste liquid pool respectively；
Data acquisition process unit, the temperature controller module, the conductivity sensors are additionally provided with the detection unit
Device is electrically connected with the data acquisition process unit respectively, and the photoelectric receiving system is adopted by photomultiplier with the data
Collect processing unit electrical connection.
Preferably, the adsorption stuffing is bentonite, attapulgite, nano silicon, organosilicon, nano titanium oxide
It is material modified with macroporous absorbent resin and above-mentioned material.
Preferably, the indicator is phenol phthalein indicator, riodoxol phthalein indicator or azo indicator.
Further, the sampling unit is disposed with three layer filtration layer from injection port to outlet, is followed successively by 80 mesh
At stainless steel mesh, 200 mesh stainless steel mesh and 0.45 μm of glass fibre or polyether sulfone filter core, the injection port of the sampling unit
It is provided with magnetic valve.
Preferably, the heating module is the electrothermal module that appearance covers lead.
Preferably, the light source is xenon lamp or LED.
Preferably, the photoelectric receiving system uses CCD linear imaging sensors, model ILX511.
Preferably, the temperature controller module uses STM93 Series Microprocessor Temperature Controller modules.
Preferably, the conductivity sensor uses UniCond2 electrode conductivity sensors.
Preferably, the constant pressure current stabilization pump uses small size constant flow pump or peristaltic pump.
The high-precision pH sensors that acid-base indicator photometry is sustained based on nano material of the present invention, by sensor
Middle setting indicator is sustained post, replacing the fluid filling pump of sensor in the prior art and indicator storage device, it is to avoid often
Storing reagent is changed, cumbersome property is reduced.The pH sensors of the present invention, accuracy is high, and stability is good, can long working,
It is convenient to use.
Brief description of the drawings
Fig. 1 is the structure composition schematic diagram of sensor of the invention；
Fig. 2 is the structural representation of Z-type flow cell；
In figure：1- filter elements；2- constant pressure current stabilization pumps；3- constant temperature is sustained unit；31- paths I；32- paths II；33- refers to
Show that agent is sustained post；34- heating modules；4- detection units；41- light sources；42- flow cells II；43- flow cells I；44- opto-electronic receivers
System；5- waste liquid pools.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.
Embodiment 1
The operation principle of the pH sensors of the present invention：Two grades of dissociation processes based on acid-base indicator are flat according to its dissociation
Weighing apparatus constant and Lambert-Beer laws calculate pH value.Accounting equation is as follows：
HI- (aq)=H+ (aq)+I2- (aq)
Wherein HI-, I2-For indicator under condition of different pH ionic strength, pK be indicator dissociation constant, AλTo indicate
Agent is in the absorbance of wavelength X, and l is detector optical path length, ελ(HI-)For molar absorption coefficient.Since it is known the dissociation of material is put down
The constant that weighs is fixed value under constant temperature and pressure state, it is only necessary to which its pH can accurately be calculated by measuring seawater sample absorbance.Due to
Optical detection reactions are sensitive, and accuracy in detection can reach ± 0.005.Seawater constitutes relative constancy, and average pH is phenol red 8.1,
Thymol blue, the indicator such as cresol red can be used as seawater pH spectroscopic assay indicator.
Because nano-grain particle diameter is small, the volume fraction that surface atom is accounted for is big, and specific surface area is big, can produce quite big
Surface energy.Because surface atom number increases, Atomic coordinate number is not enough, causes these surfaces highly active, is particularly easy to
Other atoms are adsorbed, there is very big adsorption capacity, in the mobile phase of fixed flow rate, elution speed is constant.Therefore it is suitable to select
Packing material as indicator sorbing material, be fixed in sample path, be excused from an examination agent bag with realizing, reagent pump photometry is determined
pH.Artificial synthesized functionalized nano earth silicon material is utilized in the present embodiment, is made to phenol red, the soda acid such as thymol blue refers to
Show that agent has the carrier of maximum adsorption, be fixed in chromoscope, when sample flows through chromoscope with constant flow rate, by quantitative indicator
Chromogenic reaction occurs for elution, it is to avoid use baseline drift of the indicator bag caused by flow velocity is fluctuated.
As shown in figure 1, the high-precision pH sensors that acid-base indicator photometry is sustained based on nano material of the present invention, bag
Include filter element 1, constant pressure current stabilization pump 2, constant temperature sustained release unit 3, detection unit 4 and waste liquid pool 5.
It is provided with path I31, path II32, heating module 34 and temperature control module, path I31 and connects in constant temperature sustained release pond 3
It is connected in indicator sustained release post 33, path II32 and is provided with conductivity sensor, heating module 34 is arranged on path I31 and path
II32 underface, temperature control module is electrically connected with heating module 34.
Flow cell I43 and flow cell II42 are provided with detection unit 4, flow cell I43 and flow cell II42 are high-purity stone
The Z-type flow cell that English material is made, the structure of Z-type flow cell is as shown in Fig. 2 it is liquid outlet, C that A and B mono-, which are inlet one,
It is optic fibre light path respectively with D；Flow cell I43 and flow cell II42 side are provided with light source 41, and opposite side is provided with photoelectricity and connect
Receipts system 44, from light source 41 towards the direction of photoelectric receiving system 44 on, light source 41 and photoelectric receiving system 44 respectively with Z-type
The optical fiber connection of flow cell both sides, i.e., be respectively connected with C and D.
The outlet of filter element 1 is connected with the inlet of constant pressure current stabilization pump 2, and the liquid outlet of constant pressure current stabilization pump 2 passes through one
Individual threeway is connected with path I31 and path II32 respectively, and path I31 is connected with flow cell I43, path II32 and flow cell
II42 is connected, and flow cell I43 and flow cell II42 are connected with waste liquid pool 5 respectively.
Be additionally provided with data acquisition process unit 45 in detection unit 4, temperature control module, conductivity sensor respectively with data
Acquisition process unit 45 is electrically connected, and photoelectric receiving system 44 is electrically connected by photomultiplier with data acquisition process unit 45.
Wherein, magnetic valve is provided with the injection port of sampling unit, sampling unit is set gradually from injection port to outlet
There is three layer filtration layer, 80 mesh stainless steel mesh, 200 mesh stainless steel mesh and 0.45 μm of glass fibre filter core are followed successively by, wherein 80
Mesh stainless steel mesh be used for prevent suck bulky grain sandstone, 200 mesh stainless steel mesh to remove larger particles in water body,
Particulate matter in 0.45 μm of integrated filter element filtering sea, the design can effectively be reduced and pressed before post, be reduced to sampling pump power requirement,
Enough protections can be provided for indicator sustained release post again, eliminate particulate matter in water body and scatter to spectrometric interference.
The outlet of filter element 1 is connected with the inlet of constant pressure current stabilization pump 2, and constant pressure current stabilization pump 2 is permanent using small size
Pump or peristaltic pump are flowed, flow rate pump control carries out uninterrupted sample collection in 3-10ml/min to seawater sample.Constant pressure current stabilization pump 2
Liquid outlet is connected with path I31 and path II32 respectively by a threeway, and sample is divided into two paths in equal volume, is entered
Constant-temperature sample pool 3.Conductivity sensor is provided with wherein path II32, path II32 is by sample after conductivity sensor
Flow cell II42 is delivered directly to, there is provided sample background value correction parameter as blank.UniCond2 electricity is set in path I31
Electrode conductance rate sensor, the model sensor is the conductance cell containing two pieces of parallel electrode plates, applies sinusoidal at battery lead plate two ends
Wave voltage, the electrical conductivity of water sample is measured according to Ohm's law, while water body passes through conductance cell, is measured at such a temperature
Conductivity values, are output to data processing unit, are calculated for pH meter and provide correction constant.
Indicator sustained release post 33 is connected with path I31, indicator sustained release post 33 includes stainless steel casing, the stainless steel
Enclosure is filled with surface-functionalized nano-silicon dioxide particle sorbing material, the sorbing material and is adsorbed with instruction
Agent, in the present embodiment, indicator are phenol phthalein indicator, specially phenol red, certainly in a further embodiment, can also be selected
Select the thymol blue either phenol such as cresol red phthalein indicator or selection riodoxol phthalein indicator or azo indicator.
Sample provides power by pressure-stabilizing constant flow pump in path II32, anti-by filling the stainless steel of absorption carrier of developer
Filling adsorption material can carry out Large Copacity absorption to acid-base indicator in Ying Zhu, reaction column, and can be quantitative by quantitative elution
Ground elutes indicator, while different according to the acid-base value of water sample, acid-state or alkali state, indicator is presented in indicator in aqueous
Because of the different absorption values for producing varying strength at a particular wavelength of existing forms, blank, electrical conductivity, temperature are deducted according to absorption value
Correction parameter.
Indicator is sustained post 33, and its fills thing is surface-functionalized nano-silicon dioxide particle, the system of the filler
Preparation Method is as follows：With butyl silicate, ammoniacal liquor, rapidly stirring (2800r/min) is mixed to prepare and received in ice-water bath for water and ethanol
Rice silica suspension, it is then that suspension is standby to neutrality freeze-drying with ultrafiltration Membrane cleaning.Appropriate silica is taken again
Nano-particle is put into immersion treatment in dilute nitric acid solution, realize surface hydroxyl activate, wash to neutrality, take appropriate activated species with
Stirring reaction under toluene, vinyltrimethoxy silane mixing, certain rotating speed (800r/min), then with toluene, methanol successively
Fully washing, removes unreacted reactant, dries, under nitrogen protective condition by vinylation material and stearylmercaptan-mercapto-propanediol,
Azodiisobutyronitrile, toluene are mixed in appropriate proportions, stirring reaction under certain temperature, after being washed successively with toluene, methanol, water,
The material that low-temperature vacuum drying obtains required surface hydrophilic, hydrophobic grouping interlocks.
In the present embodiment, adsorption stuffing select surface-functionalized nano-silicon dioxide particle, by processing make its into
The material interlocked for surface hydrophilic, hydrophobic grouping.Certainly in a further embodiment, adsorption stuffing can also be surface-functionalized
Bentonite, attapulgite, nano silicon, organosilicon, nano titanium oxide and macroporous absorbent resin and above-mentioned material
Material modified, the surface-functionalized process of different adsorption stuffings may be different, as long as but by processing, making specific material
Material can turn into the required adsorption stuffing of the present invention as the material that surface hydrophilic, hydrophobic grouping interlock, it is known that specific material
Species, those skilled in the relevant art know how the material for being processed into surface hydrophilic, hydrophobic grouping interlocks.
Heating module 34 and temperature control module are additionally provided with constant-temperature sample pool 3, heating module 34 is arranged on path I31 and logical
Road II32 underface, temperature control module is electrically connected with heating module 34.Temperature control module is sensitive using the serial temperature control modules of STM93
Degree is at ± 0.2 DEG C, and heating module 34 is the electrothermal module that lead is covered comprising appearance, and the heating of heating module 34 is controlled by temperature control module
Temperature.Because ocean temperature is relatively low, temperature is consistently higher than water temperature in constant-temperature sample pool 3, can be according to actual conditions
Suitable temperature value is set higher than 3-5 DEG C of water body, can either ensure that temperature is constant in test process, energy consumption can be reduced again so that
Reference water sample maintains constant mutually synthermal with the water sample to be measured by reaction column, it is to avoid temperature change is done to absorbance
Disturb.
Detection unit 4 is made up of light source 41, flow cell I43, flow cell II42, photoelectric conversion module and data acquisition, its
Middle photoelectric conversion module receives system 44 and photomultiplier including photoelectricity, and photoelectric receiving system is sensed using CCD linear images
Device, model ILX511, the electro-optical system of the species can handle multipath light signal simultaneously.In detection unit 4, correspondence circulation
Pond I43 and flow cell II42, light source 41 provides two parallel light-pathes, corresponding with water route.Wherein, light source 41 is with high-energy
Xenon lamp or LED are as light source, and wherein xenon source can provide higher sensitivity, LED/light source as a kind of new type light source,
With low, the advantage of long lifespan of generating heat, thus can be specifically chosen according to actual conditions；Flow cell is according to detection sensitivity and is passing
Shared volume considers in sensor, and according to the optional 1-10cm of sample pH value excursion flow cell；
Photoelectricity receives system and photomultiplier is used for collecting the optical signal of different paths, and it is converted into telecommunications in time
Number, data processing unit is transported to, blank is deducted, and carry out calculating accurate pH value after thermohaline correction.
Embodiment 2
In embodiment 1, the sensor is primarily used to the sensor of PH detections, and in the present embodiment, indicator is delayed
Release the indicator that post adsorbed and be changed to phthalic acid, while changing Detection wavelength, you can realize the detection to amino acid.
Embodiment 3
In embodiment 1, the sensor is primarily used to the sensor of PH detections, and in the present embodiment, indicator is delayed
Release the indicator that post adsorbed and be changed to benzocaine, while changing Detection wavelength, you can realize the detection to sugar.
It should be appreciated that described above is only the preferred embodiment of the present invention, those of ordinary skill in the art are come
Say, can according to the above description be improved or converted, and all these modifications and variations should all belong to right appended by the present invention
It is required that protection domain.
Claims (10)
1. a kind of high-precision pH sensors that acid-base indicator photometry is sustained based on nano material, it is characterised in that including mistake
Filter unit (1), constant pressure current stabilization pump (2), constant temperature sustained release unit (3), detection unit (4) and waste liquid pool (5)；
Path I (31), path II (32), heating module (34) and temperature controller module are provided with the constant temperature sustained release unit (3),
It is connected with the path I (31) in indicator sustained release post (33), the path II (32) and is provided with conductivity sensor, it is described
Heating module (34) is arranged on the path I (31) and the path II (32) underface, the temperature controller module with it is described
Heating module (34) is electrically connected；
The indicator, which is sustained post, includes shell, and interior be filled with of the shell can Absorption quantity desorption indicator adsorption stuffing, suction
Indicator is adsorbed with attached filler；
Flow cell I (43) and flow cell II (42), the flow cell I (43) and the stream are provided with the detection unit (4)
Logical pond II (42) uses Z-type flow cell, and the flow cell I (43) and the flow cell II (42) side are provided with light source
(41), opposite side is provided with photoelectric receiving system (44), the light source (41) and the photoelectric receiving system (44) respectively with Z
The optical fiber connection of type flow cell both sides；
The outlet of the filter element (1) is connected with the inlet of the constant pressure current stabilization pump (2), the constant pressure current stabilization pump
(2) liquid outlet is connected with the path I (31) and the path II (32) respectively by knockout, the path I (31) and
The flow cell I (43) is connected, and the path II (32) is connected with the flow cell II (42), the flow cell I (43)
It is connected respectively with the waste liquid pool (5) with the flow cell II (42)；
Data acquisition process unit (45) is additionally provided with the detection unit (4), the temperature controller module, the electrical conductivity are passed
Sensor is electrically connected with the data acquisition process unit (45) respectively, the photoelectric receiving system (44) by photomultiplier with
Data acquisition process unit (45) electrical connection.
2. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The adsorption stuffing is bentonite, attapulgite, nano silicon, organosilicon, nano titanium oxide and macropore
Polymeric adsorbent and above-mentioned material it is material modified.
3. the high-precision pH sensors according to claim 1 or 2 that acid-base indicator photometry is sustained based on nano material,
It is characterized in that：The indicator is phenol phthalein indicator, riodoxol phthalein indicator or azo indicator.
4. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The sampling unit is disposed with three layer filtration layer from injection port to outlet, is followed successively by 80 mesh stainless steels sieve
Electricity is provided with net, 200 mesh stainless steel mesh and 0.45 μm of glass fibre or polyether sulfone filter core, the injection port of the sampling unit
Magnet valve.
5. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The heating module (34) is the electrothermal module that appearance covers lead.
6. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The light source (41) is xenon lamp or LED.
7. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The photoelectric receiving system (44) uses CCD linear imaging sensors, model ILX511.
8. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The temperature controller module uses STM93 Series Microprocessor Temperature Controller modules.
9. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The conductivity sensor uses UniCond2 electrode conductivity sensors.
10. the high-precision pH sensors according to claim 1 that acid-base indicator photometry is sustained based on nano material, its
It is characterised by：The constant pressure current stabilization pump (2) uses small size constant flow pump or peristaltic pump.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872214A (en) * | 2018-05-04 | 2018-11-23 | 大连理工大学 | Part CO is measured using absorbance2The experimental system visualizing and method of concentration of ordinary dissolution |
| CN110361381A (en) * | 2019-08-23 | 2019-10-22 | 江西师范大学 | A kind of color sensation acid base detemination device and method based on molecular screen membrane |
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