CN107084981B - High-precision pH sensor based on nanomaterial sustained-release acid-base indicator photometry - Google Patents
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Abstract
The invention relates to the technical field of environmental chemistry monitoring, in particular to a high-precision pH sensor based on a nanomaterial sustained-release acid-base indicator photometry, which comprises a filtering unit, a constant-pressure steady-flow pump, a constant-temperature sustained-release unit, a detection unit and a waste liquid pool. According to the high-precision pH sensor based on the nanomaterial sustained-release acid-base indicator photometry, the indicator sustained-release column is arranged in the sensor to replace a liquid adding pump and an indicator storage device of the sensor in the prior art, so that the frequent replacement of a storage reagent is avoided, and the operation complexity is reduced. The pH sensor has high accuracy, good stability, long-time operation and convenient and quick use.
Description
Technical Field
The invention relates to the technical field of environmental chemistry monitoring, in particular to a high-precision pH sensor based on a nanomaterial sustained-release acid-base indicator photometry.
Background
Recently, ocean acidification is more and more paid attention to by oceanographic students, and the change of the pH of the seawater reflects the change of a carbonate balance system in the ocean, so that the ocean ecological diversity is directly influenced. Currently, the electrode potential method is widely used for measuring pH, and the method is designed based on the Nernst equation, and is used for analysis and measurement by measuring the potential difference between an indicating electrode and a reference electrode under the condition of zero current. The method is mature, simple and convenient to operate, simple in equipment and low in cost, but the method is difficult to accurately monitor the fine change of the pH value due to electrode drift, and the calibration is carried out by frequently using standard buffer solution so as to ensure the accuracy of measurement. The accuracy of the Dickson evaluation method recognizes that the accuracy of the method is difficult to exceed 0.01pH under laboratory conditions, and the in-situ sensor is only +/-0.1 pH. Subsequently, tapp, yao et al sequentially proposed the concept of on-line measurement of pH by calculating the relationship between pH and absorbance based on the maximum absorption at a specific wavelength of indicator molecules of different molecular morphologies when the acid-base indicator reached dissociation equilibrium at different pH conditions, and proposed the use of phenol red as an indicator to detect absorbance changes at 439nm and 577nm for accurate measurement of pH. The method has the advantages that the detection precision is high up to +/-0.001 pH, frequent calibration is not needed, but the sensor is used as a sensor, a liquid adding pump and an indicator storage device are required to be independently configured, a reagent pack is required to be frequently replaced, and the operation is complex.
Disclosure of Invention
The invention aims to provide a high-precision pH sensor based on a nanomaterial sustained-release acid-base indicator photometry, which has the advantages of high precision, good stability, convenience, quickness, simple operation, long-time operation, no need of independently configuring a liquid adding pump and an indicator storage device and no need of frequently replacing a reagent pack.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a high-precision pH sensor based on a nanomaterial sustained-release acid-base indicator photometry comprises a filtering unit, a constant-pressure steady-flow pump, a constant-temperature sustained-release unit, a detection unit and a waste liquid pool;
a passage I, a passage II, a heating module and a temperature controller module are arranged in the constant-temperature slow-release unit, an indicator slow-release column is connected in the passage I, a conductivity sensor is arranged in the passage II, the heating module is arranged right below the passage I and the passage II, and the temperature controller module is electrically connected with the heating module;
the indicator slow-release column comprises a shell, wherein the shell is filled with an adsorption filler capable of quantitatively adsorbing and desorbing an indicator, and the adsorption filler is adsorbed with the indicator;
the detection unit is internally provided with a flow cell I and a flow cell II, the flow cell I and the flow cell II are Z-shaped flow cells, one sides of the flow cell I and the flow cell II are provided with light sources, the other sides of the flow cell I and the flow cell II are provided with photoelectric receiving systems, and the light sources and the photoelectric receiving systems are respectively connected with optical fibers at two sides of the Z-shaped flow cells;
the sample outlet of the filtering unit is communicated with the liquid inlet of the constant-pressure steady flow pump, the liquid outlet of the constant-pressure steady flow pump is respectively communicated with the passage I and the passage II through a liquid separator, the passage I is communicated with the flow cell I, the passage II is communicated with the flow cell II, and the flow cell I and the flow cell II are respectively communicated with the waste liquid tank;
the detection unit is internally provided with a data acquisition and processing unit, the temperature controller module and the conductivity sensor are respectively and electrically connected with the data acquisition and processing unit, and the photoelectric receiving system is electrically connected with the data acquisition and processing unit through a photomultiplier.
Preferably, the adsorption filler is bentonite, attapulgite, nano silicon dioxide, organic silicon, nano titanium dioxide and macroporous adsorption resin, and modified materials of the materials.
Preferably, the indicator is a phenolphthalein type indicator, a sulfophenolphthalein type indicator or an azo type indicator.
Further, the sampling unit is provided with three layers of filter layers from the sample inlet to the sample outlet in sequence, wherein the filter layers are an 80-mesh stainless steel screen, a 200-mesh stainless steel screen and a 0.45-mu m glass fiber or polyether sulfone filter core in sequence, and an electromagnetic valve is arranged at the sample inlet of the sampling unit.
Preferably, the heating module is an electrothermal module with lead coated on the outer surface.
Preferably, the light source is a xenon lamp or an LED lamp.
Preferably, the photoelectric receiving system adopts a CCD linear image sensor, and the model is ILX511.
Preferably, the temperature controller module adopts STM93 series temperature controller module.
Preferably, the conductivity sensor is a UniCond2 electrode conductivity sensor.
Preferably, the constant-pressure steady-flow pump adopts a small-volume constant-flow pump or a peristaltic pump.
According to the high-precision pH sensor based on the nanomaterial sustained-release acid-base indicator photometry, the indicator sustained-release column is arranged in the sensor to replace a liquid adding pump and an indicator storage device of the sensor in the prior art, so that the frequent replacement of a storage reagent is avoided, and the operation complexity is reduced. The pH sensor has high accuracy, good stability, long-time operation and convenient and quick use.
Drawings
FIG. 1 is a schematic diagram of the structural composition of a sensor of the present invention;
FIG. 2 is a schematic diagram of the structure of a Z-type flow cell;
in the figure: 1-a filtration unit; 2-a constant-pressure steady flow pump; 3-a constant temperature slow release unit; 31-pathway I; 32-pathway II; 33-an indicator slow release column; 34-a heating module; a 4-detection unit; 41-a light source; 42-flow cell II; 43-flow cell I; 44-an optoelectronic receiving system; 5-a waste liquid pool.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The working principle of the pH sensor of the invention is as follows: the pH value is calculated according to the dissociation equilibrium constant and the Lambert-Beer law of the secondary dissociation process based on the acid-base indicator. The calculation equation is as follows:
HI - (aq) ＝H + (aq) +I 2- (aq)
wherein HI is - ，I 2- For the ionic strength of the indicator under different pH conditions, pK is the dissociation constant of the indicator, A λ For the absorbance of the indicator at wavelength lambda, l is the detector path length, ε λ(HI-) Is the molar absorption coefficient. Because the dissociation equilibrium constant of the known substance is a fixed value under the constant temperature and constant pressure state, only the absorption of the seawater sample is needed to be measuredThe pH can be accurately calculated. Due to the sensitivity of the optical detection reaction, the detection accuracy can reach +/-0.005. The seawater composition is relatively constant, the average pH is 8.1, and indicators such as phenol red, thymol blue, cresol red and the like can be used as seawater pH spectrometry indicators.
Due to the small particle size of the nano material particles, the volume fraction of surface atoms is large, the specific surface area is large, and considerable surface energy can be generated. The number of atoms on the surface is increased, and the coordination number of the atoms is insufficient, so that the surfaces have high activity, are particularly easy to adsorb other atoms, have large adsorption capacity, and have constant elution speed in a mobile phase with a fixed flow rate. Therefore, a proper filling material is selected as an indicator adsorption material and is fixed in the sample passage so as to realize reagent-free package and the measurement of pH by a reagent pump photometry. In the embodiment, the artificially synthesized functionalized nano silicon dioxide material is utilized to prepare the carrier with maximum adsorption on the acid-base indicators such as phenol red, thymol blue and the like, the carrier is fixed in the color development tube, and when a sample flows through the color development tube at a constant flow rate, the quantitative indicator is eluted to generate color development reaction, so that baseline drift of the indicator package caused by flow rate fluctuation is avoided.
As shown in figure 1, the high-precision pH sensor based on the nanomaterial sustained-release acid-base indicator photometry comprises a filtering unit 1, a constant-pressure steady-flow pump 2, a constant-temperature sustained-release unit 3, a detection unit 4 and a waste liquid pool 5.
The constant temperature slow release pond 3 is internally provided with a passage I31, a passage II32, a heating module 34 and a temperature control module, the passage I31 is internally connected with an indicator slow release column 33, the passage II32 is internally provided with a conductivity sensor, the heating module 34 is arranged under the passage I31 and the passage II32, and the temperature control module is electrically connected with the heating module 34.
The detection unit 4 is internally provided with a flow cell I43 and a flow cell II42, the flow cell I43 and the flow cell II42 are Z-shaped flow cells made of high-purity quartz materials, the structure of the Z-shaped flow cells is shown in figure 2, one of A and B is a liquid inlet, the other is a liquid outlet, and C and D are optical fiber optical paths respectively; the light source 41 is arranged on one side of the flow cell I43 and one side of the flow cell II42, the photoelectric receiving system 44 is arranged on the other side of the flow cell II, and the light source 41 and the photoelectric receiving system 44 are respectively connected with optical fibers on two sides of the Z-shaped flow cell, namely, are respectively connected with C and D in the direction from the light source 41 to the photoelectric receiving system 44.
The sample outlet of the filtering unit 1 is communicated with the liquid inlet of the constant-pressure steady flow pump 2, the liquid outlet of the constant-pressure steady flow pump 2 is respectively communicated with the passage I31 and the passage II32 through a tee joint, the passage I31 is communicated with the flow cell I43, the passage II32 is communicated with the flow cell II42, and the flow cell I43 and the flow cell II42 are respectively communicated with the waste liquid tank 5.
The detection unit 4 is also internally provided with a data acquisition and processing unit 45, the temperature control module and the conductivity sensor are respectively and electrically connected with the data acquisition and processing unit 45, and the photoelectric receiving system 44 is electrically connected with the data acquisition and processing unit 45 through a photomultiplier.
The sampling unit is provided with three layers of filter layers from the sample inlet to the sample outlet, and the filter layers are an 80-mesh stainless steel screen, a 200-mesh stainless steel screen and a 0.45-mu m glass fiber filter core in sequence, wherein the 80-mesh stainless steel screen is used for preventing large-particle sand and stones from being inhaled, the 200-mesh stainless steel screen is used for removing large particles in water, and the 0.45-mu m integrated filter core is used for filtering particles in seawater.
The sample outlet of the filtering unit 1 is communicated with the liquid inlet of the constant-pressure steady-flow pump 2, the constant-pressure steady-flow pump 2 adopts a small-volume constant-flow pump or a peristaltic pump, and the pump flow rate is controlled to be 3-10ml/min to collect the seawater sample continuously. The liquid outlet of the constant-pressure steady-flow pump 2 is respectively communicated with a passage I31 and a passage II32 through a tee joint, and divides the volume of a sample and the like into two passages and enters the constant-temperature sample pool 3. The conductivity sensor is arranged in the channel II32, and the channel II32 directly conveys the sample to the flow cell II42 after passing through the conductivity sensor, and the sample is used as a blank to provide a sample background value correction parameter. The UniCond2 electrode conductivity sensor is arranged in the passage I31, the sensor is a conductivity cell containing two parallel electrode plates, sine wave voltage is applied to two ends of the electrode plates, the conductivity of a water sample is measured according to ohm law, and when a water body passes through the conductivity cell, the conductivity value at the temperature is measured and is output to the data processing unit, so that a correction constant is provided for pH calculation.
The passage I31 is connected with an indicator slow-release column 33, the indicator slow-release column 33 comprises a stainless steel shell, a nano silica particle adsorption material with a functionalized surface is filled in the stainless steel shell, and an indicator is adsorbed on the adsorption material, in this embodiment, the indicator is a phenolphthalein indicator, specifically phenol red, and in other embodiments, a phenolphthalein indicator such as thymol blue or cresol red, or a sulfophenolphthalein indicator or an azo indicator can be selected.
The sample in the passage II32 is powered by a constant-pressure constant-flow pump, passes through a stainless steel reaction column filled with an adsorption carrier of a color developing agent, and the reaction column is filled with an adsorption material which can carry out high-capacity adsorption on an acid-base indicator, can be quantitatively eluted, and can quantitatively elute the indicator.
The indicator slow release column 33 contains surface functionalized nano silica particles as filler, and the preparation method of the filler is as follows: the nano silicon dioxide suspension is prepared by rapidly stirring (2800 r/min) butyl orthosilicate, ammonia water, water and ethanol in ice water bath, and then the suspension is washed to be neutral by an ultrafiltration membrane and freeze-dried for standby. And then a proper amount of silicon dioxide nano particles are put into dilute nitric acid solution for soaking treatment, so as to realize surface hydroxyl activation, washing is carried out to neutrality, a proper amount of activated particles are mixed with toluene and vinyl trimethoxy silane, stirring reaction is carried out at a certain rotating speed (800 r/min), then toluene and methanol are used for sequentially and fully washing, unreacted substances are removed, drying is carried out, the vinylation material, octadecanethiol-mercaptopropylene glycol, azodiisobutyronitrile and toluene are mixed in a proper proportion under the protection of nitrogen, stirring reaction is carried out at a certain temperature, and after the mixture is washed by toluene, methanol and water in turn, the material with hydrophilic surface and staggered hydrophobic groups is obtained by low-temperature vacuum drying.
In this embodiment, the adsorption filler is surface functionalized nano silica particles, and the surface functionalized nano silica particles are made into a material with hydrophilic and hydrophobic groups staggered by treatment. Of course, in other embodiments, the adsorption filler may be surface functionalized bentonite, attapulgite, nano silica, organosilicon, nano titania, macroporous adsorption resin, and modified materials of the above materials, and the surface functionalization process of different adsorption fillers may be different, but as long as a specific material is made into a material with hydrophilic surface and staggered hydrophobic groups through treatment, the adsorption filler required by the present invention can be made, and the type of the specific material is known, and a person skilled in the relevant art knows how to treat the specific material into a material with hydrophilic surface and staggered hydrophobic groups.
The constant temperature sample cell 3 is also provided with a heating module 34 and a temperature control module, the heating module 34 is arranged under the passage I31 and the passage II32, and the temperature control module is electrically connected with the heating module 34. The temperature control module adopts STM93 series temperature control modules, the sensitivity is +/-0.2 ℃, the heating module 34 is an electric heating module with lead coated on the outer surface, and the temperature control module controls the heating temperature of the heating module 34. The temperature in the constant-temperature sample pool 3 is always higher than the water temperature because the seawater temperature is relatively low, and a proper temperature value can be set to be higher than the water temperature by 3-5 ℃ according to actual conditions, so that the temperature is constant in the test process, the energy consumption can be reduced, the reference water sample and the water sample to be tested passing through the reaction column are maintained at the same constant temperature, and the interference of temperature change on absorbance is avoided.
The detection unit 4 is composed of a light source 41, a flow cell I43, a flow cell II42, a photoelectric conversion module and a data acquisition, wherein the photoelectric conversion module comprises a photoelectric receiving system 44 and a photomultiplier, the photoelectric receiving system adopts a CCD linear image sensor, the model is ILX511, and the photoelectric system of the type can process multipath optical signals simultaneously. In the detection unit 4, the light source 41 provides two parallel light paths corresponding to the waterway corresponding to the flow cell I43 and the flow cell II 42. The light source 41 uses a high-energy xenon lamp or an LED lamp as a light source, wherein the xenon lamp light source can provide higher sensitivity, and the LED light source as a novel light source has the advantages of low heat generation and long service life, so that the xenon lamp light source can be specifically selected according to practical situations; the flow cell is comprehensively considered according to the detection sensitivity and the occupied volume in the sensor, and a 1-10cm flow cell can be selected according to the pH change range of the sample;
the photoelectric receiving system and the photomultiplier are used for collecting optical signals of different paths, converting the optical signals into electric signals in time, transmitting the electric signals to the data processing unit, deducting blank, and calculating accurate pH value after temperature and salt correction.
Example 2
In example 1, the sensor was mainly used as a sensor for PH detection, and in this example, the detection wavelength was changed while changing the indicator adsorbed by the indicator slow-release column to phthalic acid, so that the detection of amino acid was achieved.
Example 3
In example 1, the sensor was mainly used as a sensor for PH detection, and in this example, the detection of sugar was achieved by changing the wavelength of detection while changing the indicator adsorbed by the indicator slow-release column to ethyl aminobenzoate.
It should be understood that the foregoing is only a preferred embodiment of the present invention and that modifications and changes may be made by those skilled in the art in light of the foregoing description, all such modifications and changes being intended to fall within the scope of the present invention as defined by the appended claims.
Claims (9)
1. The high-precision pH sensor based on the nanomaterial sustained-release acid-base indicator photometry is characterized by comprising a filtering unit (1), a constant-pressure steady-flow pump (2), a constant-temperature sustained-release unit (3), a detection unit (4) and a waste liquid pool (5);
a passageway I (31), a passageway II (32), a heating module (34) and a temperature controller module are arranged in the constant-temperature slow-release unit (3), an indicator slow-release column (33) is connected in the passageway I (31), a conductivity sensor is arranged in the passageway II (32), the heating module (34) is arranged right below the passageway I (31) and the passageway II (32), and the temperature controller module is electrically connected with the heating module (34); the indicator slow-release column comprises a shell, wherein the shell is filled with an adsorption filler capable of quantitatively adsorbing and desorbing an indicator, and the adsorption filler is adsorbed with the indicator;
a flow cell I (43) and a flow cell II (42) are arranged in the detection unit (4), the flow cell I (43) and the flow cell II (42) are Z-shaped flow cells, a light source (41) is arranged on one side of the flow cell I (43) and one side of the flow cell II (42), a photoelectric receiving system (44) is arranged on the other side of the flow cell I (43) and one side of the flow cell II (42), and the light source (41) and the photoelectric receiving system (44) are respectively connected with optical fibers on two sides of the Z-shaped flow cell;
the sample outlet of the filtering unit (1) is communicated with the liquid inlet of the constant-pressure steady-flow pump (2), the liquid outlet of the constant-pressure steady-flow pump (2) is respectively communicated with the passage I (31) and the passage II (32) through a liquid separator, the passage I (31) is communicated with the flow cell I (43), the passage II (32) is communicated with the flow cell II (42), and the flow cell I (43) and the flow cell II (42) are respectively communicated with the waste liquid tank (5);
the detection unit (4) is internally provided with a data acquisition processing unit (45), the temperature controller module and the conductivity sensor are respectively and electrically connected with the data acquisition processing unit (45), the photoelectric receiving system (44) is electrically connected with the data acquisition processing unit (45) through a photomultiplier, and the photoelectric receiving system and the photomultiplier are used for collecting optical signals of different paths and converting the optical signals into electric signals in time and transmitting the electric signals to the data processing unit, and the electric signals are deducted and corrected by warm salt to calculate accurate pH values.
2. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the indicator is a phenolphthalein indicator, a sulfophenolphthalein indicator or an azo indicator.
3. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the sampling unit is provided with three layers of filter layers from the sample inlet to the sample outlet in sequence, wherein the filter layers are an 80-mesh stainless steel screen, a 200-mesh stainless steel screen and a 0.45-mu m glass fiber or polyether sulfone filter core in sequence, and an electromagnetic valve is arranged at the sample inlet of the sampling unit.
4. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the heating module (34) is an electrothermal module with lead coated on the outer surface.
5. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the light source (41) is a xenon lamp or an LED lamp.
6. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the photoelectric receiving system (44) adopts a CCD linear image sensor, and the model is ILX511.
7. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the temperature controller module adopts STM93 series temperature controller module.
8. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the conductivity sensor adopts a UniCond2 electrode conductivity sensor.
9. The nanomaterial-based sustained release acid-base indicator photometry high-precision pH sensor of claim 1, characterized in that: the constant-pressure steady-flow pump (2) adopts a small-volume constant-flow pump or a peristaltic pump.
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