CN103822887B - A kind of detection method of laser detection nitrite anions concentration - Google Patents
A kind of detection method of laser detection nitrite anions concentration Download PDFInfo
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- CN103822887B CN103822887B CN201410100551.5A CN201410100551A CN103822887B CN 103822887 B CN103822887 B CN 103822887B CN 201410100551 A CN201410100551 A CN 201410100551A CN 103822887 B CN103822887 B CN 103822887B
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Abstract
The invention discloses a kind of pick-up unit and detection method thereof of laser detection nitrite anions concentration.Pick-up unit of the present invention comprises: light-source system, cuvette, sample cell, silicon photocell and voltage table; Wherein, sample is filled and developer light-source system launches one-wavelength laser in cuvette, through the cuvette be placed in sample cell, received by silicon photocell, convert light signal to electric signal, transfer to voltage table, by the equation of linear regression of the concentration of the variable quantity-nitrite anions of contrast potential, obtain the concentration of sample Nitrite.Pick-up unit of the present invention is anti-to jolt, durable, easy care; Adopt 532nm laser and the silicon photocell of low price, significantly reduce cost; Inner structure is simple, and volume is little and quality light, is convenient for carrying, can the concentration of local measurement environmental water sample Nitrite in the wild, ensure that authenticity and the reliability of test result; Ensure higher measuring accuracy simultaneously.
Description
Technical field
The present invention relates to water quality monitoring technical field, be specifically related to a kind of pick-up unit and detection method thereof of laser detection nitrite anions concentration.
Background technology
Nitrite is intermediate active in nitrogen cycle, incomplete or the reducing nitrate radical of ammoxidation not exclusively can produce nitrite, nitrite is extensively present in many materials as in many materials such as water, soil, vegetables and salted vegetables, is chemical substance biosome being had to serious toxic action.China prohibits the use nitrite in a lot of industry, and nitrite has also become a big event of water quality, environment, food, drugs of abuse.This analyzer all can have wide practical use in environmental protection, environmental surveys, aquaculture, food industry and inspection and quarantine etc.
At present, content of nitrite method for measuring mainly contains UV-spectrophotometry, Catalytic-Kinetic Spectrophotometric, fluorescence spectrophotometry, chemoluminescence method, polarography, the chromatography of ions and ion-selective electrode potentiometry etc.(nitrous nitrification Advances in Methods, Yellow River Conservancy Technical Institute's journal, 2005,17th volume, the 1st phase, 50-52 page) consider from experimental implementation and institute's use instrument, UV-spectrophotometry is more similar with Catalytic-Kinetic Spectrophotometric, is all, after quantitatively adding in test solution to be measured or not adding certain developer, to test the difference of its absorbance and reference solution absorbance under a certain specific wavelength, after contrast standard curve, draw the concentration of solution Nitrite to be measured.Within the scope of UV-visible wavelength, the standard method of domestic and international mensuration nitrite is diazo coupling colourimetry, nitrite and sulfanilic acid generate heavy ammonia salt in acid condition, generate aubergine dyestuff with N-1-naphthyl-ethylenediamine-hydrochloride (or alpha-naphthylamine) coupling again, under a certain specific wavelength, measure absorbance.Catalytic-Kinetic Spectrophotometric, be nitrite catalysis potassium bromate (or potash chlorate) oxidation-reduction quality dyestuff delicately under acid medium, make it to fade, after certain hour is carried out in reaction, by cooling, change the method cessation reactions such as pH, under a certain specific wavelength, measure absorbance.(nitrous nitrification Advances in Methods, Yellow River Conservancy Technical Institute's journal, the 2005,17th volume, the 1st phase, 50-52 page)
The classical Grignard of the utilization that China had reported measures the method for content of nitrite, and its range of linearity mainly concentrates on 0 ~ 5ng/ μ l, and Monitoring lower-cut concentrates on 0.001-0.01ng/ μ l; Although good Monitoring lower-cut can be obtained with catalytic spectrophotometric content of nitrite, generally all need to use water-bath in mensuration process, and the reaction time to control very accurately, not so there will be the phenomenon that repetition rate is lower; Ultraviolet Photometric Method Monitoring lower-cut can reach 0.0069ng/ μ l, has higher sensitivity, but survey data need more complicated mathematics manipulation or need adopt dual wavelength, even Spectrophotometry Method Using Three-wavelength measures, and adds the complexity of measuring and data processing.(interior spectrphotometric method for measuring nitrite progress, spectrographic laboratory, in May, 2010,900-907 page)
At present, national and foreign standards method or additive method measure nitrite in solution content use the price of instrument from thousands of to ten tens thousand of not etc., the instrument that estimating precision is higher, all be not suitable for or onsite application in the wild because of too heavy, sample need be treated meeting experimental determination, but the nitrite in natural water is very unstable, when containing oxygen and under microbial action, oxidable one-tenth nitrate, also ammonia can be reduced under anoxic or oxygen free condition, therefore should analyze as early as possible after sampling, if measure again after sample being taken back laboratory, the content of nitrite anions will change to some extent, cause measurement result inaccurate.But be easy to carry can in the wild or the instrument of field test content of nitrite, its measuring accuracy is not very high.
Summary of the invention
For above problems of the prior art, the invention provides a kind of with low cost, structure simple and be convenient for carrying, can the high-precision measuring device of the concentration of the real time measure environmental water sample Nitrite on the spot in the wild, ensure authenticity and the reliability of test result simultaneously.
One object of the present invention is the pick-up unit providing a kind of laser detection nitrite anions concentration.
The pick-up unit of nitrite anions concentration of the present invention comprises: light-source system, cuvette, sample cell, silicon photocell and voltage table; Wherein, sample and developer is filled in cuvette, the one-wavelength laser that developer and light-source system send is corresponding, and the nitrite anions in developer and sample reacts the aubergine dyestuff generated, linear to the concentration of the absorption of one-wavelength laser and nitrite anions that are incident to cuvette; Light-source system launches one-wavelength laser, through the cuvette be placed in sample cell, received by silicon photocell, convert light signal to electric signal, transfer to voltage table, according to the reading of voltage table, the equation of linear regression of the concentration of logical superpotential variable quantity-nitrite anions, obtains the concentration of sample Nitrite.
Light-source system comprises laser instrument, collimating apparatus, heating radiator and voltage stabilizer; Wherein, laser instrument sends one-wavelength laser, for laser instrument provides stable voltage, ensures the power stability of shoot laser; The surface of laser instrument connects heating radiator, carries out active heat removal to laser instrument; Before collimating apparatus is placed on laser instrument, the one-wavelength laser sent by laser instrument collimates, and becomes directional light, thus ensure that laser vertical is incident to cuvette, can not occur to reflect or total reflection and cause the loss of laser, and be irradiated to the sample in cuvette equably, ensure stability.
The present invention adopts mono-colour laser, filling in the cuvette containing the sample of nitrite anions, the nitrite anions added in developer and sample reacts and generates aubergine dyestuff, when the laser light sample of respective wavelength, absorption of sample laser, thus the intensity of the laser transmitted relatively weakens, the laser intensity that silicon photocell absorbs reduces, this light signal is transformed into electric signal, is measured the electromotive force change of silicon photocell generation by voltage table, thus the change of laser intensity is characterized; Add the concentration of the sample Nitrite of developer, linear with the laser intensity absorbed, thus the electromotive force of the silicon photocell measured with voltage table changes and has good linear relationship, the pick-up unit of the concentration of nitrite anions is detected according to this principle preparation, by the reading of voltage table, the concentration of nitrite anions can be obtained.
Laser is all high artificial light sources of a kind of brightness, collimation, monochromaticity, stability, and the wavelength of its medium green laser is 532nm.Through investigation, green semiconductor laser diode stable supply in China market of 5 ~ 100mW.Silicon photocell luminous energy is worn the semiconductor device changing electric energy into, and when being subject to illumination, silicon photocell converts luminous energy to electric energy, causes the deflection of the pointer of the voltage table of connection.With the development of China's photovoltaic industry, supply high quality silicon photoelectric cell has also been stablized in market, and price is all very low.
The present invention finds through test, and silicon photocell has good response to 532nm laser.
The present invention adopts the mono-colour laser of 532nm, correspondingly, is filling the developer adding respective wavelength in the cuvette containing the sample of nitrite anions, thus absorbs the laser of 532nm, and the concentration of nitrite anions is directly proportional to the intensity of the laser of absorption.The present invention obtains through the also repetition test that studies for a long period of time, and the developer be equipped with by a certain percentage makes nitrite anions present aubergine, and this aubergine is to the absorption of the laser of 532nm, linear with the concentration of nitrite anions.For the sample solution that cumulative volume is certain, relative to cumulative volume ratio, volume ratio 0.1 ~ 0.12 concentration is the citric acid solution of 210.10g/L, volume ratio 0.060 ~ 0.075 concentration is the sulfanilic acid solution of 1.00g/L, after vibration, to add volume ratio be again 0.035 ~ 0.050 concentration is the N-1-naphthyl-ethylenediamine-hydrochloride solution of 0.5g/L, makes nitrite anions present aubergine.Experimental result shows, the concentration of nitrite anions is within the scope of 0 ~ 1.8ng/ μ l, and above-mentioned purplish red solution is good linear relationship to the absorption of the laser of wavelength 532nm and the concentration of nitrite anions.The present invention adopts citric acid, and citric acid is solid-state at normal temperatures, is convenient for carrying, is conducive to taking field to, and to environment without harm.
Further, silicon photocell is connected to voltage table through diode, due to the unilateral conduction of diode, make electric current can only flow to voltage table from silicon photocell, and can not from voltage table reverse direction flow to silicon photocell, thus when preventing the light intensity on silicon photocell from dying down, the reversed flow of electric current.
Further, the present invention includes cabinet, light-source system, cuvette, sample cell, silicon photocell and voltage table are placed in the chassis, is well suited for bringing to scene and measures.
Another object of the present invention is the detection method providing a kind of laser detection nitrite anions concentration.
The detection method of nitrite anions concentration of the present invention, comprises the following steps:
1) according to the solution of the nitrite anions of concentration known, and the reading of corresponding voltage table, set up typical curve and the equation of linear regression of the concentration of the variable quantity-nitrite anions of voltage, obtain parameter a and regression coefficient b;
2) open laser instrument and voltage table, and wait for the stable reading of voltage table, 10 ~ 30 seconds;
3) be positioned in sample cell by the cuvette filling the sample not adding developer, light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
0;
4) developer is added fill in the cuvette of sample, after color stability, cuvette is positioned in sample cell;
5) light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U(U of now voltage table
0>U);
6) according to U
0the value of-U, the equation of linear regression U of the concentration of logical superpotential variable quantity-nitrite anions
0-U=a+bx, obtains the concentration x of sample Nitrite.
Wherein, in step 1), set up typical curve and the regression equation of the concentration of the variable quantity-nitrite anions of voltage, comprise the following steps:
A) solution not containing nitrite anions is injected cuvette, then add quantitative developer, overall solution volume is certain;
B) open laser instrument and voltage table, and wait for the stable reading of voltage table, 10 ~ 30 seconds;
C) be placed in sample cell by cuvette, light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
0;
D) cumulative volume is constant, and in the cuvette filling developer, add concentration is C
initrite anions, after color stability, cuvette is positioned in sample cell;
E) light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
i, 1≤i≤n, n and i is natural number, and n>=2;
F) i gets n successively from 1, repeats step d) ~ e), obtain the variable quantity U of voltage
0-U
iwith the concentration C of nitrite anions
itypical curve, and set up the variable quantity U of voltage
0-U
iwith the concentration C of nitrite anions
iequation of linear regression U
0-U
i=a+bC
i, obtain parameter a and regression coefficient b.
Advantage of the present invention:
The present invention adopts the one-wavelength laser of 532nm, utilizes silicon photocell linear with the absorption of nitrite anions solution to 532nm laser of the developer adding special ratios, is obtained the concentration of nitrite anions by the variable quantity of the reading of voltage table; Due to need not the beam splitting system such as prism, grating, signal collection, amplification system etc. that need not be complicated be complicated, exquisite system exists, and the anti-bumpiness of device, durability, ease for maintenance are more outstanding, and high degree has saved human and material resources, financial resources; Adopt 532nm laser and the silicon photocell of low price, significantly reduce cost; Inner structure is simple, and volume is little and quality light, is convenient for carrying, is well suited for bringing to scene and measures; Ensure higher measuring accuracy, can the concentration of local measurement environmental water sample Nitrite in the wild, ensure that authenticity and the reliability of test result.
Accompanying drawing explanation
Fig. 1 is the structural representation of the pick-up unit of nitrite anions concentration of the present invention;
Fig. 2 is the canonical plotting of the concentration of the variable quantity-nitrite anions of the voltage obtained according to the detection method of nitrite anions concentration of the present invention.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention will be further described.
As shown in Figure 1, the pick-up unit of the nitrite anions concentration of the present embodiment comprises: light-source system 1, cuvette 2, sample cell 3, silicon photocell 4 and voltage table 5; Wherein, fill sample and developer in cuvette 2, developer is corresponding with the one-wavelength laser of light-source system 1; Light-source system 1 launches one-wavelength laser, through the cuvette 2 be placed in sample cell 3, is received, convert light signal to electric signal by silicon photocell 4, transfer to voltage table 5.Light-source system 1 comprises laser instrument 11, collimating apparatus 12, heating radiator 13 and voltage stabilizer; Wherein voltage stabilizer connecting laser 11; The surface of laser instrument 11 connects heating radiator 13; Before collimating apparatus 12 is placed on laser instrument by sleeve, the one-wavelength laser sent by laser instrument collimates, and becomes directional light, thus ensures that laser vertical is incident to cuvette.
In the present embodiment, laser instrument 11 adopts 532nm semiconductor laser tube; Collimating apparatus 12 adopts optical coating lens; Heating radiator 13 adopts aluminium alloy radiating fin, carries out active heat removal with 4cm radiator fan to radiating fin and laser instrument; Adopt lithium battery be that laser instrument is powered, and by voltage stabilizer by voltage stabilization at 3.02V; Silicon photocell 4 adopts and drips offset plate ICO-SPC-45MA0.5V, and crest voltage is 0.5V, and peak point current is 45mA; Voltage table 5 adopts 3 half digital display voltmeters, range 0 ~ 1.999V, connects silicon photocell 4 through schottky diode D.Above device is arranged on length, width and height and is respectively in the cabinet of the aluminum of 13cm, 8cm and 5cm, and quality is 278g, and volume is little, quality is light and be convenient for carrying.
In order to realize responding the linear absorption of the laser of 532nm wavelength, the present invention proposes the developer of a certain proportion of citric acid, sulfanilic acid and N-1-naphthyl-ethylenediamine-hydrochloride.Determine the ratio of each composition, realized by following steps:
1) composition of anhydrous sulfanilic acid is first determined: the components unchanged of first fixing citric acid and N-1-naphthyl-ethylenediamine-hydrochloride, increase ascending for the composition of sulfanilic acid successively, obtain the absorption spectra of solution to 532nm laser, be defined as the composition of sulfanilic acid with the point that absorption value is maximum;
2) composition of citric acid is then determined: the components unchanged of fix N-1-naphthyl-ethylenediamine-hydrochloride, and the composition of fixing sulfanilic acid is the composition determined in step 1), increase ascending for the composition of citric acid successively, obtain the absorption spectra of solution to 532nm laser, be defined as the composition of citric acid with the point that absorption value is maximum;
3) sulfanilic acid determined with the point that absorption obtained above is maximum and citric acid components unchanged, increase ascending for the composition of N-1-naphthyl-ethylenediamine-hydrochloride successively, obtain the absorption spectra of solution to 532nm laser, be defined as the composition of N-1-naphthyl-ethylenediamine-hydrochloride with the point that absorption value is maximum, thus obtain the composition of each material of the developer of the laser linear absorption to 532nm.The present invention draws through prolonged and repeated test, 1ml solution to be measured is sequentially added in the 10ml cuvette of fully washing, 1.2ml concentration is the citric acid solution of 210.10g/L, 0.7ml concentration is the sulfanilic acid solution of 1.00g/L, after vibration, add the N-1-naphthyl-ethylenediamine-hydrochloride solution of 0.4ml0.5g/L again, be settled to 10ml.Now, the absorbance of device reaches maximum, and absorbance near it is comparatively stable.Solvent adopts secondary deionized water.
The detection method of the nitrite anions concentration of the present embodiment, comprises the following steps:
1) at 21(n=20) add concentration C successively in the cuvette of only fully washing
ibe respectively 0,0.1,0.2, after 0.3......2.0ml10ng/ μ l sodium nitrite solution, all add 210.10g/L citric acid solution 1.2ml, 0.7ml concentration is 1.00g/L sulfanilic acid solution, after 150rpm vibrates 5 minutes, add N-1-naphthyl-ethylenediamine-hydrochloride solution that 0.4ml concentration is 0.5g/L, be settled to 10ml, the concentration of sodium nitrite is followed successively by 0,0.1,0.2,0.3......2.0ng/ μ l, set up typical curve and the equation of linear regression of the concentration of the variable quantity-nitrite anions of voltage, determine parameter a and regression coefficient b:
A) solution not containing sodium nitrite is injected cuvette, then add quantitative developer, overall solution volume is settled to 10ml;
B) open laser instrument and the voltage table of 532nm, and wait for the stable reading of voltage table, 10 ~ 30 seconds;
C) be placed in sample cell by cuvette, light-source system launches the laser of 532nm, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
0;
D) in cuvette, add concentration is C
initrite anions, after color stability, cuvette is positioned in sample cell;
E) light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
i, 1≤i≤n, n is 20;
F) i is taken to n successively from 1, repeats step d) ~ e), obtain the variable quantity U of voltage
0-U
iwith the concentration C of nitrite anions
itypical curve, and set up the variable quantity U of voltage according to typical curve
0-U
iwith the concentration C of nitrite anions
iequation of linear regression U
0-U
i=a+bC
i, obtain parameter a and regression coefficient b.
The sampling spot of the concentration of nitrite anions is from 0 ~ 2.0ng/ μ l, and be the arithmetic progression that is tolerance with 0.1ng/ μ l, the sampling spot of the concentration of totally 21 nitrite anions, correspondingly obtains the reading of 20 voltage tables, the variable quantity of corresponding 20 voltages; With the concentration of nitrite anions for horizontal ordinate, with the variable quantity U of corresponding voltage table
0-U
ifor ordinate typical curve as shown in Figure 2.Equation of linear regression U is set up according to typical curve
0-U
i=0.1094+0.0070C
i, obtain linear coefficient a=0.1094, b=0.0070.The correlation coefficient r of this equation of linear regression is 0.9984, experimental result shows that the concentration of nitrite anions is within the scope of 0 ~ 1.8ng/ μ l, the aubergine that developer of the present invention makes nitrite anions show, to the absorption of the laser of wavelength 532nm, is good linear relation with the concentration of nitrite anions.
After obtaining parameter a and regression coefficient b, sample is tested, obtains the concentration of the nitrite anions of testing sample:
2) open laser instrument and voltage table, and wait for the stable reading of voltage table, 10 ~ 30 seconds;
3) be positioned in sample cell by the cuvette filling the sample not adding developer, light-source system launches the laser of 532nm, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
0;
4) in the 10ml color comparison tube fully cleaned, 1ml sample to be tested is added, then the 210.10g/L citric acid solution 1.2ml prepared is sequentially added into, 0.7ml concentration is 1.00g/L sulfanilic acid solution, after vibration, add N-1-naphthyl-ethylenediamine-hydrochloride solution that 0.4ml concentration is 0.5g/L, be settled to 10ml, abundant reaction, after color stability, contain and be put in sample cell into cuvette, read voltage table numerical value U;
5) according to U
0the value of-U, the equation of linear regression U of the concentration of logical superpotential variable quantity-nitrite anions
0-U=a+bx, obtains the concentration x of sample Nitrite, wherein, and a=0.1094, b=0.0070.
It is finally noted that, the object publicizing and implementing mode is to help to understand the present invention further, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the content disclosed in embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Claims (2)
1. a detection method for nitrite anions concentration, is characterized in that, described detection method, comprises the following steps:
1) set up typical curve and the equation of linear regression of the concentration of the variable quantity-nitrite anions of voltage, obtain parameter a and regression coefficient b;
2) open mono-colour laser and voltage table, and wait for the stable reading of voltage table;
3) be positioned in sample cell by the cuvette filling the sample not adding developer, light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table
0;
4) developer is added fill in the cuvette of sample, after color stability, cuvette is positioned in sample cell;
5) light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U of now voltage table;
6) according to U
0the value of-U, the equation of linear regression U of the concentration of logical superpotential variable quantity-nitrite anions
0-U=a+bx, obtains the concentration x of sample Nitrite;
Wherein, in step 1) in, set up typical curve and the regression equation of the concentration of the variable quantity-nitrite anions of voltage, comprise the following steps:
A) solution not containing nitrite anions is injected cuvette, then add quantitative developer, overall solution volume is certain;
B) open laser instrument and voltage table, and wait for the stable reading of voltage table;
C) be placed in sample cell by cuvette, light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading U0 of now voltage table;
D) cumulative volume is constant, adds the nitrite anions that concentration is Ci in the cuvette filling developer, after color stability, is positioned over by cuvette in sample cell;
E) light-source system launches one-wavelength laser, through cuvette, is received by silicon photocell, converts light signal to electric signal, transfer to voltage table, records the reading Ui of now voltage table, and 1≤i≤n, n and i is natural number, and n >=2;
F) i gets n successively from 1, repeat steps d) ~ e), obtain the typical curve of the variable quantity U0-Ui of voltage and the concentration C i of nitrite anions, and set up the equation of linear regression U0-Ui=a+bCi of the variable quantity U0-Ui of voltage and the concentration C i of nitrite anions, obtain parameter a and regression coefficient b.
2. detection method as claimed in claim 1, is characterized in that, described in step 2) in, the time of the stable reading of described voltage table is 10 ~ 30 seconds.
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