CN104596995A - Device and method for measuring chlorine elements in water in real time - Google Patents
Device and method for measuring chlorine elements in water in real time Download PDFInfo
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Abstract
The invention relates to the technical field of water detection and in particular relates to a device and a method for measuring chlorine elements in water in real time. The device comprises a water supply unit, a detection chamber, a laser driving unit, a spectra collection unit and a system control unit, wherein the water supply unit is communicated with the detection chamber; a laser transmitting head and a spectra receiving head are arranged in the detection chamber; the laser driving unit is connected with the laser transmitting head; the spectra collection unit is connected with the spectra receiving head; and the system control unit is connected with the laser driving unit and the spectra collection unit. The method comprises the following steps: directly introducing a to-be-measured water body into the detection chamber, exciting chlorine elements in the water body into a plasma state by utilizing high-energy laser, measuring the atomic emission spectroscopy, and measuring the chlorine elements in the water by virtue of the atomic characteristic spectrum of the chlorine elements. According to the method, manual sampling is not needed, pretreatment is avoided, the total chlorine content in the water can be rapidly measured, real-time measurement can be realized, high sensitivity is achieved, secondary pollution is avoided, and the operation is simple and rapid.
Description
Technical field
The present invention relates to water body detection technique field, particularly relate to a kind of real-time measurement apparatus for chlorine element in water and method.
Background technology
At present, have multiple method to measure for chloride test, summary gets up to mainly contain following several:
1, reversed-phased high performace liquid chromatographic, detects and is limited to 0.01mg/L.It detects mechanism is according to solvophobic theory, after solute molecule enters polarity mobile phase, namely occupies corresponding space in mobile phase, and squeezes a part of solvent molecule.When solute molecule is promoted to contact with same phasing by mobile phase, the solvent membrane that nonpolar phasing adheres to exclusion can be held by the nonpolar moiety of solute molecule or the nonpolar factor, and directly combine with the alkyl functional group in non-polar stationary phase (absorption) forms association complex, form monomolecular adsorption layer.When mobile phase polarity reduces, this thin solvent repulsion declines, and solution can occur and form, and solute molecule liberation is eluted.In this detection system, in sample, negative ion retention time immobilizes, and utilizes this feature of sample negative ion to carry out qualitative analysis.In sample, the mass concentration of negative ion is directly proportional to the height (or peak area) of negative signal simultaneously, utilizes this relation to carry out quantitative test.
2, mole method, detects and is limited to 5-100mg/L.Detecting mechanism is to (pH6.5 ~ 10.5) within the scope of alkalescent in neutrality, take potassium chromate as indicator, during with silver nitrate titration chloride, due to the solubleness of the solubleness boy siliver chromate of silver chloride, after first chlorion is precipitated out completely, then chromate is precipitated with the form of siliver chromate, produces brick-red, and instruction titration end-point arrives.
3, potentiometric titration, detects and is limited to 5-100mg/L.Detecting mechanism is for contrast electrode with dual liquid type saturated calomel electrode, take silver electrode as indicator electrode, water sample silver nitrate titer is titrated to chlorine ion concentration equal with concentration of silver ions (namely during theoretical end point), the potential difference (PD) of two electrodes can be used as terminal current potential, stops titration when being titrated to this current potential.Consume volume from silver nitrate titer and can be regarded as out chloride ion content.
4, mercury salt titrimetry, detects and is limited to 1-100mg/L.Detecting mechanism is in the aqueous solution of p H 2.3 ~ 2.8, and chlorion and mercury ion react, and generate micro-mercuric chloride dissociated.Excessive mercury ion and diphenylcarbazone (the even chlorine carbohydrazide of hexichol) form violet complex directing terminal, chloride content in available mercury salt Titration Water Sample.
5, Enrichment spectrophotometric method, detects and is limited to 10-100ug/L.Detecting mechanism is do carrier based on lead phosphate precipitation, Enrichment trace amounts of chlorine compound, after supercentrifuge is separated, with the complete dissolution precipitation of ferric nitrate-perchloric acid solution, add mercuric thiocyanate-methanol solution colour developing, with spectrophotometric method indirect determination underwater trace chloride.
6, turbidimetry, detects and is limited to 1-6mg/L.The method grows up on the basis of colourimetry, is to be carried out according to measuring light a kind of analytical approach of analyzing by the intensity of transmitted light after suspending liquid.
7, ion-exchange chromatography, detects and is limited to 0.1-20mg/L.Detect mechanism for the phase that fixes with ion exchange resin, when mobile phase passes through ion exchange resin with sample, obtain because different ions and Stationary liquid have different affinities the chromatography be separated.
8, polarography, detects and is limited to 0-5mg/L.Polarographic electrode basic structure is that polarized electrode (dropping-mercury electrode) is connected with polarizing voltage negative terminal usually, and contrast electrode (mercurous chloride electrode) is connected with polarizing voltage anode.When putting on before the impressed DC voltage on two electrodes reaches the decomposition voltage being enough to make tested electroactive material reduce in dropping-mercury electrode, by the electric current of electrolytic cell always very little (this Weak current is called aftercurrent), when reaching decomposition voltage, measured matter starts to reduce in dropping-mercury electrode, produce polarogram electric current, after this polarogram electric current increases with impressed voltage and sharply increases, and reaches the limit values gradually (limiting current), no longer increases with impressed voltage and increases.The current-voltage curve obtained like this, is called polarogram.The half wave potential E1/2 of polarogram is the eigenwert of measured matter, can be used to carry out qualitative analysis.Dissufion current depends on measured matter from solution bulk to the speed of dropping-mercury electrode surface diffusion, and its size is determined by the concentration of measured matter in solution, can carry out quantitative test accordingly.
In water, chlorine element is except (comprising hypochlorous acid with ionic state, the elemental chlorine of hypochlorite ion and dissolving) exist outside, some exists with the form in conjunction with state (comprising all chlorinated derivatives of monochloro amine, dichlormaine, agene and organic nitrogen compound), be determined as when pH is 6.2 ~ 6.5 for chlorine total in water, under excessive potassium iodide exists, total chlorine and N in sample, N-diethyl-1,4-phenylenediamine (DPD) reacts, generate red compound, in 510nm wavelength place, use spectrophotometry.
For said method, although wherein RP-HPLC method remolding sensitivity is higher, technical sophistication, expensive equipment, sample has to pass through pre-service, can not realize real-time measurement; Mole method, potentiometric titration, this several method sensitivity of mercury salt titrimetry are lower, poor reproducibility, and error is large, and is easily subject to other ions (bromine, iodine, sulphur plasma) interference, can not real-time online measuring; Enrichment spectrophotometric method complicated operation, takes time and effort, equally can not real-time online measuring; Turbidimetry has requirement to water pH value, and must under sour environment, and need to add silver nitrate, detection of complex, universality is poor; Ion-exchange chromatography, because ion exchange resin is to the selectivity difference of different ions, is therefore difficult to detect the chlorion of different shape simultaneously, more can not detects the chlorine element in conjunction with state; Polarography is mainly subject to precision and the life-span restriction of polarographic electrode, and need to demarcate once every one or two months, measuring speed is slow, is also to measure ionic state chlorine element.
Therefore, for above deficiency, need a kind of can not only chloride content in Quick Measuring water gaging, do not need pre-service of sampling, do not need other medicines to carry out chemical reaction, there is no secondary pollution, simple and convenient, but also there is higher sensitivity, the device and method of on line real time control can be realized.
Summary of the invention
(1) technical matters that will solve
The technical problem to be solved in the present invention there is provided a kind of real-time measurement apparatus for chlorine element in water and method, can not only chloride content in Quick Measuring water gaging, do not need pre-service of sampling, other medicines are not needed to carry out chemical reaction, there is no secondary pollution, simple and convenient, but also there is higher sensitivity, can on line real time control be realized.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of real-time measurement apparatus for chlorine element in water, it comprises water supplying unit, sensing chamber, laser drive unit, spectra collection unit and system control unit; Described water supplying unit is communicated with sensing chamber; Laser beam emitting head and spectrum acquisition head is provided with in described sensing chamber; Described laser drive unit is connected with laser beam emitting head, forms laser for driving laser emitting head; Described spectra collection unit is connected with spectrum acquisition head, for gathering the spectrum that spectrum acquisition hair goes out; Described system control unit is connected with laser drive unit and spectra collection unit, for controlling laser drive unit and spectra collection unit in real time.
Wherein, this device also comprises nitrogen and purges unit, and described nitrogen purges unit and comprises gas-holder, tracheae and operation valve, and described gas-holder is communicated with sensing chamber by tracheae, and described operation valve is arranged on tracheae.
Wherein, the top of described sensing chamber is provided with the air admission hole be communicated with tracheae, and is provided with vent port bottom it.
Wherein, described water supplying unit comprises gutter, water pump and liquid trap; Described water pump is communicated with gutter, liquid trap by water-supply-pipe, and described water pump is used for the water in gutter to be pumped in liquid trap; Described liquid trap is communicated in the top of sensing chamber.
Wherein, the lower end of described liquid trap is positioned at sensing chamber and is opening shape; The upper end of described liquid trap to be positioned at outside sensing chamber and to be connected with water-supply-pipe.
Wherein, the upper end of described liquid trap is provided with scale.
Wherein, described laser beam emitting head and spectrum acquisition head are all towards the water outlet direction of liquid trap, and described spectrum acquisition head is positioned at the below of laser beam emitting head.
Wherein, the front of described spectrum acquisition head is provided with lens.
The present invention also provides a kind of method for real-time measurement for chlorine element in water, and it comprises the steps:
S1, by water supplying unit water sample to be measured to be delivered in sensing chamber and to form current;
S2, by laser beam emitting head, laser impact is carried out to current, make element in current excite as plasma state instantaneously;
S3, the spectrum launched by spectrum acquisition head reception plasma state element, and this spectrum is passed to spectra collection unit;
S4, spectra collection unit carry out light splitting screening to the spectrum gathered, thus select the spectrum of chlorine element.
S5, by system control unit, long-range real time and on line monitoring is carried out to step S2-S4.
Wherein, also comprise in step S1 utilize nitrogen purge unit in sensing chamber, input nitrogen, to eliminate the interference of oxygen.
(3) beneficial effect
Technique scheme of the present invention has following beneficial effect: the present invention is used for real-time measurement apparatus and the method for chlorine element in water, superlaser is utilized to excite as plasma state by chlorine element in water body, then its atomic emission spectrum is measured, can according to the measurement of atomic features spectral line realization to chlorine element in water of chlorine element.The method can not only chloride content in Quick Measuring water gaging, does not need pre-service of sampling, does not need other medicines to carry out chemical reaction, do not have secondary pollution, simple and convenient, but also has higher sensitivity, can realize on line real time control.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention for the real-time measurement apparatus of chlorine element in water.
Wherein, 1: gutter; 2: water pump; 3: water-supply-pipe; 4: liquid trap; 5: sensing chamber; 6: lens; 7: laser beam emitting head; 8: spectrum acquisition head; 9: laser drive unit; 10: spectra collection unit; 11: system control unit; 12: gas-holder; 13: tracheae; 14: operation valve; 15: optical fiber; 16: air admission hole; 17: vent port; 18: water sample to be measured.
Embodiment
Below in conjunction with drawings and Examples, embodiments of the present invention are described in further detail.Following examples for illustration of the present invention, but can not be used for limiting the scope of the invention.
In describing the invention, except as otherwise noted, the implication of " multiple " is two or more; Term " on ", D score, "left", "right", " interior ", " outward ", " front end ", " rear end ", " head ", the orientation of the instruction such as " afterbody " or position relationship be based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.In addition, term " first ", " second ", " the 3rd " etc. only for describing object, and can not be interpreted as instruction or hint relative importance.
In describing the invention, it should be noted that, unless otherwise clearly defined and limited, term " installation ", " being connected ", " connection " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary.For the ordinary skill in the art, concrete condition above-mentioned term concrete meaning in the present invention can be understood.
As shown in Figure 1, the real-time measurement apparatus for chlorine element in water that the present embodiment provides, it comprises water supplying unit, sensing chamber 5, laser drive unit 9, spectra collection unit 10 and system control unit 11; Wherein, water supplying unit is communicated with sensing chamber 5, and forms current in sensing chamber 5; And be provided with laser beam emitting head 7 and spectrum acquisition head 8 in sensing chamber 5, laser beam emitting head 7 and spectrum acquisition head 8 are all towards water (flow) direction.Laser beam emitting head 7 can carry out laser impact to current, makes element in current excite as plasma state instantaneously, and meanwhile, spectrum acquisition head 8 receives the spectrum that plasma state element is launched; Laser drive unit 9 is connected with laser beam emitting head 7, forms laser for driving laser emitting head 7; Spectra collection unit 10 is connected with spectrum acquisition head 8, for gathering the plasma emission spectroscopy after laser excitation current, and filters out the atomic emission spectrum of chlorine element; System control unit 11 is connected with laser drive unit 9 and spectra collection unit 10 respectively, for controlling laser drive unit 9 and spectra collection unit 10 in real time.This device can not only chloride content in Quick Measuring water gaging, but also does not need to carry out pre-service to water sample, does not need other medicines to carry out chemical reaction, there is no secondary pollution, simple and convenient, simultaneously, there is higher sensitivity, online portable type measuring can be realized.
In order to eliminate the interference of oxygen, this device also comprises nitrogen and purges unit, and wherein nitrogen purging unit comprises gas-holder 12, tracheae 13 and operation valve 14, and gas-holder 12 is communicated with sensing chamber 5 by tracheae 13, and operation valve 14 is arranged on tracheae 13.
Concrete, the hole of a diameter 3cm can be opened near the place of liquid trap 4 on sensing chamber 5 top as air admission hole 16, side, bottom also be opened the hole of a diameter 1cm as vent port 17.During detection, purge with the laser excitation point of nitrogen to liquid, object is driven away by the oxygen in air.Because the emission spectrum wavelength of chlorine element and oxygen are closely, oxygen easily forms interference to detection.Driven away by oxygen with nitrogen, avoid the generation of this interference, nitrogen imports in sensing chamber 5 by tracheae 13, tracheae 13 has operation valve 14, is used for controlling gas velocity.Tracheae 13 other end is ined succession gas-holder 12, and be nitrogen in gas-holder 12, the position of gas-holder 12 higher than the air intake opening 16 of sensing chamber 5, should be beneficial to nitrogen and be purged by tracheae 13.
Water supplying unit comprises gutter 1, water pump 2 and liquid trap 4; Water pump 2 is communicated with gutter 1, liquid trap 4 respectively by water-supply-pipe 3, for being pumped in liquid trap 4 by the water in gutter 1; Liquid trap 4 is communicated in the top of sensing chamber 5.
Wherein, gutter 1 is be communicated with water sample 18 to be measured and the rectangle glass groove constantly having water body to exchange, and effect is introduced through by water sample 18 to be measured, and water quality in gutter 1 is consistent with water body overall situation all the time, ensures real-time and the accuracy of measurement.
And water pump 2 effect is drawn in liquid trap 4 by the water sample to be measured 18 in gutter 1 by water-supply-pipe 3, and liquid trap 4 is fixed on directly over gutter 1, height adjustable.Termination water-supply-pipe 3 on liquid trap 4, its bottom end opening, makes water can flow down with the form of freely falling body.And liquid trap 4 has half to be embedded in sensing chamber 5, indicates scale above the half be exposed, the water level in liquid trap 4 is made to maintain the position of 2/3rds by the power adjusting water pump 2.
Sensing chamber 5 is cubes of a hollow, and the current that liquid trap 4 lower end is flowed out can be flow in gutter 1 below by the aperture of sensing chamber 5 lower end.And be provided with laser beam emitting head 7 and spectrum acquisition head in sensing chamber 5, laser beam emitting head 7 and spectrum acquisition head 8 all towards the water outlet direction of liquid trap 4, that is, can carry out the direction of laser excitation to current; Spectrum acquisition head 8 is positioned at the below of laser beam emitting head 7.The superlaser that laser beam emitting head 7 sends directly is beaten on the current that flow down at liquid trap 4, element in current is excited instantaneously into plasma state, then the emission spectrum of each element of plasma state is received by spectrum acquisition head 8, the front of spectrum acquisition head 8 is provided with lens 6, its focal length is 10cm, this distance can effectively avoid liquid by the impact of gasifying during laser excitation, and liquid splash also can be avoided on lens 6 simultaneously.
Wherein, laser beam emitting head 7 is connected with laser drive unit 9 by optical fiber 15, and laser drive unit 9 comprises solid state laser, light source, electronic control circuit, cooling system etc.; Correspondingly, spectrum acquisition head 8 is also connected with spectra collection unit 10 by optical fiber 15, spectra collection unit 10 inside comprises beam splitting system, detecting device and driving circuit, the bandpass filter of a slice 835nm is added in the entrance location of spectra collection unit 10, bandwidth is 40nm, is used for selecting the emission spectrum of chlorine element; Simultaneously, laser drive unit 9 is all connected with system control unit 11 by cable with spectra collection unit 10, system control unit 11 comprises the modules such as data calculating, model analysis, control circuit, communicating circuit, supports ICP/IP protocol, can realize teledata and read and system state control.
The present invention also provides a kind of method for real-time measurement for chlorine element in water, and it comprises the steps:
S1, by water supplying unit water sample to be measured to be delivered in sensing chamber and to form current, meanwhile, utilize nitrogen to purge unit and in sensing chamber, input nitrogen, to eliminate the interference of oxygen.In this step, current are directly introduced sensing chamber, instead of take test in laboratory with container splendid attire, its real-time is good, and can reduce sample sampling link, reduces the probability of sample changed, can be implemented in line and measure.
S2, by laser beam emitting head, laser impact is carried out to current, make element in current excite as plasma state instantaneously; After formation current, re-use the direct laser printer current of laser in this step, instead of use laser laser printer again after being filled with water with container.This method ensure that the homogeneity of sample, is conducive to keeping sample original state, reduces artificial interference, and does not need laser beam emitting head to be immersed in the water, do not introduce other medicines and there is not chemical reaction, has speed fast, does not have the advantage of secondary pollution.
S3, the spectrum launched by spectrum acquisition head reception plasma state element, and this spectrum is passed to spectra collection unit; The spectrum acquisition head of this step, away from spectral emissions point, without the need to being immersed in the water by spectrum acquisition head (focal length of signal collection part lens is 10cm), effectively prevent closely liquid gasification and splashing on the impact of probe.
S4, spectra collection unit carry out light splitting screening to the spectrum gathered, thus select the spectrum of chlorine element, and by installing optical filter additional, the interference of filtering parasitic light, selects the spectrum of cleaner chlorine element.
S5, by system control unit, long-range real time and on line monitoring is carried out to step S2-S4, read and system state control to realize teledata.
In sum, the present invention is used for real-time measurement apparatus and the method for chlorine element in water, utilize superlaser to excite as plasma state by chlorine element in water body, then measure its atomic emission spectrum, can according to the measurement of atomic features spectral line realization to chlorine element in water of chlorine element.The method can not only chloride content in Quick Measuring water gaging, does not need pre-service of sampling, does not need other medicines to carry out chemical reaction, do not have secondary pollution, simple and convenient, but also has higher sensitivity, can realize on line real time control.
Embodiments of the invention provide in order to example with for the purpose of describing, and are not exhaustively or limit the invention to disclosed form.Many modifications and variations are apparent for the ordinary skill in the art.Selecting and describing embodiment is in order to principle of the present invention and practical application are better described, and enables those of ordinary skill in the art understand the present invention thus design the various embodiments with various amendment being suitable for special-purpose.
Claims (10)
1. the real-time measurement apparatus for chlorine element in water, it is characterized in that, comprise water supplying unit, sensing chamber (5), laser drive unit (9), spectra collection unit (10) and system control unit (11); Described water supplying unit is communicated with sensing chamber (5); Laser beam emitting head (7) and spectrum acquisition head (8) is provided with in described sensing chamber (5); Described laser drive unit (9) is connected with laser beam emitting head (7), forms laser for driving laser emitting head (7); Described spectra collection unit is connected with spectrum acquisition head (8), for gathering the spectrum that spectrum acquisition head (8) sends; Described system control unit (11) is connected with laser drive unit (9) and spectra collection unit (10), for controlling laser drive unit (9) and spectra collection unit (10) in real time.
2. the real-time measurement apparatus for chlorine element in water according to claim 1, it is characterized in that, also comprise nitrogen and purge unit, described nitrogen purges unit and comprises gas-holder (12), tracheae (13) and operation valve (14), described gas-holder (12) is communicated with sensing chamber (5) by tracheae (13), and described operation valve (14) is arranged on tracheae (13).
3. the real-time measurement apparatus for chlorine element in water according to claim 2, it is characterized in that, the top of described sensing chamber (5) is provided with the air admission hole (16) be communicated with tracheae (13), and is provided with vent port (17) bottom it.
4. the real-time measurement apparatus for chlorine element in water according to claim 2, is characterized in that, described water supplying unit comprises gutter (1), water pump (2) and liquid trap (4); Described water pump (2) is communicated with gutter (1), liquid trap (4) by water-supply-pipe (3), and described water pump (2) is for being pumped in liquid trap (4) by the water in gutter (1); Described liquid trap (4) is communicated in the top of sensing chamber (5).
5. the real-time measurement apparatus for chlorine element in water according to claim 4, is characterized in that, the lower end of described liquid trap (4) is positioned at sensing chamber (5) and is opening shape; The upper end of described liquid trap (4) is positioned at sensing chamber (5) and be connected with water-supply-pipe (3) outward.
6. the real-time measurement apparatus for chlorine element in water according to claim 5, is characterized in that, the upper end of described liquid trap (4) is provided with scale.
7. the real-time measurement apparatus for chlorine element in water according to claim 4, it is characterized in that, described laser beam emitting head (7) and spectrum acquisition head (8) are all towards the water outlet direction of liquid trap (4), and described spectrum acquisition head (8) is positioned at the below of laser beam emitting head (7).
8. the real-time measurement apparatus for chlorine element in water according to claim 1, is characterized in that, the front of described spectrum acquisition head (8) is provided with lens (6).
9. the measuring method for the real-time measurement apparatus of chlorine element in water according to any one of claim 1-8, is characterized in that, comprise the steps:
S1, by water supplying unit water sample to be measured to be delivered in sensing chamber and to form current;
S2, by laser beam emitting head, laser impact is carried out to current, make element in current excite as plasma state instantaneously;
S3, the spectrum launched by spectrum acquisition head reception plasma state element, and this spectrum is passed to spectra collection unit;
S4, spectra collection unit carry out light splitting screening to the spectrum gathered, thus select the spectrum of chlorine element.
S5, by system control unit, long-range real time and on line monitoring is carried out to step S2-S4.
10. measuring method according to claim 9, is characterized in that, also comprises and utilize nitrogen purging unit in sensing chamber, to input nitrogen, to eliminate the interference of oxygen in step S1.
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