CN104458878A - Saccharin sodium concentration detection device and saccharin sodium concentration detection method - Google Patents
Saccharin sodium concentration detection device and saccharin sodium concentration detection method Download PDFInfo
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- CN104458878A CN104458878A CN201410502330.0A CN201410502330A CN104458878A CN 104458878 A CN104458878 A CN 104458878A CN 201410502330 A CN201410502330 A CN 201410502330A CN 104458878 A CN104458878 A CN 104458878A
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Abstract
The invention discloses a saccharin sodium concentration detection device and a saccharin sodium concentration detection method. The saccharin sodium concentration detection device comprises a controller, a storage device, a container which is provided with an opening in the upper end and is capable of containing liquid, a cover plate which is arranged on the container, a counter electrode which is arranged on the cover plate, extends downwards and is made of a platinum material, an evolvent-shaped guide rail which is embedded into an opening in the lower end of the lower part of the cover plate, a rotating device which is arranged on the guide rail and can move along the guide rail, a stirring device which is arranged on the bottom of the container and a dropping funnel which is arranged on the cover plate and used for dropwise adding saccharin sodium solution into the container, wherein the counter electrode is connected with the cover plate through a first motor, one end of the guide rail is close to the first motor, and the other end of the guide rail is close to the edge of the cover plate. The saccharin sodium concentration detection device has characteristics of high detection precision, high speed, good stability and good repeatability.
Description
Technical field
The present invention relates to technical field of food detection, especially relate to a kind of detection accuracy high, fireballing saccharin sodium concentration detection apparatus and detection method.
Background technology
Existing sugared detection technique method has instrumental analysis detection method and chemical measure, although instrumental analysis detection method is simple to operate, there is the defect that accuracy of detection is low; There is complex operation in chemical measure, the deficiency of poor repeatability.
Chinese patent mandate publication number: CN103528877A, authorizes publication date on January 22nd, 2014, discloses the online system of detecting concentration of sugar of a kind of miniature biochemical reactor, comprise 1 touch-screen, be responsible for the setting and the operation that accept field staff; 2 constant flow pumps, are responsible for diluting reactant liquor; 1 online sugar analyzer, is responsible for the on-line checkingi of sugared concentration; 1 off-line sugar concentration analyzer, is responsible for the offline inspection of sugared concentration; 1 flush bonding module BL2100, as the control module of system, control the flow velocity of constant flow pump and the action of sugared concentration analyzer, gather the sugared Concentration Testing value of online glycan analysis instrument, on-line correction is carried out to collection value, to obtain in biochemical reactor sugared Concentration Testing value accurately, and according to the value of off-line sugar concentration analyzer, model parameter is revised.The weak point of this invention is, the deficiency of the low and poor repeatability of accuracy of detection.
Summary of the invention
Goal of the invention of the present invention is the deficiency in order to overcome the low and poor repeatability of detection method accuracy of detection of the prior art, provides a kind of detection accuracy high, fireballing saccharin sodium concentration detection apparatus and detection method.
To achieve these goals, the present invention is by the following technical solutions:
A kind of saccharin sodium concentration detection apparatus, described saccharin sodium concentration detection apparatus is electrically connected with electrochemical workstation; Comprise controller, storer, fill the container of the upper end open of liquid, be located at the cover plate on container, the alloy platinum material to downward-extension be located on cover plate make to electrode, embed the involute urve shape guide rail of lower ending opening of cover plate bottom, be located on guide rail can along the wheelwork of guide rail movement, the agitating device being located at container bottom and the tap funnel for instilling saccharin sodium solution in container be located on cover plate; Be connected with cover plate by the first motor to electrode, guide rail one end is near the first motor, and the guide rail other end is near side edge thereof;
Described wheelwork bottom is provided with the working electrode that foam copper material is made, and agitating device is connected with container bottom by waterproof machine; Working electrode and to electrode all in bar shaped tabular; Described controller is electrically connected with waterproof machine, storer, the first motor, wheelwork and electrochemical workstation respectively; Electrode and working electrode are electrically connected with electrochemical workstation respectively.
The setting of the guide rail in involute urve shape of the present invention, makes working electrode and to the spacing continuously adjustabe between electrode, is convenient to electrochemical workstation and finds the optimum position residing for two electrodes when making current density maximum, thus improve accuracy of detection.Agitating device is used for stirring the liquid in container, and wheelwork moves for driving working electrode.
The present invention, by detecting concentration known saccharin sodium solution, obtains the saccharin sodium concentration prediction model of saccharin sodium concentration, and detects the saccharin sodium concentration of unknown concentration with saccharin sodium concentration prediction model.
Therefore, the present invention has simple to operate, and automaticity is high; Accuracy of detection is high, and speed is fast; Device stability is good, reproducible feature.
As preferably, described guide rail comprises top board and is located at two baffle plates of top board both sides, and two baffle plates are provided with corresponding guide openings; Described wheelwork comprises motor fixing seat, the second motor be located in motor fixing seat, two gears be connected respectively with two rotating shafts of the second motor and two extension rods be located at respectively on outside two gears, and two extension rods stretch in two guide openings respectively;
The position corresponding with two gears, described guide rail bottom is provided with the track plates of two upper surfaces with groove; Guide rail is provided with the dual-cavity for coordinating with two gears, and two track plates two ends are all connected with guide rail, and described working electrode is connected with motor fixing seat; Described second motor is electrically connected with controller.
The setting of guide rail, wheelwork and shut, makes working electrode can along the stable movement of guide rail.
As preferably, described agitating device comprises the horizontal stirring pipe be connected with the rotating shaft of waterproof machine, and horizontal stirring pipe is provided with some through holes to being oppositely arranged; Horizontal stirring pipe is provided with several straight-bars vertical with the axial line of horizontal stirring pipe.
As preferably, described straight-bar comprises longitudinal rod and horizon bar.
The vibrational power flow of agitating device, what the solution in container can be stirred is more even.
As preferably, cover plate and container are all rounded; Cover plate lower surface is provided with annular groove, and container upper end is inserted in annular groove and is connected with cover plate.
Be applicable to a detection method for saccharin sodium concentration detection apparatus, comprise the steps:
(6-1) be provided with sweep interval A in controller, scanning times maximal value N, the initial value of scanning times sequence number i, i is 1;
The 0.1M NaOH getting 20 to 50ml inserts in container, cover plate is installed to container finish, makes working electrode and stretch in NaOH to electrode;
Electrochemical workstation exports the constant voltage of 0.40V to 0.6V to working electrode, regulates the piston filling the tap funnel of the saccharin sodium solution of 0.1M, makes the per interval A of tap funnel instill a saccharin sodium solution in container;
(6-2), extremely instill second saccharin sodium solution after tap funnel instills first saccharin sodium in container before, controller controls stirring apparatus to the liquid agitation time B in container, B < A by waterproof machine; Controller controls the first driven by motor and horizontally rotates electrode, control wheelwork drives working electrode to reciprocate along guide rail simultaneously, electrochemical workstation detects current density, when the current density detected reaches maximal value, controller controls wheelwork and the first motor quits work, and obtains the optimum position to electrode and working electrode;
Electrode is horizontally rotated and working electrode movement process in, maximum relative area is remained to electrode and working electrode;
Controller calculates the saccharin sodium concentration k in current container
1, by k
1and with k
1corresponding current density S (t) is stored in storer;
(6-3) tap funnel instills the i-th+1 saccharin sodium solution in container, and controller controls stirring apparatus to the liquid agitation time B in container, B < A by waterproof machine; Electrochemical workstation detects current density, and controller calculates the saccharin sodium concentration k in current container
i+1, by k
i+1and with k
i+1corresponding current density S (t) is stored in storer;
(6-4) as i≤N-1, make i value increase by 1, proceed to step (6-3); Otherwise, proceed to step (6-5);
(6-5) the N number of current density S (t) obtained is inputted second-order linear system accidental resonance model by controller respectively
In; And second-order linear system accidental resonance model is resonated;
Wherein, x (t) is the displacement of vibration particle, and Ω is angular frequency, r and ω is the attenuation coefficient of setting and the frequency of linear oscillator particle respectively, and c is the signal adjustment coefficient of setting, and b is the quadratic noise ξ of setting
2t the coefficient of (), ξ (t) is three discrimination noises, and { dismutation of noise follows Poisson distribution to ξ (t) ∈ for-a, 0, a}, a > 0, and its probability distribution is p
s(a)=p
s(-a)=q, p
s(0)=1-2q, wherein 0 < q < 0.5;
Noise average and correlativity follow < ξ (t) >=0, < ξ (t) ξ (t+ τ) >=2qa
2e
-λ τ;
Wherein λ is correlation ratio, and the flatness of three discriminations noise ξ (t) is
Controller utilizes formula
calculate and obtain the output signal-to-noise ratio SNR corresponding respectively with N number of current density S (t)
1, SNR
2..., SNR
n;
Controller reads the saccharin sodium concentration k in storer
1, k
2..., k
n; Controller utilizes point (k
1, SNR
1), (k
2, SNR
2) ..., (k
n, SNR
n) fit to straight line, draw saccharin sodium concentration prediction model according to the straight line of matching:
the liquid of container is poured out, and vessel cleaning is clean;
(6-6) detection of the saccharin sodium solution W of unknown concentration:
The saccharin sodium solution W of getting 20 to 50ml is inserted in container, cover plate is installed to container finish, makes working electrode and stretch in saccharin sodium solution electrode, and make working electrode and be positioned at step (6-2) determined optimum position to electrode; Electrochemical workstation exports the constant voltage of 0.40V to 0.6V to working electrode, and electrochemical workstation detects current density S (t), and S (t) inputs in second-order linear system accidental resonance model by controller,
And utilize formula
calculate and obtain output signal-to-noise ratio SNR, SNR is substituted into
obtain the concentration k of saccharin sodium solution W.
As preferably, also comprise alarm, alarm and controller electrical connection; Also comprise alarm, alarm and controller electrical connection; Following electrode calibration step was also comprised before step (6-1):
(7-1) the 0.1M NaOH getting 30 to 48ml inserts in the first beaker, by working electrode and insert in the NaOH solution of the first beaker to electrode, electrochemical workstation is utilized to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, reduce gradually again, obtaining horizontal ordinate is driving voltage, and ordinate is the curve of current density, the difference g between the maximal value of calculating current density and minimum value;
(7-2) get 0.1M NaOH and 0.1mM saccharin sodium successively and to insert in the second beaker according to the ratio of 3: 2 and to stir, by working electrode and insert in the solution of the second beaker to electrode, electrochemical workstation is utilized to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, reduce gradually again, obtaining horizontal ordinate is driving voltage, ordinate is the curve of current density, the difference g ' between the maximal value of calculating current density and minimum value;
(7-3) controller utilizes
the error of calculation, when e≤4.7%, proceeds to step (6-1);
Otherwise controller controls alarm equipment alarm, operating personnel are to electrode being carried out to surface treatment or changing electrode; Return step (7-1).
Because the working electrode that foam copper material is made is disposable, all detect with new working electrode at every turn, but what alloy platinum material was made will repeatedly Reusability to electrode, access times are more, more serious to the oxidized corrosion of electrode, so need to detect to the state of electrode, after calibration, only have and qualified just detection is used in electrode, guarantee the accuracy of testing result.
As preferably, driving voltage first increases gradually with the speed of 0.05V/s in-0.2V-0.75V scope, then reduces gradually with the speed of 0.05V/s.
As preferably, the area that foam copper and platinum electrode stretch into solution is 0.085cm
2to 0.135cm
2.
As preferably, A is 42 to 58 seconds, and N is 10 to 108, B is 9 to 30 seconds.
Therefore, the present invention has following beneficial effect: simple to operate, and automaticity is high; Accuracy of detection is high, and speed is fast; Device stability is good, reproducible.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of the present invention;
Fig. 2 is a kind of structural representation of guide rail of the present invention;
Fig. 3 is a kind of structural representation of wheelwork of the present invention;
Fig. 4 is a kind of theory diagram of the present invention;
Fig. 5 is a kind of process flow diagram of embodiments of the invention 1;
Fig. 6 is cyclic voltammetry calibration result figure of the present invention.
In figure: electrochemical workstation 1, controller 2, storer 3, container 4, cover plate 5, guide rail 6, platinum are to electrode 7, wheelwork 8, agitating device 9, tap funnel 10, working electrode 11, first motor 12, waterproof machine 13, stirring pipe 14, track plates 15, baffle plate 16, motor fixing seat 17, second motor 18, rotating shaft 19, gear 20, extension rod 21, dual-cavity 22, through hole 23, longitudinal rod 24, horizon bar 25.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
Embodiment is as Figure 1 and Figure 4 a kind of saccharin sodium concentration detection apparatus, and saccharin sodium concentration detection apparatus is electrically connected with electrochemical workstation 1; Comprise controller 2, storer 3, fill the container 4 of the upper end open of liquid, be located at the cover plate 5 on container, the alloy platinum material to downward-extension be located on cover plate make to electrode 7, the agitating device 9 being located at container bottom and the tap funnel 10 for instilling saccharin sodium solution in container be located on cover plate; Agitating device comprises the horizontal stirring pipe 14 be connected with the rotating shaft of waterproof machine, and horizontal stirring pipe is provided with some through holes 23 to being oppositely arranged; Horizontal stirring pipe is provided with several straight-bars vertical with the axial line of horizontal stirring pipe.Cover plate adopts polytetrafluoroethylmaterial material to make, and container adopts glass material to make.
Straight-bar comprises longitudinal rod 24 and horizon bar 25.Cover plate and container are all rounded; Cover plate lower surface is provided with annular groove, and container upper end is inserted in annular groove and is connected with cover plate.
The involute urve shape guide rail 6 of the lower ending opening of embedding cover plate bottom as shown in Figure 2, be located on guide rail can along the wheelwork 8 of guide rail movement,
As shown in Figure 3, wheelwork bottom is provided with the working electrode 11 that foam copper material is made, and guide rail comprises top board and is provided with corresponding guide openings with two baffle plates, 16, two baffle plates being located at top board both sides; Wheelwork comprises motor fixing seat 17, the second motor 18 be located in motor fixing seat, two gears 20 be connected respectively with two rotating shafts 19 of the second motor and two extension rods, 21, two extension rods be located at respectively on outside two gears stretch in two guide openings respectively;
The position corresponding with two gears, guide rail bottom is provided with the track plates 15 of two upper surfaces with groove; Dual-cavity 22, two track plates two ends that guide rail is provided with for coordinating with two gears are all connected with guide rail, and working electrode is connected with motor fixing seat;
As shown in Figure 4, agitating device is connected with container bottom by waterproof machine 13; Working electrode and to electrode all in bar shaped tabular; Controller is electrically connected with waterproof machine, storer, the first motor, wheelwork and electrochemical workstation respectively; Be electrically connected with electrochemical workstation respectively electrode and working electrode, the second motor is electrically connected with controller.
As shown in Figure 5, a kind of detection method of saccharin sodium concentration detection apparatus, comprises the steps:
Step 100, is provided with sweep interval 50 seconds, scanning times maximal value N=10 in controller, the initial value of scanning times sequence number i, i is 1;
The 0.1M NaOH getting 30ml inserts in container, cover plate is installed to container finish, makes working electrode and stretch in NaOH to electrode;
Electrochemical workstation exports the constant voltage of 0.5V to working electrode, regulates the piston filling the tap funnel of the saccharin sodium solution of 0.1M, makes tap funnel in container, instill a saccharin sodium solution every 50 seconds;
Step 200, finds optimum position by k
1and with k
1corresponding current density S (t) is stored in storer:
To before instillation second saccharin sodium solution after tap funnel instills first saccharin sodium in container, controller controls stirring apparatus to the liquid agitation in container 10 seconds by waterproof machine; Controller controls the first driven by motor and horizontally rotates electrode, control wheelwork drives working electrode to reciprocate along guide rail simultaneously, electrochemical workstation detects current density, when the current density detected reaches maximal value, controller controls wheelwork and the first motor quits work, and obtains the optimum position to electrode and working electrode;
Electrode is horizontally rotated and working electrode movement process in, maximum relative area is remained to electrode and working electrode;
Controller calculates the saccharin sodium concentration k in current container
1(such as, often dripping saccharin sodium solution is 0.05ml, and controller calculates saccharin sodium concentration k according to the total measurement (volume) of solution in the molten number of drops of the saccharin sodium instilled in container and container
1), by k
1and with k
1corresponding current density S (t) is stored in storer;
Step 300,
Tap funnel instills the i-th+1 saccharin sodium solution in container, and controller controls stirring apparatus to the liquid agitation in container 10 seconds by waterproof machine; Electrochemical workstation detects current density, and controller calculates the saccharin sodium concentration k in current container
i+1, by k
i+1and with k
i+1corresponding current density S (t) is stored in storer;
Step 400, when i≤9, makes i value increase by 1, proceeds to step 300; Otherwise, proceed to step 500;
Step 500, data processing:
10 the current density S (t) obtained are inputted second-order linear system accidental resonance model by controller respectively
In; And second-order linear system accidental resonance model is resonated;
Wherein, x (t) is the displacement of vibration particle, and Ω is angular frequency, r and ω is the attenuation coefficient of setting and the frequency of linear oscillator particle respectively, and c is the signal adjustment coefficient of setting, and b is the quadratic noise ξ of setting
2t the coefficient of (), ξ (t) is three discrimination noises, and { dismutation of noise follows Poisson distribution to ξ (t) ∈ for-a, 0, a}, a > 0, and its probability distribution is p
s(a)=p
s(-a)=q, p
s(0)=1-2q, wherein 0 < q < 0.5;
Noise average and correlativity follow < ξ (t) >=0, < ξ (t) ξ (t+ τ) >=2qa
2e
-λ τ;
Wherein λ is correlation ratio, and the flatness of three discriminations noise ξ (t) is
Utilize formula
calculate and obtain the output signal-to-noise ratio SNR corresponding respectively with 10 current density S (t)
1, SNR
2..., SNR
10;
Controller reads the saccharin sodium concentration k in storer
1, k
2..., k
10; Controller utilizes point (k
1, SNR
1), (k
2, SNR
2) ..., (k
10, SNR
10) fit to straight line, draw saccharin sodium concentration prediction model according to the straight line of matching:
the liquid of container is poured out, and vessel cleaning is clean;
Step 600, the detection of the saccharin sodium solution W of unknown concentration:
The saccharin sodium solution W of getting 30ml is inserted in container, cover plate is installed to container finish, makes working electrode and stretch in saccharin sodium solution electrode, and make working electrode and be positioned at the determined optimum position of step 200 to electrode; Electrochemical workstation exports the constant voltage of 0.5V to working electrode, and electrochemical workstation detects current density S (t), and S (t) inputs in second-order linear system accidental resonance model by controller,
And utilize formula
calculate and obtain output signal-to-noise ratio SNR, SNR is substituted into
obtain the concentration k of saccharin sodium solution W.
Embodiment 2
Comprise all structures and the step part of embodiment 1 in embodiment 2, also comprise alarm, alarm and controller electrical connection; Following electrode calibration step was also comprised before step 100:
Step 710, the 0.1M NaOH getting 40ml inserts in the first beaker, by working electrode and insert in the NaOH solution of the first beaker to electrode, electrochemical workstation is utilized to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, then reduces gradually, obtaining horizontal ordinate is driving voltage, ordinate is the curve of current density, the difference g between the maximal value of calculating current density and minimum value;
Step 720, ratio according to 3: 2 gets 0.1M NaOH successively and 0.1mM saccharin sodium inserts in the second beaker, and stir, by working electrode and insert electrode in the solution of the second beaker, utilize electrochemical workstation to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, reduce gradually again, obtaining horizontal ordinate is driving voltage, and ordinate is the curve of current density, the difference g ' between the maximal value of calculating current density and minimum value;
Step 730, controller utilizes
the error of calculation, when e≤4.7%, proceeds to step 100;
Otherwise controller controls alarm equipment alarm, and operating personnel detect to electrode, in the present embodiment, find there is defect to electrode surface, change to electrode; Return step 710.
Fig. 6 is the cyclic voltammetry calibration testing result figure demonstrated on electrochemical workstation, can draw, g '=6.8V, g '=6.6V by figure,
therefore step 100 is proceeded to.
In the present embodiment, driving voltage first increases gradually with the speed of 0.05V/s in-0.2V-0.75V scope, then reduces gradually with the speed of 0.05V/s.The area that foam copper and platinum electrode stretch into solution is 0.1cm
2.
Should be understood that the present embodiment is only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Claims (10)
1. a saccharin sodium concentration detection apparatus, described saccharin sodium concentration detection apparatus is electrically connected with electrochemical workstation (1); It is characterized in that, comprise controller (2), storer (3), fill the container (4) of the upper end open of liquid, be located at the cover plate (5) on container, the alloy platinum material to downward-extension be located on cover plate make to electrode (7), embed the involute urve shape guide rail (6) of the lower ending opening of cover plate bottom, be located on guide rail can along the wheelwork of guide rail movement (8), the agitating device (9) being located at container bottom and the tap funnel (10) for instilling saccharin sodium solution in container be located on cover plate; Be connected with cover plate by the first motor (12) to electrode, guide rail one end is near the first motor, and the guide rail other end is near side edge thereof;
Described wheelwork bottom is provided with the working electrode (11) that foam copper material is made, and agitating device is connected with container bottom by waterproof machine (13); Working electrode and to electrode all in bar shaped tabular; Described controller is electrically connected with waterproof machine, storer, the first motor, wheelwork and electrochemical workstation respectively; Electrode and working electrode are electrically connected with electrochemical workstation respectively.
2. saccharin sodium concentration detection apparatus according to claim 1, is characterized in that, described guide rail comprises top board and is located at two baffle plates (16) of top board both sides, and two baffle plates are provided with corresponding guide openings; Described wheelwork comprises motor fixing seat (17), the second motor (18) be located in motor fixing seat, two gears (20) be connected respectively with two rotating shafts (19) of the second motor and two extension rods (21) be located at respectively on outside two gears, two extension rods stretch in two guide openings respectively;
The position corresponding with two gears, described guide rail bottom is provided with the track plates (15) of two upper surfaces with groove; Guide rail is provided with the dual-cavity (22) for coordinating with two gears, and two track plates two ends are all connected with guide rail, and described working electrode is connected with motor fixing seat; Described second motor is electrically connected with controller.
3. saccharin sodium concentration detection apparatus according to claim 1, it is characterized in that, described agitating device comprises the horizontal stirring pipe (14) be connected with the rotating shaft of waterproof machine, and horizontal stirring pipe is provided with some through holes (23) to being oppositely arranged; Horizontal stirring pipe is provided with several straight-bars vertical with the axial line of horizontal stirring pipe.
4. saccharin sodium concentration detection apparatus according to claim 3, is characterized in that, described straight-bar comprises longitudinal rod (24) and horizon bar (25).
5. the saccharin sodium concentration detection apparatus according to claim 1 or 2 or 3 or 4, it is characterized in that, cover plate and container are all rounded; Cover plate lower surface is provided with annular groove, and container upper end is inserted in annular groove and is connected with cover plate.
6. be applicable to a detection method for saccharin sodium concentration detection apparatus according to claim 1, it is characterized in that, comprise the steps:
(6-1) be provided with sweep interval A in controller, scanning times maximal value N, the initial value of scanning times sequence number i, i is 1;
The 0.1M NaOH getting 20 to 50ml inserts in container, cover plate is installed to container finish, makes working electrode and stretch in NaOH to electrode;
Electrochemical workstation exports the constant voltage of 0.40V to 0.6V to working electrode, regulates the piston filling the tap funnel of the saccharin sodium solution of 0.1M, makes the per interval A of tap funnel instill a saccharin sodium solution in container;
(6-2), extremely instill second saccharin sodium solution after tap funnel instills first saccharin sodium in container before, controller controls stirring apparatus to the liquid agitation time B in container, B < A by waterproof machine; Controller controls the first driven by motor and horizontally rotates electrode, control wheelwork drives working electrode to reciprocate along guide rail simultaneously, electrochemical workstation detects current density, when the current density detected reaches maximal value, controller controls wheelwork and the first motor quits work, and obtains the optimum position to electrode and working electrode;
Electrode is horizontally rotated and working electrode movement process in, maximum relative area is remained to electrode and working electrode;
Controller calculates the saccharin sodium concentration k in current container
1, by k
1and with k
1corresponding current density S (t) is stored in storer;
(6-3) tap funnel instills the i-th+1 saccharin sodium solution in container, and controller controls stirring apparatus to the liquid agitation time B in container, B < A by waterproof machine; Electrochemical workstation detects current density, and controller calculates the saccharin sodium concentration k in current container
i+1, by k
i+1and with k
i+1corresponding current density S (t) is stored in storer;
(6-4) as i≤N-1, make i value increase by 1, proceed to step (6-3); Otherwise, proceed to step (6-5);
(6-5) the N number of current density S (t) obtained is inputted second-order linear system accidental resonance model by controller respectively
In; And second-order linear system accidental resonance model is resonated;
Wherein, x (t) is the displacement of vibration particle, and Ω is angular frequency, r and ω is the attenuation coefficient of setting and the frequency of linear oscillator particle respectively, and c is the signal adjustment coefficient of setting, and b is the quadratic noise ξ of setting
2t the coefficient of (), ξ (t) is three discrimination noises, and { dismutation of noise follows Poisson distribution to ξ (t) ∈ for-a, 0, a}, a > 0, and its probability distribution is p
s(a)=p
s(-a)=q, p
s(0)=1-2q, wherein 0 < q < 0.5;
Noise average and correlativity follow < ξ (t) >=0, < ξ (t) ξ (t+ τ) >=2qa
2e
-λ τ;
Wherein λ is correlation ratio, and the flatness of three discriminations noise ξ (t) is
Controller utilizes formula
calculate and obtain the output signal-to-noise ratio SNR corresponding respectively with N number of current density S (t)
1, SNR
2..., SNR
n;
Controller reads the saccharin sodium concentration k in storer
1, k
2..., k
n; Controller utilizes point (k
1, SNR
1), (k
2, SNR
2) ..., (k
n, SNR
n) fit to straight line, draw saccharin sodium concentration prediction model according to the straight line of matching:
the liquid of container is poured out, and vessel cleaning is clean;
(6-6) detection of the saccharin sodium solution W of unknown concentration:
The saccharin sodium solution W of getting 20 to 50ml is inserted in container, cover plate is installed to container finish, makes working electrode and stretch in saccharin sodium solution electrode, and make working electrode and be positioned at step (6-2) determined optimum position to electrode; Electrochemical workstation exports the constant voltage of 0.40V to 0.6V to working electrode, and electrochemical workstation detects current density S (t), and S (t) inputs in second-order linear system accidental resonance model by controller,
And utilize formula
calculate and obtain output signal-to-noise ratio SNR, SNR is substituted into
obtain the concentration k of saccharin sodium solution W.
7. the detection method of saccharin sodium concentration detection apparatus according to claim 6, is characterized in that, also comprise alarm, alarm and controller electrical connection; Following electrode calibration step was also comprised before step (6-1):
(7-1) the 0.1M NaOH getting 30 to 48ml inserts in the first beaker, by working electrode and insert in the NaOH solution of the first beaker to electrode, electrochemical workstation is utilized to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, reduce gradually again, obtaining horizontal ordinate is driving voltage, and ordinate is the curve of current density, the difference g between the maximal value of calculating current density and minimum value;
(7-2) get 0.1M NaOH and 0.1mM saccharin sodium successively and to insert in the second beaker according to the ratio of 3: 2 and to stir, by working electrode and insert in the solution of the second beaker to electrode, electrochemical workstation is utilized to carry out cyclic voltammetry scanning, the driving voltage of working electrode is first increased gradually in-0.2V-0.75V scope, reduce gradually again, obtaining horizontal ordinate is driving voltage, ordinate is the curve of current density, the difference g ' between the maximal value of calculating current density and minimum value;
(7-3) controller utilizes
the error of calculation, when e≤4.7%, proceeds to step (6-1);
Otherwise controller controls alarm equipment alarm, operating personnel are to electrode being carried out to surface treatment or changing electrode; Return step (7-1).
8. the detection method of saccharin sodium concentration detection apparatus according to claim 7, is characterized in that, driving voltage first increases gradually with the speed of 0.05V/s in-0.2V-0.75V scope, then reduces gradually with the speed of 0.05V/s.
9. the detection method of saccharin sodium concentration detection apparatus according to claim 7, is characterized in that, the area that foam copper and platinum electrode stretch into solution is 0.085cm
2to 0.135cm
2.
10. the detection method of the saccharin sodium concentration detection apparatus according to claim 6 or 7 or 8 or 9, it is characterized in that, A is 42 to 58 seconds, and N is 10 to 108, B is 9 to 30 seconds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410502330.0A CN104458878B (en) | 2014-09-26 | 2014-09-26 | Saccharin sodium concentration detection device and saccharin sodium concentration detection method |
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| CN103528877A (en) * | 2013-10-25 | 2014-01-22 | 江南大学 | On-line sugar concentration detection system for small-scale biochemical reactor |
| CN104458876A (en) * | 2014-09-26 | 2015-03-25 | 浙江工商大学 | Device and method for detecting concentration of L-rhamnose solution |
| CN104569110A (en) * | 2013-10-27 | 2015-04-29 | 中国石油化工集团公司 | Device for measuring ion concentration of drilling fluid |
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| CN2384221Y (en) * | 1999-06-25 | 2000-06-21 | 中山大学 | Multifunctional microcomputerized automatic titrator |
| JP2007171119A (en) * | 2005-12-26 | 2007-07-05 | Nikka Micron Kk | Sensor for detecting concentration of aqueous ozone solution |
| JP2013044712A (en) * | 2011-08-26 | 2013-03-04 | Jfe Steel Corp | Method for measuring amount of hydrogen penetrated into metal and method for monitoring amount of hydrogen penetrated into metal portion of moving body |
| CN103257172A (en) * | 2012-10-09 | 2013-08-21 | 武汉华科新材料有限公司 | Limestone activity determination and detection apparatus |
| CN203011903U (en) * | 2012-12-20 | 2013-06-19 | 王克超 | Multifunctional intelligent titration machine |
| CN103528877A (en) * | 2013-10-25 | 2014-01-22 | 江南大学 | On-line sugar concentration detection system for small-scale biochemical reactor |
| CN104569110A (en) * | 2013-10-27 | 2015-04-29 | 中国石油化工集团公司 | Device for measuring ion concentration of drilling fluid |
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