CN101694471A - Drinking water COD online automatic detection method and detection instrument - Google Patents
Drinking water COD online automatic detection method and detection instrument Download PDFInfo
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- CN101694471A CN101694471A CN200910217740A CN200910217740A CN101694471A CN 101694471 A CN101694471 A CN 101694471A CN 200910217740 A CN200910217740 A CN 200910217740A CN 200910217740 A CN200910217740 A CN 200910217740A CN 101694471 A CN101694471 A CN 101694471A
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Abstract
The invention relates to a drinking water COD online automatic detection method and a detection instrument. The detection instrument is characterized by comprising a water sample quantitative injection device, a reagent and a standard sample quantitative injection device, a combined COD detector, a waste liquor discharging device and a meter circuit, the combined COD detector integrates water sample, the reagent, standard sample quantitative mixing, heating and controlling, stirring, dissolving, titrating, detecting and washing functions into a whole, and the detection instrument has compact structure and complete functions. The drinking water COD online automatic detection method not only retains scientific cores applied to laboratorial drinking water COD national standard inspection method GB/T 5707.7-2006, but also solves key problems which must be solved when the laboratorial national standard inspection method is applied to online detection. Further, the method is simple, convenient, reliable, scientific and reasonable, provides solid technique support for the drinking water COD online automatic detection instrument. The detection instrument has the advantages of accurate measurement, reliable operation, little maintenance and the like.
Description
Technical field
The present invention relates to a kind of drinking water COD online automatic detection method and detector.
Background technology
The importance of the water quality of Drinking Water and people's health relation more and more is people's understanding, wherein potable water by the overall target-chemical oxygen consumption (COC) of organic pollutants degree (COD) to list the important indicator of national management department monitoring drinking water quality in, and the method that COD is detected in the laboratory, that is: GB/T 5750.7-2006 have been formulated.But being suitable in the drinking water COD online automatic detection, the method for existing GB/T 5750.7-2006 laboratory detection COD do not use.For the COD of better monitoring potable water, in time monitor the waterworks quality of water supply continuously, prevent that defective water from using for the user, pressing for provides drinking water COD online automatic detection method and detector.
At present, the potable water online automatic detection instrument that is used for of existing lower range such as some developed countries such as U.S. HACH company, KORBA company of Korea S, Japanese HORIBA company uses for the user.China does not still have a kind of online automatic detection instrument that meets national test stone (GB/T 5750.7-2006) method, demestic user's dependence on import, the general analytical instrument factory of analysing in nearest domestic Beijing copies Japan, develop COD online automatic detection instrument according to the UVA principle, this potable water COD online automatic detection instrument is in Japan, Europe is not because of needing reagent, the fast grade of measuring speed obtains using comparatively widely, but because of the different types of organic ultraviolet absorptivity difference that exists in the potable water, form reasons such as variation, accuracy and comparability that influence is measured to measuring different water bodys or same water body.So do not become a kind of standard method and the reference instrument of this state or this area always.
Summary of the invention
The objective of the invention is, provide a kind of method easy, reliable, scientific and reasonable drinking water COD online automatic detection method.
Another object of the present invention is, provides a kind of and matches with this method, measures accurately, and is reliable, the drinking water COD online automatic detection instrument that maintenance is few.
Realize that the technical scheme that purpose of the present invention adopts is, a kind of drinking water COD online automatic detection method is characterized in that, it comprises following content:
(a) the breadboard drinking water COD national standard of adopting by equivalent method of inspection GB/T5707.7-2006, be that measuring principle is under uniform temperature and acid condition, potassium permanganate with in the water based on the reducing substances oxidation of organism, the remaining potassium permanganate of sodium oxalate titration, determine in the water to calculate content based on the reducing substances of organism by the consumption of accurate mensuration titration process mesoxalic acid sodium based on the reducing substances oxygen utilization of organic substance;
(B) in every detection one-period, a small amount of sodium oxalate solution and M
nO
2M is eliminated in reaction
nO
2Pollution;
(c) the drop reaction terminal point determining is that dynamic process is judged, dynamic process judges it is according to titration during near terminal point, and light receiving element is accepted light intensity and changed and be tending towards constant and judge.
Realize that the technical scheme that another object of the present invention adopted is, a kind of drinking water COD online automatic detection instrument that matches with this method, it is characterized in that, it comprises the quantitative injection device 1 of water sample, reagent, the quantitative injection device 2 of standard specimen, combined type COD detecting device 3, waste liquid discharge device 4 and appliance circuit 5, the structure of the quantitative injection device 1 of described water sample is, comprises that water sample valve 8 is connected with overflow cup 7 by water sample filtrator 6, overflow cup 7 with measure sample valve 9 and be connected; The structure of described reagent, the quantitative injection device 2 of standard specimen is, comprise that liquor potassic permanganate kit 31 is connected with liquor potassic permanganate volume pump 32, sodium oxalate solution kit 33 is connected with sodium oxalate solution volume pump 34, sulfuric acid solution kit 35 is connected with sulfuric acid solution metering valve 36, and sodium oxalate solution standard specimen box 37 is connected with standard specimen solution metering valve 38; The structure of described combined type COD detecting device 3 is, comprise reaction cup carriage 14, be built-in with reaction cup 11 at reaction cup carriage 14, cup 13 upper sheds place of reaction cup 11 are equipped with bowl cover 12, the electrically heated rod outer tube 16 that cup 13 is provided with is built-in with electrically heated rod 15, the temperature element outer tube 18 that cup 13 is provided with is built-in with temperature element 17, bottom in cup 13 is equipped with magnetic stir bar 22, be built-in with the stirring motor 23 that is connected with magnetic stir bar 22 magnetic at the reaction cup carriage 14 that is positioned at cup 13 bottoms, in reaction cup carriage 14, and the both sides of cup 13 are oppositely arranged light-emitting component 24 respectively relatively, light receiving element 25; The structure of described waste liquid discharge device 4 is to comprise waste discharge slot 26; The metering sample valve 9 of the quantitative injection device 1 of water sample is connected with the reaction cup 11 of combined type COD detecting device 3; The liquor potassic permanganate volume pump 32 of reagent, the quantitative injection device 2 of standard specimen, sodium oxalate solution volume pump 34, sulfuric acid solution metering valve 36 and standard specimen solution metering valve 38 are connected with the reaction cup 11 of combined type COD detecting device 3 respectively; The reaction cup 11 of combined type COD detecting device 3 is connected with the waste discharge slot 26 of waste liquid discharge device 4 by waste valve 10.
Drinking water COD online automatic detection method of the present invention, not only kept the science kernel that is used for breadboard drinking water COD national standard method of inspection GB/T 5707.7-2006, and solved the key issue that must solve when this laboratory standard method of inspection refers to online the detection, its method is easy, reliable, scientific and reasonable, for drinking water COD online automatic detection instrument provides solid technical support.
The combined type COD detecting device of drinking water COD online automatic detection instrument of the present invention catchments that sample, reagent, standard specimen quantitatively mix, heat and control, stir, clear up, titration, detection, cleaning function be in one, its compact conformation, function are complete, and can be indeformable under high temperature, jump in temperature, strong oxidizer etching condition, do not damage; Reaction cup double as optical window has been simplified the structure of light path, has prevented to take place in the long-term on-line measurement process seepage and the corrosion of optical window seal member, long service life.Have and measure advantages such as accurate, reliable, that maintenance is few.
Description of drawings
Fig. 1 is a drinking water COD online automatic detection instrument structural representation.
Fig. 2 is combined type COD detecting device 3 structure cross-sectional schematic.
Fig. 3 is reaction cup 11 structure cross-sectional schematic.
Fig. 4 appliance circuit 5 functional-block diagrams.
Fig. 5 control Driver Circuit 55 schematic diagrams.
Fig. 6 analogue amplifier 53 schematic diagrams.
Fig. 7 I/O interface circuit 52 schematic diagrams.
Among the figure: the quantitative injection device of 1 water sample, 2 reagent, the quantitative injection device of standard specimen, 3 combined type COD detecting devices, 4 waste liquid discharge devices, 5 appliance circuits, 6 filtrators, 7 overflow cups, 8 water sample valves, 9 metering sample valves, 10 waste valves, 11 reaction cup, 12 bowl covers, 13 cups, 14 reaction cup carriages, 15 electrically heated rods, 16 electrically heated rod outer tubes, 17 temperature elements, 18 temperature element outer tubes, 19 water samples connect to be chewed, and 20 overflows connect chews, and 21 waste discharges connect chews, 22 magnetic stir bars, 23 stirring motors, 24 light-emitting components, 25 light receiving elements, 26 waste discharge slots, 31 liquor potassic permanganate kits, 32 liquor potassic permanganate volume pumps, 33 oxalic acid solution kits, 34 oxalic acid solution volume pumps, 35 sulfuric acid solution kits, 36 sulfuric acid solution metering valves, 37 standard specimen solution boxes, 38 standard specimen solution metering valves, 50A/D converter, 51 single chip circuits, the 52I/O interface circuit, 53 analogue amplifiers, 54 sequential control circuits, 55 control Driver Circuit.
Embodiment
Utilize drawings and Examples that the present invention is further described below.
Drinking water COD online automatic detection method, it comprises following content:
(1) the breadboard drinking water COD national standard of adopting by equivalent method of inspection GB/T5707.7-2006, be that measuring principle is under uniform temperature and acid condition, potassium permanganate with in the water based on the reducing substances oxidation of organism, the remaining potassium permanganate of sodium oxalate titration, determine in the water to calculate content based on the reducing substances of organism by the consumption of accurate mensuration titration process mesoxalic acid sodium based on the reducing substances oxygen utilization of organic substance.
(2) in every detection one-period, a small amount of sodium oxalate solution and M
nO
2M is eliminated in reaction
nO
2Pollution.
(3) the drop reaction terminal point determining is that dynamic process is judged, dynamic process judges it is according to titration during near terminal point, and light receiving element is accepted light intensity and changed and be tending towards constant and judge.
Be after with a certain amount of potassium permanganate of finite concentration reducing substanceses such as organism in a certain amount of water sample being cleared up in described adopting by equivalent laboratory standard GB/T 5707.7-2006 method of inspection, remaining potassium permanganate and certain density a certain amount of sodium oxalate reaction, use the titration of potassium permanganate visual colorimetry again, determine the amount of excessive sodium oxalate, determine the oxygen utilization of sample water at last.Be the oxygen utilization of directly determining water sample with sodium oxalate titration potassium permanganate surplus among the present invention, this method has been simplified analytical procedure, helps online making at detecting instrument, kept the content of core in the analysis principle simultaneously.
Described in every detection one-period, a small amount of sodium oxalate solution and M
nO
2M is eliminated in reaction
nO
2Pollution, when thoroughly having solved on-line automatic analysis, clearing up, in the titration process, producing black pollution thing M
nO
2On the optical window attached to reaction cup, have a strong impact on testing result, even can't carry out, general every detection three, five all after dates will be used the concentrated hydrochloric acid clean contaminants, have not only consumed the concentrated hydrochloric acid cleaning fluid, and have caused the problem to severe environmental pollution.
Described drop reaction terminal point determining is that dynamic process is judged, dynamic process judges it is according to titration during near terminal point, light receiving element is accepted light intensity and is changed and to be tending towards constant and to judge, in standard GB/T 5707.7-2006 method of inspection is to judge titration end-point with visual colorimetric determination, human factor can cause the error of assay, and method dynamic process of the present invention judges it is according to titration during near terminal point, light receiving element is accepted light intensity and is changed and to be tending towards constant and to judge, this method can be considered external environment condition in the time of short duration constant, it is not affected by environment that judged result can be thought, improved the accuracy of testing result greatly.
With reference to Fig. 1-3, the drinking water COD online automatic detection instrument that matches with the inventive method, it comprises the quantitative injection device 1 of water sample, reagent, standard specimen quantitative injection device 2, combined type COD detecting device 3, waste liquid discharge device 4 and appliance circuit 5.The structure of the quantitative injection device 1 of described water sample is, comprises that water sample valve 8 is connected with overflow cup 7 by water sample filtrator 6, overflow cup 7 with measure sample valve 9 and be connected.The structure of described reagent, the quantitative injection device 2 of standard specimen is, comprise that liquor potassic permanganate kit 31 is connected with liquor potassic permanganate volume pump 32, sodium oxalate solution kit 33 is connected with sodium oxalate solution volume pump 34, sulfuric acid solution kit 35 is connected with sulfuric acid solution metering valve 36, and sodium oxalate solution standard specimen box 37 is connected with standard specimen solution metering valve 38.The structure of described combined type COD detecting device 3 is, comprise reaction cup carriage 14, be built-in with reaction cup 11 at reaction cup carriage 14, cup 13 upper sheds place of reaction cup 11 are equipped with bowl cover 12, the electrically heated rod outer tube 16 that cup 13 is provided with is built-in with electrically heated rod 15, the temperature element outer tube 18 that cup 13 is provided with is equipped with temperature element 17, bottom in cup 13 is equipped with magnetic stir bar 22, be built-in with the stirring motor 23 that is connected with magnetic stir bar 22 magnetic at the reaction cup carriage 14 that is positioned at cup 13 bottoms, in reaction cup carriage 14, and the both sides of cup 13 are oppositely arranged light-emitting component 24 respectively relatively, light receiving element 25.The structure of described waste liquid discharge device 4 is to comprise waste discharge slot 26.The reaction cup 11 of the metering sample valve 9 of the quantitative injection device 1 of water sample and combined type COD detecting device 3 connects by the water sample on the reaction cup and chews 19 and be connected.The liquor potassic permanganate volume pump 32 of reagent, the quantitative injection device 2 of standard specimen, sodium oxalate solution volume pump 34, sulfuric acid solution metering valve 36 and standard specimen solution metering valve 38 are connected by four ascending pipes on the bowl cover 12 with the reaction cup 11 of combined type COD detecting device 3 respectively.The waste discharge that the reaction cup 11 of combined type COD detecting device 3 is provided with by its bottom connects chews 21 and is connected with waste valve 10, and waste valve 10 is connected with the waste discharge slot 26 of waste liquid discharge device 4.Being equipped with overflow on the reaction cup 11 connects and chews 20.
In the combined type COD detecting device 3, reaction cup 11 double as optical windows, saved and established required retaining element of optical window and encapsulant in addition, solution seepage and corrosion phenomenon can not take place in this incorporate optical window in the rugged surroundings of violent temperature variation and deep-etching, become non-maintaining parts.
The mixing that the magnetic stir bar 22 of the bottom in stirring motor 23 and the reaction cup 11 is finished jointly to solution in the reaction cup 11 stirs.
Waste liquid after solution is finished the titration end-point judgement and polluted cleaning in the reaction cup 11 is discharged after waste discharge solenoid valve 10 enters waste discharge slot 26, and the overflow of overflow in the overflow cup 7 and reaction cup 11 all flows into waste discharge slot 26 and discharges.
With reference to Fig. 4, appliance circuit 5 is a prior art, comprises A/D converter 50, single chip circuit 51, I/O interface circuit 52, analogue amplifier 53, sequential control circuit 54 and control Driver Circuit 55.Appliance circuit 5 used components and parts are the commercially available prod.In the appliance circuit 5, it is core devices that single chip circuit 51 adopts the C8051F020 single-chip microcomputer based on Cygnal, and the C8051F020 single-chip microcomputer has 64 digital I/O pins, 12, the 8 passage ADC of 100ksps.Under the control of C8051F020 monolithic, potable water COD online automatic detection instrument of the present invention is according to sequential control circuit 54 certain time sequence control Driver Circuit 55, the quantitative injection device 1 of water sample and reagent, the quantitative injection device 2 of standard specimen are operated, and the metering valve and the orderly action of volume pump that drive separately add water sample and reagent, standard specimen respectively.Carry out chemical reaction in combined type COD detecting device 3, finish the conversion of light signal to electric signal, electrical signal converted is carried out signal Processing through analogue amplifier 53, analyzes through the A/D converter 50 of single-chip microcomputer.Liquid after the analysis discharges through waste liquid discharge device 4.I/O interface circuit 52 comprises the keyboard operation of man-machine exchange, the output of alerting signal and the demonstration of instrument etc.
With reference to Figure 4 and 5, control Driver Circuit 55 mainly is that metering valve and volume pump are controlled, wherein the control device of metering valve adopts the optical relay AQY212GH of NAIS company, this relay has that volume is little, the life-span is long, contactless, antijamming capability is strong, insulation between output and the input, advantages such as one-way transmission signal.Guaranteed to measure each time the accurate injection of water sample and reagent, standard specimen.The unlatching of volume pump is controlled by the switching signal of relay.
With reference to Fig. 4 and 6, the photoelectric cell received current signal of analogue amplifier 53 becomes positive voltage signal behind this signal process I/V conversion and the inverting amplifier, enters Chip Microcomputer A/D converter 50 and handles.
With reference to Fig. 4 and 7, comprise the keyboard operation of man-machine exchange, the output of alerting signal and the demonstration of instrument in the I/O interface circuit 52.Wherein: the exchange of keyboard operation responsible official machine information, software comprise that keyboard goes to tremble function etc.Alerting signal is exported by relay, for the user provides the normally opened relay contact point signal.Advantages such as the M320240-14A3-E display that display adopts TRULY company to produce, this product have that volume is little, power consumptive province, life-span length, no ray, antidetonation are explosion-proof.This display can show many data messages simultaneously, as measured value, history curve, alarm condition, electric current output, temperature, time etc., can satisfy the needs of different user.
The course of work of drinking water COD online automatic detection instrument is as follows: the quantitative injection device 1 of water sample is that sampling device is injected in the controlled timing of constant pressure type, quantitative water sample accurately is injected in the reaction cup 11 of combined type COD detecting device 3; Reagent, the quantitative injection device 2 of standard specimen are injected into a certain amount of liquor potassic permanganate in the liquor potassic permanganate kit 31 in the reaction cup 11 by liquor potassic permanganate volume pump 32; A certain amount of concentrated sulfuric acid solution in the sulfuric acid solution kit 35 is injected reaction cup 11 by sulfuric acid solution metering valve 36, above-mentioned two kinds of reagent and water sample stir abundant mixing through the magnetic stir bar 22 that stirring motor 23 drives, electrically heated rod 15 heating simultaneously, temperature element 17 is delivered to appliance circuit 5 with temperature signal, and constant temperature is cleared up half an hour for 100 ℃ under its control, then appliance circuit 5 drives sodium oxalate solution volume pump 34, reaction cup 11 is injected in sodium oxalate solution titration in the sodium oxalate solution kit 33, the magnetic stir bar 22 that stirring motor 23 drives does not stop to stir, drop reaction carries out fully rapidly, in the whole process by the absorbance of sample liquid by the light-emitting component 24 of combined type COD detecting device 3, light receiving element 25 is monitored.When titration end-point arrives, under appliance circuit 5 controls, end titration, the sodium oxalate solution amount that the single-chip microcomputer metering titration process of single chip circuit 51 consumes, calculate the COD value of corresponding water sample, and on display screen, show, surpass the setting value output alarm signal and report to the police.
For preventing at the M that clears up, potassium permanganate decomposites in the sample in the titration process
nO
2Pollute reaction cup 11, particularly cup 13 double as optical window positions, after finishing titration process, under appliance circuit 5 controls, sodium oxalate solution volume pump 34 continues to inject to reaction cup 11 M of the sample of sodium oxalate solution and reaction cup 11
nO
2Reaction is up to eliminating M
nO
2Pollute and end.After finishing said process, waste valves 10 are opened in appliance circuit 5 control, close waste valve 10 after finishing waste discharge, reenter next cycle detection.
Timing signal, standard specimen solution metering valve 38 substitutes water sample with the sodium oxalate solution standard specimen in the sodium oxalate solution standard specimen box 37 and quantitatively is injected in the reaction cup 11, and the similar measuring process of following process is finished calibrating procedure under appliance circuit 5 controls.
Drinking water COD online automatic detection instrument of the present invention is in waterworks, Songjiang, Shanghai site test examination operation.Table 1 is the data table of comparisons of the laboratory of drinking water COD online automatic detection instrument actual measurement COD data and waterworks, Songjiang, Shanghai according to national standard (GB/T 5750.7-2006) actual measurement.
Table 1: laboratory, waterworks, Songjiang, Shanghai and Guangda Power Equipment LLC, Jilin City online COD table measured value (mg/L)
Data shown in the table 1 show the method for inspection of employing laboratory, laboratory, waterworks, Songjiang, Shanghai standard GB/T 5707.7-2006, the data of desk checking and Guangda Power Equipment LLC, Jilin City according to the present invention potable water COD on-line detector measured value (except that waterworks manual analysis on May 6 as a result the kick reason unclear) to compare be quite to meet, its maximum absolute error is in 0.5mg/L.Purpose of the present invention and technique effect have been realized.
Claims (5)
1. a drinking water COD online automatic detection method is characterized in that, it comprises following content:
(a) the breadboard drinking water COD national standard of adopting by equivalent method of inspection GB/T5707.7-2006, be that measuring principle is under uniform temperature and acid condition, potassium permanganate with in the water based on the reducing substances oxidation of organism, the remaining potassium permanganate of sodium oxalate titration, determining in the water content based on the reducing substances of organism by the consumption of accurate mensuration titration process mesoxalic acid sodium, is that main reducing substances oxygen utilization is calculated with organic substance;
(B) in every detection one-period, a small amount of sodium oxalate solution and M
nO
2M is eliminated in reaction
nO
2Pollution;
(c) the drop reaction terminal point determining is that dynamic process is judged, dynamic process judges it is according to titration during near terminal point, and light receiving element is accepted light intensity and changed and be tending towards constant and judge.
2. drinking water COD online automatic detection instrument that matches with this method, it is characterized in that, it comprises the quantitative injection device of water sample (1), reagent, the quantitative injection device of standard specimen (2), combined type COD detecting device (3), waste liquid discharge device (4) and appliance circuit (5), the structure of the quantitative injection device of described water sample (1) is, comprise that water sample valve (8) is connected with overflow cup (7) by water sample filtrator (6), overflow cup (7) is connected with metering sample valve (9); The structure of described reagent, the quantitative injection device of standard specimen (2) is, comprise that liquor potassic permanganate kit (31) is connected with liquor potassic permanganate volume pump (32), sodium oxalate solution kit (33) is connected with sodium oxalate solution volume pump (34), sulfuric acid solution kit (35) is connected with sulfuric acid solution metering valve (36), and sodium oxalate solution standard specimen box (37) is connected with standard specimen solution metering valve (38); The structure of described combined type COD detecting device (3) is, comprise reaction cup carriage (14), be built-in with reaction cup (11) at reaction cup carriage (14), cup (13) upper shed place of reaction cup (11) is equipped with bowl cover (12), the electrically heated rod outer tube (16) that cup (13) is provided with is built-in with electrically heated rod (15), the temperature element outer tube (18) that cup (13) is provided with is built-in with temperature element (17), bottom in cup (13) is equipped with magnetic stir bar (22), be built-in with the stirring motor (23) that is connected with magnetic stir bar (22) magnetic at the reaction cup carriage (14) that is positioned at cup (13) bottom, in reaction cup carriage (14), and the both sides of cup (13) are oppositely arranged light-emitting component (24) respectively relatively, light receiving element (25); The structure of described waste liquid discharge device (4) is to comprise waste discharge slot (26); The metering sample valve (9) of the quantitative injection device of water sample (1) is connected with the reaction cup (11) of combined type COD detecting device (3); The liquor potassic permanganate volume pump (32) of reagent, the quantitative injection device of standard specimen (2), sodium oxalate solution volume pump (34), sulfuric acid solution metering valve (36) and standard specimen solution metering valve (38) are connected with the reaction cup (11) of combined type COD detecting device (3) respectively; The reaction cup (11) of combined type COD detecting device (3) is connected with the waste discharge slot (26) of waste liquid discharge device (4) by waste valve (10).
3. drinking water COD online automatic detection instrument according to claim 2 is characterized in that described temperature element (17) is a platinum resistance.
4. drinking water COD online automatic detection instrument according to claim 2 is characterized in that described light-emitting component (24) is a luminotron.
5. drinking water COD online automatic detection instrument according to claim 2 is characterized in that described light receiving element (25) is a photoelectric cell.
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