CN1110703C - Automatic analyzer of chemically needed oxygen quantity for full digestion and its application method - Google Patents
Automatic analyzer of chemically needed oxygen quantity for full digestion and its application method Download PDFInfo
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- CN1110703C CN1110703C CN 99122502 CN99122502A CN1110703C CN 1110703 C CN1110703 C CN 1110703C CN 99122502 CN99122502 CN 99122502 CN 99122502 A CN99122502 A CN 99122502A CN 1110703 C CN1110703 C CN 1110703C
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Abstract
The present invention relates to a full-counteraction automatic analyzer for chemical oxygen demand (COD) and an application method thereof. The present invention has the technical scheme that a plurality of reflux cooling tubes and reaction cups corresponding to the reflux cooling tubes are arranged in a reflux counteracting device in parallel, a constant temperature heating device is arranged at the lower part of the reaction cup, and the reflux cooling tubes are connected with a water tank which is provided with a refrigerator element. In addition, an automatic analysis and detection device is provided with a capacitance cell, the upper end and the lower end of the capacitance cell are provided with a dropping liquid electromagnetic valve and a titration valve, and the present invention is also provided with a sample self-care system which is composed of a microcomputer, and a miniature printer and a digital display which are connected with the microcomputer. The analyzer can adopt two analytical methods. The full-digestion automatic analyzer has the advantages of capability of carrying out cold titration, difficult pollution of electrodes, high automation, high precision, high speed, and simple and convenient operation.
Description
Technical field
The present invention relates to a kind of electrochemical analytical instrument, particularly a kind of hydrochemistry oxygen demand oxidation-reduction potential automatic analyzer.
Background technology
Hydrochemistry oxygen demand analytical equipment still follows making power consumption formula coulometric titration ceremony digestion device now both at home and abroad, and the former is in the boiling electrolysis, and electrode easily stains, and no longer advocates and uses; And most manufacturers produce digestion devices keep away unavoidably to collapse and spatter phenomenon, and COD is lost, and it and spectrophotometer coupling exist detected solution repeatedly to shift, and are subjected to time and Temperature Influence between chromophore and the auxochrome.Reduce the accuracy of analyzing.
Summary of the invention
The purpose of this invention is to provide a kind of automatic analyzer of chemically needed oxygen quantity for full digestion, carry out cold titration, electrode is difficult for being stain, and the automaticity height is accurately fast, easy and simple to handle.
The object of the present invention is achieved like this: its instrument comprises the backflow digestion device that has the backflow cooling tube, the automatic analysis and detection device that is connected with the analyzing and testing circuit and the sample self-care system that is made of microcomputer and the miniprinter that is attached thereto and digital indicator, it is characterized in that: be set up in parallel several Zhi Huiliu cooling tubes and corresponding with it reaction cup in the housing of backflow digestion device; The reaction cup bottom is provided with constant temperature heating device; The water tank of each cooling tube connecting band water pump that refluxes is equipped with semiconductor cooler on the water tank; Automatically in the analysis and detection device tubular capacitance pool is set, the outside surface set metal light wall pipe of tubular capacitance pool loads platinum filament on the tubular cavity central axial line of capacitance pool; The metal light wall pipe is drawn the lead that is connected automatic analyzing and testing circuit respectively with platinum filament; The capacitance pool top is provided with the solenoid valve of band dripping hole, and solenoid valve is communicated with reservoir; The titration valve of capacitance pool lower end connecting band titration mouth; Electrode assemblie lifting pivot is set between capacitance pool and reaction cup; The stirrer that is driven by stirring motor is arranged in the reaction cup.
Utilizing above-mentioned instrument to carry out water quality clears up the COD analytical work entirely and has following two kinds of methods:
Method 1: routine analyzer comprises the preparation oxygenant, adds acid, clears up with titration etc., and its main technical points is: adopt potassium dichromate method preparation oxygenant, its concentration is 0.125N, contains 0.1 milliliter of concentrated sulphuric acid in one milliliter of oxygenant, contains 0.01 gram mercuric sulfate; Blank sample reaction cup and each detected water sample reaction cup add 1 milliliter in 10 milliliters in blank water and oxygenant respectively; Respectively add 1 milliliter of detected water sample in the detected water sample reaction cup; By the concentration ratio preparation digestion solution that contains 0.09 gram silver sulfate in 10 milliliters of concentrated sulphuric acids, blank sample reaction cup and each detected water sample reaction cup add 10 milliliters of digestion solutions respectively; Cleared up 10 minutes, mend then and add water to 75 milliliters, carry out titration, blank sample and each detected water sample are successively placed respectively on the automatic analyzing and testing device, fill with ferrous titrant then in capacitance pool, stir by stirrer, display shows initial potential, displacement variable by titrant in the capacitance pool demonstrates the terminal point current potential at last, and the demonstration of terminal point current potential shows the COD value of water sample after moment.
Method 2: routine analyzer comprises the preparation oxygenant, clear up with titration etc., and its technical scheme main points are: adopt permanganimetric method preparation oxygenant, its concentration is 0.025N; Blank sample reaction cup and each detected water sample reaction cup add 1 milliliter in 10 milliliters in blank water and oxygenant respectively; Respectively add 1 milliliter of detected water sample in the detected water sample reaction cup, and in each reaction cup 10 milliliters of power mouth 225% concentration dilute sulfuric acids, place and clear up cup, cleared up 5 minutes, add water to 75 milliliters again and carry out titration, blank sample and each detected water sample are successively placed respectively on the automatic analyzing and testing device, in capacitance pool, fill with ferrous titrant again, stir by stirrer, display shows initial potential, displacement variable by titrant in the capacitance pool causes indicator electrode current potential generation hop with the working battery of accepting mutually with it at last, shows the terminal point current potential, and the demonstration of terminal point current potential demonstrates the COD value of water sample after moment.
Advantage of the present invention is: carry out cold titration, electrode is difficult for being stain the automaticity height.Accurately fast, easy and simple to handle.
Description of drawings
Fig. 1 is the Facad structure synoptic diagram of backflow digestion device.
Fig. 2 is a backflow cooling tube synoptic diagram.
Fig. 3 is the rear view of Fig. 1.
Fig. 4 is the structural representation of automatic analyzing and testing part and sample self-care part.
Fig. 5 is the capacitance pool structural representation.
Fig. 6 is circuit theory diagrams
Embodiment
Embodiment 1
Analyser provided by the invention is made up of three parts, and the digestion device that wherein refluxes is an autonomous device, and analyzing and testing part and sample are taken care of oneself and partly be combined into a device automatically.Their concrete structure is as follows:
See Fig. 1-3, four backflow cooling tubes 3 of fixing side by side assembling in the housing 1 of backflow digestion device, the import of backflow cooling tube 3 is connected supply mains 13 and return main 12 with outlet by latex flexible pipe 2 with divider 14, last supply mains 13 is connected the water pump 9 that is arranged in the water tank 10 with return main 12.Conductor refrigeration parts 11 are installed on the tank lid.Reaction cup 8,4,5,6 is cleared up in four of the corresponding placements in the bottom of four backflow cooling tubes 3, and the bottom correspondence of table top is cleared up reaction cup electric heating tubular heater 7 is set.The table top side is provided with the control button.
See Fig. 4,5,6, automatically housing 25 tops of analysis and detection device are provided with reservoir 20, reservoir 20 connects by woven hose and adds liquid electromagnetic valve 21, it is suitable for reading that the liquid feeding mouth of solenoid valve 21 is aimed at the capacitance pool buret 22 that is assembled in the housing, electric capacity dropping liquid fixed tube 22 is fixed on the fixed support 31, the outside suit metal foil pipe 32 of tubular capacitance pool buret 22, load platinum filament 33 on the tubular cavity central axial line of capacitance pool, metal light wall pipe 32 and platinum filament 33 are drawn lead A, B respectively, two lead A, the external testing circuit of B.Titration valve 19 lower ends that are connected with the capacitance pool buret are provided with titration mouth 18.Reaction cup 8 is placed on the table top, is positioned at the below of titration valve titration mouth 18.The bipolar electrode that is made of platinum electrode 27 and mercurous chloride electrode 28 is assembled on the crane 31; Crane 31 thread connection the band spiral elevating lever 26 on, elevating lever 26 driving coupling drive motor 24, along with the commentaries on classics anyway of elevating lever 26, two electrodes rise under the drive of crane 31 or fall.Place the stirrer 17 of a magnetism stick in the reaction cup 8.In the bottom of table top stirring motor 16 is installed, when the rotor of stirring motor 16 rotated, stirrer 17 also rotated under it attracts, thereby produced beating action.The microcomputer 30 of sample self-care part and printer 15 are contained in the bottom in the housing 25, and housing is provided with operating key 29 outward.Digital display device 23 is contained in the top in the housing 25.
Analytical approach 1: at first adopt potassium dichromate method preparation oxygenant.The potassium dichromates of 6.125 grams are dissolved in 500 milliliters the water, mercuric sulfate with 10 grams dissolves in 100 milliliters of concentrated sulphuric acids simultaneously, join after cooling in the potassium dichromate oxidation agent, in 1000 milliliters of volumetric flasks, dilute under 25 ℃ with water, solution is 0.125N, takes the chromium legal system to be equipped with the catalysis digestion solution then; 10 gram silver sulfates are dissolved in 1000 milliliters of sulfuric acid.
And then three kinds of reaction cup that detected water sample is housed are placed respectively on the automatic analysis and detection instrument, to be undertaken by said procedure, stoichiometric point shows the CODmgL of O2
-1Value is pressed printing key, prints the analysis result of quoting three kinds of detected water sample automatically.
Analytical approach 2: at first adopt potassium permanganate preparation oxygenant, 1.2 gram potassium permanganate are dissolved in 1.2 premium on currency, PROCESS FOR TREATMENT just is 0.025N through demarcating routinely.Reaction cup 8,4,5,6 is injected 10 milliliters in 1 milliliter in oxygenant and blank water respectively, and reaction cup 4,5,6 is injected 1 milliliter of three kinds of detected water sample respectively.Respectively inject 10 milliliters of 25% concentration dilute sulfuric acids then in four reaction cup, cleared up 5 minutes, add water to 75 milliliters again and carry out titration, the following analysis process is sketched with embodiment 1.
Claims (3)
1, a kind of automatic analyzer of chemically needed oxygen quantity for full digestion, comprise the backflow digestion device that has backflow cooling tube (3), the automatic analysis and detection device that is connected with the analyzing and testing circuit and the sample self-care system that constitutes by microcomputer (30) and the miniprinter (15) that is attached thereto and digital indicator (23), it is characterized in that: be set up in parallel the several Zhi Huiliu cooling tubes (3) and the reaction cup of correspondence with it in the housing of backflow digestion device (1); The reaction cup bottom is provided with constant temperature heating device; The water tank (10) of each cooling tube that refluxes (3) connecting band water pump (9) is equipped with semiconductor cooler (11) on the water tank (10); Automatically in the analysis and detection device tubular capacitance pool is set, the outside surface set metal light wall pipe (32) of tubular capacitance pool loads platinum filament (33) on the tubular cavity central axial line of capacitance pool; Metal light wall pipe (32) is drawn lead (A), (B) that is connected automatic analyzing and testing circuit respectively with platinum filament (33); The capacitance pool top is provided with the solenoid valve (21) of band dripping hole, and solenoid valve (21) is communicated with reservoir (20); The titration valve (19) of capacitance pool lower end connecting band titration mouth (18); Electrode assemblie lifting pivot is set between capacitance pool and reaction cup; The stirrer (17) that is driven by stirring motor (16) is arranged in the reaction cup.
2, a kind of using method of automatic analyzer of chemically needed oxygen quantity for full digestion as claimed in claim 1, routine analyzer comprises the preparation oxygenant, add acid, clear up and titration, it is characterized in that: adopt potassium dichromate method preparation oxygenant, its concentration is 0.125N, contains 0.1 milliliter of concentrated sulphuric acid in one milliliter of oxygenant, contains 0.01 gram mercuric sulfate; Blank sample reaction cup and each detected water sample reaction cup add 1 milliliter in 10 milliliters in blank water and oxygenant respectively; Respectively add 1 milliliter of detected water sample in the detected water sample reaction cup; By the concentration ratio preparation digestion solution that contains 0.09 gram silver sulfate in 10 milliliters of concentrated sulphuric acids, blank sample reaction cup and each detected water sample reaction cup add 10 milliliters of digestion solutions respectively; Cleared up 10 minutes, mend then and add water to 75 milliliters, carry out titration, blank sample and each detected water sample are successively placed respectively on the automatic analyzing and testing device, fill with ferrous titrant then in capacitance pool, stir by stirrer, display shows initial potential, displacement variable by titrant in the capacitance pool demonstrates the terminal point current potential at last, and the demonstration of terminal point current potential shows the chemical oxygen demand value of water sample after moment.
3, a kind of using method of automatic analyzer of chemically needed oxygen quantity for full digestion as claimed in claim 1, routine analyzer comprises the preparation oxygenant, adds acid, clears up and titration, it is characterized in that: adopt permanganimetric method preparation oxygenant, its concentration is 0.025N; Blank sample reaction cup and each detected water sample reaction cup add 1 milliliter in 10 milliliters in blank water and oxygenant respectively; Respectively add 1 milliliter of detected water sample in the detected water sample reaction cup, and in each reaction cup, add 10 milliliters of 25% concentration dilute sulfuric acids, place and clear up cup, cleared up 5 minutes, add water to 75 milliliters again and carry out titration, blank sample and each detected water sample are successively placed respectively on the automatic analyzing and testing device, in capacitance pool, fill with ferrous titrant again, stir by stirrer, display shows initial potential, displacement variable by titrant in the capacitance pool causes indicator electrode current potential generation hop with the working battery of accepting mutually with it at last, shows the terminal point current potential, and the demonstration of terminal point current potential demonstrates the chemical oxygen demand value of water sample after moment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122502 CN1110703C (en) | 1999-11-04 | 1999-11-04 | Automatic analyzer of chemically needed oxygen quantity for full digestion and its application method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122502 CN1110703C (en) | 1999-11-04 | 1999-11-04 | Automatic analyzer of chemically needed oxygen quantity for full digestion and its application method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1264837A CN1264837A (en) | 2000-08-30 |
| CN1110703C true CN1110703C (en) | 2003-06-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99122502 Expired - Fee Related CN1110703C (en) | 1999-11-04 | 1999-11-04 | Automatic analyzer of chemically needed oxygen quantity for full digestion and its application method |
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| Country | Link |
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| CN (1) | CN1110703C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539223A (en) * | 2012-01-08 | 2012-07-04 | 中国科学院南京地理与湖泊研究所 | COD (Chemical Oxygen Demand)Cr batch digestion device |
| CN103777030B (en) * | 2014-01-26 | 2015-05-27 | 石家庄德润环保科技有限公司 | Automatic laboratory chemical oxygen demand analysis device |
| CN104914209A (en) * | 2015-06-25 | 2015-09-16 | 无锡点创科技有限公司 | Laboratory COD automatic analysis robot |
| CN109655574B (en) * | 2018-12-17 | 2023-05-12 | 西南石油大学 | Method for measuring oxidizable capacity of shale reservoir |
| CN111141868B (en) * | 2020-03-27 | 2024-09-06 | 安徽帝业分析仪器有限公司 | Reaction device and detection method for double-electrode method detection |
-
1999
- 1999-11-04 CN CN 99122502 patent/CN1110703C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1264837A (en) | 2000-08-30 |
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