CN101566489B - Reagent constant volume method and CODcr on-line monitoring art - Google Patents
Reagent constant volume method and CODcr on-line monitoring art Download PDFInfo
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- CN101566489B CN101566489B CN2009103033044A CN200910303304A CN101566489B CN 101566489 B CN101566489 B CN 101566489B CN 2009103033044 A CN2009103033044 A CN 2009103033044A CN 200910303304 A CN200910303304 A CN 200910303304A CN 101566489 B CN101566489 B CN 101566489B
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Abstract
The invention relates to a reagent constant volume method and a CODcr on-line monitoring art, belonging to chemical analysis field. The technical scheme is that: setting a reagent refluxing mouth at the position aligned with the constant volume line horizontal direction; during constant volume, feeding the reagent for constant volume into a constant volume cup; leading out the reagent higher than the constant volume line from the refluxing mouth; performing subsequent reaction for the residual reagent in the constant volume cup, i.e. constant volume reagent. The method is used for reagent constant volume method in the chemical reaction or analysis test. The constant volume method can accurately test the COD value in the waste water by the CODcr on-line automatic monitoring art and greatly improve the stability and reliability of the monitoring instrument that MTBF is more than or equal to 720 hours.
Description
Technical field
The present invention relates to a kind of peristaltic pump rotating reagent constant volume method and CODcr on-line monitoring instrument technology, belong to chemical analysis field.
Background technology
Chemical oxygen consumption (COC) (COD) is meant under certain conditions, the amount of the oxygenant that reducing substances consumed (is calculated with the oxygen amount in the oxidation 1 premium on currency sample, represent with mg/L), being an important overall target estimating polluter relative content in the water body, also is one of important indicator to river, industrial sewage monitoring and sewage treatment plant's blowdown control.CODcr measures chemical method, coulometric titration and instrumental method.Instrumental method principle of work: with the mixed liquor (catalyzer) of a certain amount of water sample, potassium dichromate digestion solution (oxygenant), silver sulfate and the concentrated sulphuric acid, be heated to 165 ℃ and fully clear up reaction, organism in the water and some reducing substances, oxidized in acid potassium bichromate solution, Cr
6+Be reduced to Cr
3+, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse chemical oxygen demand (COD) (CODcr).Facts have proved that the quality of CODcr online automatic monitor measuring accuracy and stability depends on the accuracy and the reproducible degree of accuracy of classes of agents metering.At present general metering method is that peristaltic pump is realized through the timing liquid feeding through the pump line of certain diameter, but as time goes by, and the fatigue of pump line or pipe clamp will cause the deviation of constant volume, or causes error in dipping because of voltage fluctuation.
Summary of the invention
Technical matters to be solved by this invention provides a kind of accurate, stable reagent constant volume method.And CODcr online automatic monitor technology proposed on this basis.
Technical solution of the present invention: the reagent constant volume method adopts the peristaltic pump rotating to extract constant volume.The place of flushing is provided with the reagent refluxing opening in constant volume scale mark horizontal direction, and the above reagent of constant volume line is derived from refluxing opening, and remaining reagent promptly is the reagent through constant volume in the constant volume cup.
The mode that described refluxing opening can be realized usually is the overflow vent at constant volume cup constant volume line place, the reagent automatic overflow that the constant volume line is above.The preferred mode of the present invention is: the outlet of adopting the delivery of therapeutic agents conduit is as refluxing opening, the outlet of delivery of therapeutic agents conduit (also can be described as inlet) outlet flushes with the constant volume scale mark, to need the reagent of constant volume to import the constant volume cup from the reagent storage bottle by the reagent delivery conduit, guarantee that liquid level surpasses the constant volume line, again the reagent solution more than the constant volume line is derived, subsequent reactions can be carried out, the accuracy of constant volume can be guaranteed simultaneously.
In order to save reagent, adopt peristaltic pump will need the reagent of constant volume to import the constant volume cup during constant volume from the reagent storage bottle, guarantee that liquid level surpasses the constant volume line, leads back the reagent corresponding storage bottle with the reagent solution more than the constant volume line again.
In order to carry out constant volume to the required reagent of each reaction simultaneously, described peristaltic pump can adopt many raceways peristaltic pump.And needn't adopt a plurality of single raceway peristaltic pumps, thus saved the program work time greatly, also reduced the use cost of equipment simultaneously.
The constant volume line can adopt the standard measuring cup to demarcate.1ml can be arranged, 2ml ... etc. different constant volume lines, all constant volume lines all through demarcating, can use different constant volume lines according to actual conditions.
CODcr online auto monitoring method of the present invention: the mixed liquor (catalyzer) that adopts water sample, potassium dichromate digestion solution (oxygenant), silver sulfate and the concentrated sulphuric acid behind the above-mentioned constant volume method constant volume, be heated to about 165 ℃ ± 2 ℃ and fully clear up reaction, organism in the water and some reducing substances, oxidized in acid potassium bichromate solution, Cr
6+Be reduced to Cr
3+, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse chemical oxygen demand (COD) (CODcr).
Particularly, may further comprise the steps:
A, the mixed liquor of water sample to be measured, potassium dichromate digestion solution, silver sulfate and the concentrated sulphuric acid is respectively charged in separately the reagent storage bottle, be connected on the peristaltic pump by the constant volume conduit respectively, the peristaltic pump other end connects the constant volume cup of each reagent by the constant volume conduit, and each constant volume cup is connected to reactor by the reaction conduit;
The required reagent of reaction is cleared up in b, setting: the volume of water sample to be measured, potassium dichromate digestion solution, catalyzer; Employing standard measuring cup carries out volume calibration to the constant volume cup of each reagent, marks the constant volume line at the constant volume wall of cup, and the constant volume conduit outlet is flushed with constant volume line separately; Described catalyzer is the mixed liquor of the silver sulfate and the concentrated sulphuric acid;
C, peristaltic pump are just changeing in each reagent importing constant volume cup separately, guarantee that each reagent liquid level surpasses constant volume line separately, by peristaltic pump counter-rotating the reagent more than the constant volume line is led back separately reagent reservoir bottle then, remaining reagent promptly is the reagent that passes through constant volume in the constant volume cup;
Each reagent through constant volume in d, the constant volume cup is delivered to mixing reactor by the reaction conduit, is heated to and fully clears up reaction, Cr about 165 ± 2 ℃
6+Be reduced to Cr
3+, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse CODcr.
React required reagent and can also comprise distilled water, carry out identical operations simultaneously, be used for diluting reaction reagent or purge heater and colorimetric vessel with other reagent.
Further, technology is seen Fig. 3.Described peristaltic pump is four raceway peristaltic pumps, has replaced the peristaltic pump of 4 single raceways by four raceway peristaltic pumps, and four raceway peristaltic pumps are carried all ingredients by just changeing simultaneously to the constant volume cup.Simultaneously 4 kinds of different reagent are carried out constant volume by counter-rotating, thereby saved the program work time greatly, also reduced the use cost of equipment simultaneously
Another technical matters to be solved by this invention provides a kind of online automatic monitor, comprise raceway peristaltic pump more than, a plurality of reagent storage bottle, a plurality of constant volume cups, 1 reactor, endpoint monitoring and control system, and data handling system, wherein, reagent storage bottle and constant volume cup are connected on the peristaltic pump by the constant volume conduit respectively, and each constant volume cup is delivered to reactor by the reaction conduit respectively; The constant volume line is arranged on the wall of constant volume cup, and the constant volume conduit outlet flushes with the constant volume line.
Particularly, the CODcr online automatic monitor comprises one 4 raceway peristaltic pump, water sample to be measured, potassium dichromate digestion solution, catalyzer, distilled water reagent storage bottle separately and corresponding separately constant volume cup, 1 reactor, and 1 colorimetric estimation system and computer control system; Wherein on each constant volume wall of cup the constant volume line is arranged, each reagent storage bottle and corresponding separately constant volume cup are connected on the 4 raceway peristaltic pumps by the constant volume conduit respectively, and the constant volume conduit outlet flushes with the constant volume line, and each constant volume cup is delivered to reactor by the reaction conduit respectively; Adopt the colorimetric estimation system to detect titration end-point, by computer system control colorimetric titration system and calculate CODcr.
In order better to finish technical scheme of the present invention,, peristaltic pump of the present invention carries the peristaltic pump of liquid but preferably adopting rotating to wriggle.
Beneficial effect of the present invention: the present invention can measure the COD value in the waste water accurately, and every technical indicator meets country and company standard fully, has improved the stability and the reliability of monitor greatly, makes MTBF 〉=720 hour, receives Expected Results.
Description of drawings
Fig. 1 peristaltic pump is just being changed a job and is being made synoptic diagram, and peristaltic pump is just changeing all ingredients is sent in the constant volume cup, and the reagent solution liquid level substantially exceeds standard constant volume line.
Fig. 2 peristaltic pump counter-rotating work synoptic diagram is drawn back the reagent of various surplus capacities to original solution bottle during the peristaltic pump counter-rotating, makes liquid level at standard constant volume line, reaches the purpose of constant volume.
Wherein, numbering 1 is that peristaltic pump, 2 is that reagent storage bottle, 3 is that reagent, 4 is that constant volume cup, 5 is that constant volume conduit, 6 is that constant volume line, 7 is to react conduit.
Fig. 3 CODcr online auto monitoring process schematic representation.
Embodiment
Reagent constant volume method of the present invention can adopt the peristaltic pump forward and backward to extract constant volume, sees Fig. 1 and Fig. 2.Comprise reagent storage bottle 2, peristaltic pump 1, constant volume cup 4, reagent storage bottle 2, constant volume cup 4 are connected on the peristaltic pump 1 by constant volume conduit 5 respectively; Constant volume line 6 is arranged on the wall of constant volume cup 4, and constant volume conduit 5 outlets that constant volume cup 4 is connected peristaltic pump 1 flush with constant volume line 6.During constant volume, just changeing in the reagent 3 importing constant volume cups 4, guaranteeing that liquid level is much higher than the height of constant volume line 6, by peristaltic pump 1 counter-rotating the reagent more than the constant volume line 3 is being led back in the reagent reservoir bottle 2 then by raceway peristaltic pump 1.Remaining reagent 3 is the reagent of constant volume in the constant volume cup, can be delivered to reactor by reaction conduit 7 and carry out subsequent reactions.
The constant volume line can adopt the standard measuring cup to demarcate.1ml can be arranged, 2ml ... on the constant volume line of different volumes, all constant volume lines all through demarcating, can select to use different constant volume lines according to actual conditions.
CODcr online auto monitoring technology of the present invention may further comprise the steps:
A, water sample to be measured, potassium dichromate digestion solution, catalyzer (mixed liquor of the silver sulfate and the concentrated sulphuric acid), distilled water are respectively charged in separately the reagent storage bottle, and be connected on the four raceway peristaltic pumps, the four raceway peristaltic pump other ends connect the constant volume cup of each reagent, and each constant volume cup is connected to reactor;
The required reagent of reaction is cleared up in b, setting: the volume of water sample to be measured, potassium dichromate digestion solution, catalyzer, distilled water; Employing standard measuring cup carries out volume calibration to the constant volume cup of each reagent, marks the constant volume line at the constant volume wall of cup, and the constant volume conduit outlet is flushed with constant volume line separately;
C, four raceway peristaltic pumps are just changeing in the constant volume cup that simultaneously each reagent is imported separately, guarantee that each reagent liquid level surpasses constant volume line separately, simultaneously the reagent more than the constant volume line is led back separately reagent reservoir bottle by four raceway peristaltic pumps counter-rotatings then, remaining reagent promptly is the reagent that passes through constant volume in the constant volume cup; Reach the effect of simultaneously 4 kinds of different reagent being carried out constant volume.
Each reagent of d, process constant volume is delivered to reactor simultaneously by the reaction conduit to be mixed, and mixed liquor is heated to 165 ℃ and fully clears up reaction, and the organism in the water and some reducing substances are oxidized in acid potassium bichromate solution, Cr
6+Be reduced to Cr
3+, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse CODcr.Distilled water is used for diluting or purge heater and colorimetric vessel.
Can pass through classical control system, monitor to on-line continuous.
The CODcr online automatic monitor, comprise one 4 raceway peristaltic pump, water sample to be measured, potassium dichromate digestion solution, catalyzer, distilled water reagent storage bottle separately and corresponding separately constant volume cup, 1 reactor, and 1 colorimetric estimation system and computer control system; Wherein on each constant volume wall of cup the constant volume line is arranged, each reagent storage bottle and corresponding separately constant volume cup are connected on the 4 raceway peristaltic pumps by the constant volume conduit respectively, and the constant volume conduit outlet flushes with the constant volume line, and each constant volume cup is delivered to reactor by the reaction conduit respectively; Adopt the colorimetric estimation system to detect titration end-point, by computer system control colorimetric titration system and calculate CODcr
Below mode by specific embodiment the present invention is further described, be limited to following examples but should not be construed as the present invention.The modification that those skilled in the art make according to above-mentioned technological invention thought, replacement, change all belong to the present invention.
Technological parameter in following examples:
The rate of heat addition: 546s
Rate of temperature fall: 204s
Sampling rate:
1, oxygenant: 25s
2, distilled water: 40s
3, water sample: 35s
4, catalyzer: 50s
The test of embodiment 1 reappearance
According to predefined amount, with 3 milliliters COD water sample, 1 milliliter of potassium dichromate digestion solution, the mixed liquor (catalyzer) of the 5 milliliters of silver sulfates and the concentrated sulphuric acid, 2 milliliters distilled water is constant volume respectively:
1, peristaltic pump was just changeing 50 seconds, and each reagent moves in the constant volume cup, guarantees that liquid level surpasses the constant volume line.
2, the peristaltic pump counter-rotating is 50 seconds, and the reagent more than the constant volume line is drawn back each reagent reservoir bottle.
3, demarcate each constant volume cup raffinate with the standard measuring cup.
The solution of each constant volume cup constant volume is delivered to hybrid heater, is mixed and heated to 165 ℃ ± 2 ℃ heating and clears up reaction in 15 minutes, be chilled to room temperature after, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse chemical oxygen demand (COD) (CODcr).The results are shown in Table 1, range sees Table 2, and drift sees Table 3.
Table 1
| Sequence number | Time | The |
| 1 | 2009-05-12?09:00:00 | -0.75 |
| 2 | 2009-05-12?10:00:00 | 1.43 |
| 3 | 2009-05-12?11:00:00 | 2.68 |
| 4 | 2009-05-12?12:00:00 | 1.70 |
| 5 | 2009-05-12?13:00:00 | 1.06 |
| 6 | 2009-05-12?14:00:00 | -1.54 |
| 7 | 2009-05-12?15:00:00 | 2.86 |
| 8 | 2009-05-12?16:00:00 | 1.25 |
| 9 | 2009-05-12?17:00:00 | 679.54 |
| 10 | 2009-05-12?18:00:00 | 780.37 |
| 11 | 2009-05-12?19:00:00 | 799.05 |
| 12 | 2009-05-12?20:00:00 | 782.14 |
| 13 | 2009-05-12?21:00:00 | 790.39 |
| 14 | 2009-05-12-22:00:00 | 775.69 |
| 15 | 2009-05-12?23:00:00 | 801.25 |
Table 2
| Sequence number | Time | The |
| 1 | 2009-05-12?05:00:00 | 787.70 |
| 2 | 2009-05-12?06:00:00 | 790.41 |
| 3 | 2009-05-12?07:00:00 | 776.64 |
| 4 | 2009-05-12?08:00:00 | 801.79 |
| 5 | 2009-05-15?09:00:00 | 770.96 |
| 6 | 2009-05-15?10:00:00 | 775.84 |
| 7 | 2009-05-15?11:00:00 | 770.62 |
| 8 | 2009-05-15?12:00:00 | 786.47 |
Table 3
| Sequence number | Time | The |
| 1 | 2009-05-13-09:00:00 | 1.01 |
| 2 | 2009-05-13?10:00:00 | 1.76 |
| 3 | 2009-05-13?11:00:00 | 1.37 |
| 4 | 2009-0513-12:00:00 | -0.67 |
| 5 | 2009-05-13?13:00:00 | -1.35 |
| 6 | 2009-05-13?14:00:00 | 1.68 |
| 7 | 2009-05-13?15:00:00 | 2.75 |
| 8 | 2009-05-13?16:00:00 | -2.66 |
| 9 | 2009-05-13-17:00:00 | -1.07 |
| 10 | 2009-05-13-18:00:00 | 2.54 |
| 11 | 2009-05-13-19:00:00 | 0.17 |
| 12 | 2009-05-13?20:00:00 | 2.84 |
| 13 | 2009-05-13?21:00:00 | -1.38 |
| 14 | 2009-05-13?22:00:00 | 2.71 |
| 15 | 2009-05-13?23:00:00 | 1.84 |
| 16 | 2009-05-14?00:00:00 | 2.30 |
| 17 | 2009-05-14?01:00:00 | 1.67 |
| 18 | 2009-05-14?02:00:00 | -2.51 |
| 19 | 2009-05-14?03:00:00 | 0.37 |
| 20 | 2009-05-14?04:00:00 | 1.95 |
| 21 | 2009-05-14?05:00:00 | 1.42 |
| 22 | 2009-05-14?06:00:00 | 2.06 |
| 23 | 2009-05-14-07:00:00 | 2.74 |
| 24 | 2009-0514-08:00:00 | 1.59 |
From table 1, table 2, table 3 as can be seen, the deviation ratio of reappearance, drift and span drift is less; The standard deviation of method and the requirement of relative standard deviation coincidence detection; This method can be applied in the environmental monitoring water analysis work.
Get the ambient water quality standard model of standard model research institute of State Environmental Protection Administration and measure, all in given range, test result is qualified for measured value.
Test MTBF (average non-failure operation time) reagent that uses is about the actual waste water sample of 100mg/L as the COD value.
Monitor was tested 24 times from every day on May 11st, 12 days 1 April in 2009, did not break down.The result is as follows:
Table 4
| Sequence number | Time | The |
| 1 | 2009-04-12?10:00:00 | 100.95 |
| 2 | 2009-04-12?11:00:00 | 101.27 |
| 3 | 2009-04-12?12:00:00 | 101.70 |
| 4 | 2009-04-12?13:00:00 | 107.92 |
| 5 | 2009-04-12?14:00:00 | 93.48 |
| 6 | 2009-04-12?15:00:00 | 100.27 |
| 7 | 2009-04-12?16:00:00 | 91.83 |
| 8 | 2009-04-12?17:00:00 | 93.32 |
| 9 | 2009-04-12?18:00:00 | 92.38 |
| 10 | 2009-04-12?19:00:00 | 97.56 |
| 11 | 2009-04-12?20:00:00 | 102.04 |
| 12 | 2009-04-12?21:00:00 | 103.26 |
| 13 | 2009-04-12?22:00:00 | 91.14 |
| 14 | 2009-04-12?23:00:00 | 106.05 |
| 15 | 2009-04-13?00:00:00 | 107.52 |
| 16 | 2009-04-13?01:00:00 | 108.51 |
| 17 | 2009-04-13?02:00:00 | 99.24 |
| 18 | 2009-04-13?03:00:00 | 94.19 |
| 19 | 2009-04-13?04:00:00 | 109.94 |
| 20 | 2009-04-13?05:00:00 | 97.85 |
| 21 | 2009-04-13?06:00:00 | 106.80 |
| 22 | 2009-04-13?07:00:00 | 91.85 |
| 23 | 2009-04-13?08:00:00 | 90.18 |
| 24 | 2009-04-13?09:00:00 | 95.46 |
| 25 | 2009-04-13?10:00:00 | 106.75 |
| 26 | 2009-04-13?11:00:00 | 94.11 |
| 27 | 2009-04-13?12:00:00 | 99.16 |
| 28 | 2009-04-13?13:00:00 | 92.17 |
| 29 | 2009-04-13?14:00:00 | 104.70 |
| 30 | 2009-04-13?15:00:00 | 97.23 |
| 31 | 2009-04-13?16:00:00 | 98.50 |
| 32 | 2009-04-13?17:00:00 | 109.80 |
| 33 | 2009-04-13?18:00:00 | 93.38 |
| 34 | 2009-04-13?19:00:00 | 91.27 |
| 35 | 2009-04-13?20:00:00 | 92.95 |
| 36 | 2009-04-13?21:00:00 | 108.10 |
| 37 | 2009-04-13?22:00:00 | 98.53 |
| 38 | 2009-04-13?23:00:00 | 103.66 |
| 39 | 2009-04-14?00:00:00 | 106.43 |
| 40 | 2009-04-14?01:00:00 | 93.56 |
| 41 | 2009-04-14?02:00:00 | 93.11 |
| 42 | 2009-04-14?03:00:00 | 98.11 |
| 43 | 2009-04-14?04:00:00 | 103.64 |
| 44 | 2009-04-14?05:00:00 | 99.51 |
| 45 | 2009-04-14?06:00:00 | 106.69 |
| 46 | 2009-04-14?07:00:00 | 103.26 |
| 47 | 2009-04-14?08:00:00 | 108.99 |
| 48 | 2009-04-14?09:00:00 | 96.92 |
| 49 | 2009-04-14?10:00:00 | 106.94 |
| 50 | 2009-04-14?11:00:00 | 95.44 |
| 51 | 2009-04-14?12:00:00 | 104.78 |
| 52 | 2009-04-14?13:00:00 | 105.23 |
| 53 | 2009-04-14?14:00:00 | 100.02 |
| 54 | 2009-04-14?15:00:00 | 109.89 |
| 55 | 2009-04-14?16:00:00 | 100.63 |
| 56 | 2009-04-14?17:00:00 | 102.54 |
| 57 | 2009-04-14?18:00:00 | 106.84 |
| 58 | 2009-04-14?19:00:00 | 104.86 |
| 59 | 2009-04-14?20:00:00 | 95.72 |
| 60 | 2009-04-14?21:00:00 | 104.66 |
| 61 | 2009-04-14?22:00:00 | 102.00 |
| 62 | 2009-04-14?23:00:00 | 92.89 |
| 63 | 2009-04-15?00:00:00 | 106.12 |
| 64 | 2009-04-15?01:00:00 | 92.31 |
| 65 | 2009-04-15?02:00:00 | 92.28 |
| 66 | 2009-04-15?03:00:00 | 103.72 |
| 67 | 2009-04-15?04:00:00 | 98.73 |
| 68 | 2009-04-15?05:00:00 | 95.81 |
| 69 | 2009-04-15?06:00:00 | 101.56 |
| 70 | 2009-04-15?07:00:00 | 93.20 |
| 71 | 2009-04-15?08:00:00 | 103.92 |
| 72 | 2009-04-15?09:00:00 | 96.72 |
| 73 | 2009-04-15?10:00:00 | 99.15 |
| 74 | 2009-04-15?11:00:00 | 102.50 |
| 75 | 2009-04-15?12:00:00 | 108.63 |
| 76 | 2009-04-15?13:00:00 | 95.80 |
| 77 | 2009-04-15?14:00:00 | 98.21 |
| 78 | 2009-04-15?15:00:00 | 102.08 |
| 79 | 2009-04-15?16:00:00 | 101.96 |
| 80 | 2009-04-15?17:00:00 | 106.58 |
| 81 | 2009-04-15?18:00:00 | 101.32 |
| 82 | 2009-04-15?19:00:00 | 104.76 |
| 83 | 2009-04-15?20:00:00 | 94.86 |
| 84 | 2009-04-15?21:00:00 | 103.97 |
| 85 | 2009-04-15?22:00:00 | 99.89 |
| 86 | 2009-04-15?23:00:00 | 102.24 |
| 87 | 2009-04-16?00:00:00 | 106.09 |
| 88 | 2009-04-16?01:00:00 | 107.35 |
| 89 | 2009-04-16?02:00:00 | 104.55 |
| 90 | 2009-04-16?03:00:00 | 109.53 |
| 91 | 2009-04-16?04:00:00 | 96.12 |
| 92 | 2009-04-16?05:00:00 | 107.38 |
| 93 | 2009-04-16?06:00:00 | 93.10 |
| 94 | 2009-04-16?07:00:00 | 91.53 |
| 95 | 2009-04-16?08:00:00 | 100.90 |
| 96 | 2009-04-16?09:00:00 | 95.97 |
| 97 | 2009-04-16?10:00:00 | 93.05 |
| 98 | 2009-04-16?11:00:00 | 96.28 |
| 99 | 2009-04-16?12:00:00 | 107.47 |
| 100 | 2009-04-16?13:00:00 | 108.88 |
| 101 | 2009-04-16?14:00:00 | 105.70 |
| 102 | 2009-04-16?15:00:00 | 109.12 |
| 103 | 2009-04-16?16:00:00 | 103.08 |
| 104 | 2009-04-16?17:00:00 | 100.10 |
| 105 | 2009-04-16?18:00:00 | 108.40 |
| 106 | 2009-04-16?19:00:00 | 92.29 |
| 107 | 2009-04-16?20:00:00 | 99.94 |
| 108 | 2009-04-16?21:00:00 | 97.65 |
| 109 | 2009-04-16?22:00:00 | 102.13 |
| 110 | 2009-04-16?23:00:00 | 104.16 |
| 111 | 2009-04-17?00:00:00 | 107.26 |
| 112 | 2009-04-17?01:00:00 | 99.94 |
| 113 | 2009-04-17?02:00:00 | 101.06 |
| 114 | 2009-04-17?03:00:00 | 102.62 |
| 115 | 2009-04-17?04:00:00 | 92.63 |
| 116 | 2009-04-17?05:00:00 | 102.24 |
| 117 | 2009-04-17?06:00:00 | 91.12 |
| 118 | 2009-04-17?07:00:00 | 106.94 |
| 119 | 2009-04-17?08:00:00 | 104.43 |
| 120 | 2009-04-17?09:00:00 | 92.53 |
| 121 | 2009-04-17?10:00:00 | 94.35 |
| 122 | 2009-04-17?11:00:00 | 102.48 |
| 123 | 2009-04-17?12:00:00 | 97.35 |
| 124 | 2009-04-17?13:00:00 | 106.14 |
| 125 | 2009-04-17?14:00:00 | 105.96 |
| 126 | 2009-04-17?15:00:00 | 102.60 |
| 127 | 2009-04-17?16:00:00 | 92.73 |
| 128 | 2009-04-17?17:00:00 | 98.56 |
| 129 | 2009-04-17?18:00:00 | 100.96 |
| 130 | 2009-04-17?19:00:00 | 92.21 |
| 131 | 2009-04-17?20:00:00 | 95.68 |
| 132 | 2009-04-17?21:00:00 | 105.79 |
| 133 | 2009-04-17?22:00:00 | 97.22 |
| 134 | 2009-04-17?23:00:00 | 107.27 |
| 135 | 2009-04-18?00:00:00 | 100.85 |
| 136 | 2009-04-18?01:00:00 | 91.63 |
| 137 | 2009-04-18?02:00:00 | 91.89 |
| 138 | 2009-04-18?03:00:00 | 94.66 |
| 139 | 2009-04-18?04:00:00 | 108.63 |
| 140 | 2009-04-18?05:00:00 | 91.17 |
| 141 | 2009-04-18?06:00:00 | 97.97 |
| 142 | 2009-04-18?07:00:00 | 106.74 |
| 143 | 2009-04-18?08:00:00 | 103.87 |
| 144 | 2009-04-18?09:00:00 | 90.09 |
| 145 | 2009-04-18?10:00:00 | 97.97 |
| 146 | 2009-04-18?11:00:00 | 95.10 |
| 147 | 2009-04-18?12:00:00 | 98.71 |
| 148 | 2009-04-18?13:00:00 | 108.82 |
| 149 | 2009-04-18?14:00:00 | 101.53 |
| 150 | 2009-04-18?15:00:00 | 97.66 |
| 151 | 2009-04-18?16:00:00 | 91.64 |
| 152 | 2009-04-18?17:00:00 | 91.30 |
| 153 | 2009-04-18?18:00:00 | 103.83 |
| 154 | 2009-04-18?19:00:00 | 103.71 |
| 155 | 2009-04-18?20:00:00 | 104.56 |
| 156 | 2009-04-18?21:00:00 | 107.37 |
| 157 | 2009-04-18?22:00:00 | 91.71 |
| 158 | 2009-04-18?23:00:00 | 91.18 |
| 159 | 2009-04-19?00:00:00 | 109.64 |
| 160 | 2009-04-19?01:00:00 | 108.45 |
| 161 | 2009-04-19?02:00:00 | 94.37 |
| 162 | 2009-04-19?03:00:00 | 100.43 |
| 163 | 2009-04-19?04:00:00 | 108.05 |
| 164 | 2009-04-19?05:00:00 | 105.64 |
| 165 | 2009-04-19?06:00:00 | 105.52 |
| 166 | 2009-04-19?07:00:00 | 99.13 |
| 167 | 2009-04-19?08:00:00 | 92.28 |
| 168 | 2009-04-19?09:00:00 | 109.85 |
| 169 | 2009-04-19?10:00:00 | 93.79 |
| 170 | 2009-04-19?11:00:00 | 102.41 |
| 171 | 2009-04-19?12:00:00 | 93.91 |
| 172 | 2009-04-19?13:00:00 | 103.14 |
| 173 | 2009-04-19?14:00:00 | 108.43 |
| 174 | 2009-04-19?15:00:00 | 102.73 |
| 175 | 2009-04-19?16:00:00 | 108.86 |
| 176 | 2009-04-19?17:00:00 | 100.73 |
| 177 | 2009-04-19?18:00:00 | 97.01 |
| 178 | 2009-04-19?19:00:00 | 93.93 |
| 179 | 2009-04-19?20:00:00 | 101.81 |
| 180 | 2009-04-19?21:00:00 | 93.12 |
| 181 | 2009-04-19?22:00:00 | 102.09 |
| 182 | 2009-04-19?23:00:00 | 103.69 |
| 183 | 2009-04-20?00:00:00 | 101.84 |
| 184 | 2009-04-20?01:00:00 | 107.52 |
| 185 | 2009-04-20?02:00:00 | 93.71 |
| 186 | 2009-04-20?03:00:00 | 98.84 |
| 187 | 2009-04-20?04:00:00 | 90.99 |
| 188 | 2009-04-20?05:00:00 | 98.15 |
| 189 | 2009-04-20?06:00:00 | 104.57 |
| 190 | 2009-04-20?07:00:00 | 97.95 |
| 191 | 2009-04-20?08:00:00 | 97.76 |
| 192 | 2009-04-20?09:00:00 | 104.67 |
| 193 | 2009-04-20?10:00:00 | 104.79 |
| 194 | 2009-04-20?11:00:00 | 95.45 |
| 195 | 2009-04-20?12:00:00 | 97.36 |
| 196 | 2009-04-20?13:00:00 | 108.15 |
| 197 | 2009-04-20?14:00:00 | 103.10 |
| 198 | 2009-04-20?15:00:00 | 91.81 |
| 199 | 2009-04-20?16:00:00 | 90.56 |
| 200 | 2009-04-20?17:00:00 | 103.95 |
| 201 | 2009-04-20?18:00:00 | 91.36 |
| 202 | 2009-04-20?19:00:00 | 93.97 |
| 203 | 2009-04-20?20:00:00 | 103.10 |
| 204 | 2009-04-20?21:00:00 | 100.91 |
| 205 | 2009-04-20?22:00:00 | 99.28 |
| 206 | 2009-04-20?23:00:00 | 100.62 |
| 207 | 2009-04-21?00:00:00 | 97.44 |
| 208 | 2009-04-21?01:00:00 | 106.20 |
| 209 | 2009-04-21?02:00:00 | 96.21 |
| 210 | 2009-04-21?03:00:00 | 96.44 |
| 211 | 2009-04-21?04:00:00 | 98.80 |
| 212 | 2009-04-21?05:00:00 | 105.17 |
| 213 | 2009-04-21?06:00:00 | 106.85 |
| 214 | 2009-04-21?07:00:00 | 109.95 |
| 215 | 2009-04-21?08:00:00 | 107.27 |
| 216 | 2009-04-21?09:00:00 | 95.68 |
| 217 | 2009-04-21?10:00:00 | 97.82 |
| 218 | 2009-04-21?11:00:00 | 99.11 |
| 219 | 2009-04-21?12:00:00 | 98.04 |
| 220 | 2009-04-21?13:00:00 | 106.17 |
| 221 | 2009-04-21?14:00:00 | 101.90 |
| 222 | 2009-04-21?15:00:00 | 99.24 |
| 223 | 2009-04-21?16:00:00 | 101.38 |
| 224 | 2009-04-21?17:00:00 | 96.87 |
| 225 | 2009-04-21?18:00:00 | 96.83 |
| 226 | 2009-04-21?19:00:00 | 97.43 |
| 227 | 2009-04-21?20:00:00 | 104.51 |
| 228 | 2009-04-21?21:00:00 | 93.66 |
| 229 | 2009-04-21?22:00:00 | 105.60 |
| 230 | 2009-04-21?23:00:00 | 108.03 |
| 231 | 2009-04-22?00:00:00 | 106.98 |
| 232 | 2009-04-22?01:00:00 | 93.71 |
| 233 | 2009-04-22?02:00:00 | 95.01 |
| 234 | 2009-04-22?03:00:00 | 93.42 |
| 235 | 2009-04-22?04:00:00 | 91.63 |
| 236 | 2009-04-22?05:00:00 | 92.49 |
| 237 | 2009-04-22?06:00:00 | 99.46 |
| 238 | 2009-04-22?07:00:00 | 104.56 |
| 239 | 2009-04-22?08:00:00 | 102.95 |
| 240 | 2009-04-22?09:00:00 | 91.44 |
| 241 | 2009-04-22?10:00:00 | 106.78 |
| 242 | 2009-04-22?11:00:00 | 105.59 |
| 243 | 2009-04-22?12:00:00 | 94.63 |
| 244 | 2009-04-22?13:00:00 | 95.63 |
| 245 | 2009-04-22?14:00:00 | 93.04 |
| 246 | 2009-04-22?15:00:00 | 96.97 |
| 247 | 2009-04-22?16:00:00 | 98.29 |
| 248 | 2009-04-22?17:00:00 | 100.90 |
| 249 | 2009-04-22?18:00:00 | 103.15 |
| 250 | 2009-04-22?19:00:00 | 101.40 |
| 251 | 2009-04-22?20:00:00 | 95.20 |
| 252 | 2009-04-22?21:00:00 | 99.73 |
| 253 | 2009-04-22?22:00:00 | 104.19 |
| 254 | 2009-04-22?23:00:00 | 107.01 |
| 255 | 2009-04-23?00:00:00 | 102.90 |
| 256 | 2009-04-23?01:00:00 | 105.31 |
| 257 | 2009-04-23?02:00:00 | 108.25 |
| 258 | 2009-04-23?03:00:00 | 92.15 |
| 259 | 2009-04-23?04:00:00 | 98.55 |
| 260 | 2009-04-23?05:00:00 | 103.15 |
| 261 | 2009-04-23?06:00:00 | 91.80 |
| 262 | 2009-04-23?07:00:00 | 106.15 |
| 263 | 2009-04-23?08:00:00 | 90.97 |
| 264 | 2009-04-23?09:00:00 | 109.57 |
| 265 | 2009-04-23?10:00:00 | 108.28 |
| 266 | 2009-04-23?11:00:00 | 90.42 |
| 267 | 2009-04-23?12:00:00 | 103.08 |
| 268 | 2009-04-23?13:00:00 | 106.52 |
| 269 | 2009-04-23?14:00:00 | 101.01 |
| 270 | 2009-04-23?15:00:00 | 94.30 |
| 271 | 2009-04-23?16:00:00 | 96.85 |
| 272 | 2009-04-23?17:00:00 | 92.05 |
| 273 | 2009-04-23?18:00:00 | 93.02 |
| 274 | 2009-04-23?19:00:00 | 109.97 |
| 275 | 2009-04-23?20:00:00 | 102.42 |
| 276 | 2009-04-23?21:00:00 | 95.80 |
| 277 | 2009-04-23?22:00:00 | 100.96 |
| 278 | 2009-04-23?23:00:00 | 100.93 |
| 279 | 2009-04-24?00:00:00 | 103.40 |
| 280 | 2009-04-24?01:00:00 | 98.92 |
| 281 | 2009-04-24?02:00:00 | 109.78 |
| 282 | 2009-04-24?03:00:00 | 108.20 |
| 283 | 2009-04-24?04:00:00 | 100.11 |
| 284 | 2009-04-24?05:00:00 | 107.79 |
| 285 | 2009-04-24?06:00:00 | 95.04 |
| 286 | 2009-04-24?07:00:00 | 108.82 |
| 287 | 2009-04-24?08:00:00 | 102.83 |
| 288 | 2009-04-24?09:00:00 | 100.89 |
| 289 | 2009-04-24?10:00:00 | 109.92 |
| 290 | 2009-04-24?11:00:00 | 91.01 |
| 291 | 2009-04-24?12:00:00 | 96.65 |
| 292 | 2009-04-24?13:00:00 | 98.21 |
| 293 | 2009-04-24?14:00:00 | 103.57 |
| 294 | 2009-04-24?15:00:00 | 100.15 |
| 295 | 2009-04-24?16:00:00 | 90.09 |
| 296 | 2009-04-24?17:00:00 | 92.57 |
| 297 | 2009-04-24?18:00:00 | 107.82 |
| 298 | 2009-04-24?19:00:00 | 100.29 |
| 299 | 2009-04-24?20:00:00 | 109.14 |
| 300 | 2009-04-24?21:00:00 | 92.24 |
| 301 | 2009-04-24?22:00:00 | 99.10 |
| 302 | 2009-04-24?23:00:00 | 105.23 |
| 303 | 2009-04-25?00:00:00 | 108.72 |
| 304 | 2009-04-25?01:00:00 | 94.23 |
| 305 | 2009-04-25?02:00:00 | 92.37 |
| 306 | 2009-04-25?03:00:00 | 103.81 |
| 307 | 2009-04-25?04:00:00 | 103.39 |
| 308 | 2009-04-25?05:00:00 | 97.56 |
| 309 | 2009-04-25?06:00:00 | 94.09 |
| 310 | 2009-04-25?07:00:00 | 93.62 |
| 311 | 2009-04-25?08:00:00 | 109.20 |
| 312 | 2009-04-25?09:00:00 | 96.08 |
| 313 | 2009-04-25?10:00:00 | 90.92 |
| 314 | 2009-04-25?11:00:00 | 107.62 |
| 315 | 2009-04-25?12:00:00 | 98.53 |
| 316 | 2009-04-25?13:00:00 | 99.90 |
| 317 | 2009-04-25?14:00:00 | 101.19 |
| 318 | 2009-04-25?15:00:00 | 107.88 |
| 319 | 2009-04-25?16:00:00 | 99.82 |
| 320 | 2009-04-25?17:00:00 | 105.12 |
| 321 | 2009-04-25?18:00:00 | 105.84 |
| 322 | 2009-04-25?19:00:00 | 91.02 |
| 323 | 2009-04-25?20:00:00 | 104.08 |
| 324 | 2009-04-25?21:00:00 | 101.07 |
| 325 | 2009-04-25?22:00:00 | 105.94 |
| 326 | 2009-04-25?23:00:00 | 99.64 |
| 327 | 2009-04-26?00:00:00 | 90.02 |
| 328 | 2009-04-26?01:00:00 | 94.39 |
| 329 | 2009-04-26?02:00:00 | 103.41 |
| 330 | 2009-04-26?03:00:00 | 103.96 |
| 331 | 2009-04-26?04:00:00 | 109.63 |
| 332 | 2009-04-26?05:00:00 | 99.54 |
| 333 | 2009-04-26?06:00:00 | 92.02 |
| 334 | 2009-04-26?07:00:00 | 108.36 |
| 335 | 2009-04-26?08:00:00 | 106.28 |
| 336 | 2009-04-26?09:00:00 | 94.80 |
| 337 | 2009-04-26?10:00:00 | 95.39 |
| 338 | 2009-04-26?11:00:00 | 106.92 |
| 339 | 2009-04-26?12:00:00 | 106.90 |
| 340 | 2009-04-26?13:00:00 | 93.47 |
| 341 | 2009-04-26?14:00:00 | 98.99 |
| 342 | 2009-04-26?15:00:00 | 102.46 |
| 343 | 2009-04-26?16:00:00 | 100.45 |
| 344 | 2009-04-26?17:00:00 | 109.39 |
| 345 | 2009-04-26?18:00:00 | 92.93 |
| 346 | 2009-04-26?19:00:00 | 93.42 |
| 347 | 2009-04-26?20:00:00 | 104.33 |
| 348 | 2009-04-26?21:00:00 | 106.25 |
| 349 | 2009-04-26?22:00:00 | 92.49 |
| 350 | 2009-04-26?23:00:00 | 103.00 |
| 351 | 2009-04-27?00:00:00 | 90.64 |
| 352 | 2009-04-27?01:00:00 | 90.15 |
| 353 | 2009-04-27?02:00:00 | 93.13 |
| 354 | 2009-04-27?03:00:00 | 94.86 |
| 355 | 2009-04-27?04:00:00 | 94.27 |
| 356 | 2009-04-27?05:00:00 | 94.56 |
| 357 | 2009-04-27?06:00:00 | 107.04 |
| 358 | 2009-04-27?07:00:00 | 109.84 |
| 359 | 2009-04-27?08:00:00 | 94.55 |
| 360 | 2009-04-27?09:00:00 | 97.34 |
| 361 | 2009-04-27?10:00:00 | 97.96 |
| 362 | 2009-04-27?11:00:00 | 107.98 |
| 363 | 2009-04-27?12:00:00 | 92.50 |
| 364 | 2009-04-27?13:00:00 | 98.91 |
| 365 | 2009-04-27?14:00:00 | 101.20 |
| 366 | 2009-04-27?15:00:00 | 90.33 |
| 367 | 2009-04-27?16:00:00 | 95.35 |
| 368 | 2009-04-27?17:00:00 | 101.23 |
| 369 | 2009-04-27?18:00:00 | 105.76 |
| 370 | 2009-04-27?19:00:00 | 104.79 |
| 371 | 2009-04-27?20:00:00 | 90.40 |
| 372 | 2009-04-27?21:00:00 | 96.68 |
| 373 | 2009-04-27?22:00:00 | 105.36 |
| 374 | 2009-04-27?23:00:00 | 90.48 |
| 375 | 2009-04-28?00:00:00 | 100.01 |
| 376 | 2009-04-28?01:00:00 | 106.45 |
| 377 | 2009-04-28?02:00:00 | 95.27 |
| 378 | 2009-04-28?03:00:00 | 104.96 |
| 379 | 2009-04-28?04:00:00 | 99.53 |
| 380 | 2009-04-28?05:00:00 | 97.67 |
| 381 | 2009-04-28?06:00:00 | 101.94 |
| 382 | 2009-04-28?07:00:00 | 108.63 |
| 383 | 2009-04-28?08:00:00 | 90.20 |
| 384 | 2009-04-28?09:00:00 | 98.75 |
| 385 | 2009-04-28?10:00:00 | 102.05 |
| 386 | 2009-04-28?11:00:00 | 90.78 |
| 387 | 2009-04-28?12:00:00 | 108.75 |
| 388 | 2009-04-28?13:00:00 | 102.18 |
| 389 | 2009-04-28?14:00:00 | 98.14 |
| 390 | 2009-04-28?15:00:00 | 91.60 |
| 391 | 2009-04-28?16:00:00 | 105.63 |
| 392 | 2009-04-28?17:00:00 | 94.32 |
| 393 | 2009-04-28?18:00:00 | 107.49 |
| 394 | 2009-04-28?19:00:00 | 104.54 |
| 395 | 2009-04-28?20:00:00 | 93.81 |
| 396 | 2009-04-28?21:00:00 | 101.49 |
| 397 | 2009-04-28?22:00:00 | 91.18 |
| 398 | 2009-04-28?23:00:00 | 93.40 |
| 399 | 2009-04-29?00:00:00 | 99.90 |
| 400 | 2009-04-29?01:00:00 | 91.59 |
| 401 | 2009-04-29?02:00:00 | 100.31 |
| 402 | 2009-04-29?03:00:00 | 108.49 |
| 403 | 2009-04-29?04:00:00 | 99.52 |
| 404 | 2009-04-29?05:00:00 | 100.97 |
| 405 | 2009-04-29?06:00:00 | 106.03 |
| 406 | 2009-04-29?07:00:00 | 96.36 |
| 407 | 2009-04-29?08:00:00 | 108.87 |
| 408 | 2009-04-29?09:00:00 | 105.50 |
| 409 | 2009-04-29?10:00:00 | 90.53 |
| 410 | 2009-04-29?11:00:00 | 107.25 |
| 411 | 2009-04-29?12:00:00 | 94.26 |
| 412 | 2009-04-29?13:00:00 | 105.59 |
| 413 | 2009-04-29?14:00:00 | 105.63 |
| 414 | 2009-04-29?15:00:00 | 94.85 |
| 415 | 2009-04-29?16:00:00 | 91.51 |
| 416 | 2009-04-29?17:00:00 | 104.31 |
| 417 | 2009-04-29?18:00:00 | 95.96 |
| 418 | 2009-04-29?19:00:00 | 92.69 |
| 419 | 2009-04-29?20:00:00 | 97.18 |
| 420 | 2009-04-29?21:00:00 | 108.00 |
| 421 | 2009-04-29?22:00:00 | 93.63 |
| 422 | 2009-04-29?23:00:00 | 101.41 |
| 423 | 2009-04-30?00:00:00 | 103.30 |
| 424 | 2009-04-30?01:00:00 | 108.91 |
| 425 | 2009-04-30?02:00:00 | 101.16 |
| 426 | 2009-04-30?03:00:00 | 91.45 |
| 427 | 2009-04-30?04:00:00 | 97.77 |
| 428 | 2009-04-30?05:00:00 | 99.02 |
| 429 | 2009-04-30?06:00:00 | 109.64 |
| 430 | 2009-04-30?07:00:00 | 95.45 |
| 431 | 2009-04-30?08:00:00 | 102.01 |
| 432 | 2009-04-30?09:00:00 | 94.60 |
| 433 | 2009-04-30?10:00:00 | 108.96 |
| 434 | 2009-04-30?11:00:00 | 94.75 |
| 435 | 2009-04-30?12:00:00 | 107.96 |
| 436 | 2009-04-30?13:00:00 | 100.75 |
| 437 | 2009-04-30?14:00:00 | 96.96 |
| 438 | 2009-04-30?15:00:00 | 94.39 |
| 439 | 2009-04-30?16:00:00 | 106.14 |
| 440 | 2009-04-30?17:00:00 | 95.40 |
| 441 | 2009-04-30?18:00:00 | 104.44 |
| 442 | 2009-04-30?19:00:00 | 90.89 |
| 443 | 2009-04-30?20:00:00 | 106.76 |
| 444 | 2009-04-30?21:00:00 | 102.08 |
| 445 | 2009-04-30?22:00:00 | 102.80 |
| 446 | 2009-04-30?23:00:00 | 107.36 |
| 447 | 2009-05-01?00:00:00 | 105.73 |
| 448 | 2009-05-01?01:00:00 | 90.84 |
| 449 | 2009-05-01?02:00:00 | 91.37 |
| 450 | 2009-05-01?03:00:00 | 100.13 |
| 451 | 2009-05-01?04:00:00 | 97.35 |
| 452 | 2009-05-01?05:00:00 | 96.75 |
| 453 | 2009-05-01?06:00:00 | 91.02 |
| 454 | 2009-05-01?07:00:00 | 91.38 |
| 455 | 2009-05-01?08:00:00 | 105.74 |
| 456 | 2009-05-01?09:00:00 | 95.26 |
| 457 | 2009-05-01?10:00:00 | 101.25 |
| 458 | 2009-05-01?11:00:00 | 92.14 |
| 459 | 2009-05-01?12:00:00 | 96.68 |
| 460 | 2009-05-01?13:00:00 | 103.89 |
| 461 | 2009-05-01?14:00:00 | 107.37 |
| 462 | 2009-05-01?15:00:00 | 109.99 |
| 463 | 2009-05-01?16:00:00 | 101.90 |
| 464 | 2009-05-01?17:00:00 | 109.58 |
| 465 | 2009-05-01?18:00:00 | 94.78 |
| 466 | 2009-05-01?19:00:00 | 105.90 |
| 467 | 2009-05-01?20:00:00 | 97.59 |
| 468 | 2009-05-01?21:00:00 | 91.06 |
| 469 | 2009-05-01?22:00:00 | 97.22 |
| 470 | 2009-05-01?23:00:00 | 94.47 |
| 471 | 2009-05-02?00:00:00 | 109.07 |
| 472 | 2009-05-02?01:00:00 | 95.65 |
| 473 | 2009-05-02?02:00:00 | 95.82 |
| 474 | 2009-05-02?03:00:00 | 92.13 |
| 475 | 2009-05-02?04:00:00 | 103.44 |
| 476 | 2009-05-02?05:00:00 | 99.83 |
| 477 | 2009-05-02?06:00:00 | 95.81 |
| 478 | 2009-05-02?07:00:00 | 107.48 |
| 479 | 2009-05-02?08:00:00 | 102.12 |
| 480 | 2009-05-02?09:00:00 | 93.00 |
| 481 | 2009-05-02?10:00:00 | 97.89 |
| 482 | 2009-05-02?11:00:00 | 98.23 |
| 483 | 2009-05-02?12:00:00 | 95.18 |
| 484 | 2009-05-02?13:00:00 | 93.78 |
| 485 | 2009-05-02?14:00:00 | 90.95 |
| 486 | 2009-05-02?15:00:00 | 109.22 |
| 487 | 2009-05-02?16:00:00 | 109.25 |
| 488 | 2009-05-02?17:00:00 | 98.17 |
| 489 | 2009-05-02?18:00:00 | 103.17 |
| 490 | 2009-05-02?19:00:00 | 95.66 |
| 491 | 2009-05-02?20:00:00 | 90.99 |
| 492 | 2009-05-02?21:00:00 | 109.09 |
| 493 | 2009-05-02?22:00:00 | 98.29 |
| 494 | 2009-05-02?23:00:00 | 106.17 |
| 495 | 2009-05-03?00:00:00 | 97.89 |
| 496 | 2009-05-03?01:00:00 | 106.48 |
| 497 | 2009-05-03?02:00:00 | 93.95 |
| 498 | 2009-05-03?03:00:00 | 109.90 |
| 499 | 2009-05-03?04:00:00 | 98.38 |
| 500 | 2009-05-03?05:00:00 | 107.55 |
| 501 | 2009-05-03?06:00:00 | 109.02 |
| 502 | 2009-05-03?07:00:00 | 102.17 |
| 503 | 2009-05-03?08:00:00 | 93.02 |
| 504 | 2009-05-03?09:00:00 | 96.35 |
| 505 | 2009-05-03?10:00:00 | 96.66 |
| 506 | 2009-05-03?11:00:00 | 92.86 |
| 507 | 2009-05-03?12:00:00 | 98.78 |
| 508 | 2009-05-03?13:00:00 | 92.15 |
| 509 | 2009-05-03?14:00:00 | 90.15 |
| 510 | 2009-05-03?15:00:00 | 92.15 |
| 511 | 2009-05-03?16:00:00 | 108.08 |
| 512 | 2009-05-03?17:00:00 | 96.05 |
| 513 | 2009-05-03?18:00:00 | 98.29 |
| 514 | 2009-05-03?19:00:00 | 97.78 |
| 515 | 2009-05-03?20:00:00 | 104.70 |
| 516 | 2009-05-03?21:00:00 | 105.06 |
| 517 | 2009-05-03?22:00:00 | 97.19 |
| 518 | 2009-05-03?23:00:00 | 98.31 |
| 519 | 2009-05-04?00:00:00 | 108.27 |
| 520 | 2009-05-04?01:00:00 | 93.09 |
| 521 | 2009-05-04?02:00:00 | 95.45 |
| 522 | 2009-05-04?03:00:00 | 96.71 |
| 523 | 2009-05-04?04:00:00 | 109.27 |
| 524 | 2009-05-04?05:00:00 | 108.26 |
| 525 | 2009-05-04?06:00:00 | 99.44 |
| 526 | 2009-05-04?07:00:00 | 108.73 |
| 527 | 2009-05-04?08:00:00 | 106.45 |
| 528 | 2009-05-04?09:00:00 | 105.90 |
| 529 | 2009-05-04?10:00:00 | 95.79 |
| 530 | 2009-05-04?11:00:00 | 100.35 |
| 531 | 2009-05-04?12:00:00 | 108.42 |
| 532 | 2009-05-04?13:00:00 | 106.52 |
| 533 | 2009-05-04?14:00:00 | 97.68 |
| 534 | 2009-05-04?15:00:00 | 98.79 |
| 535 | 2009-05-04?16:00:00 | 106.69 |
| 536 | 2009-05-04?17:00:00 | 97.96 |
| 537 | 2009-05-04?18:00:00 | 90.95 |
| 538 | 2009-05-04?19:00:00 | 100.39 |
| 539 | 2009-05-04?20:00:00 | 95.79 |
| 540 | 2009-05-04?21:00:00 | 99.45 |
| 541 | 2009-05-04?22:00:00 | 101.71 |
| 542 | 2009-05-04?23:00:00 | 103.64 |
| 543 | 2009-05-05?00:00:00 | 109.31 |
| 544 | 2009-05-05?01:00:00 | 91.01 |
| 545 | 2009-05-05?02:00:00 | 101.85 |
| 546 | 2009-05-05?03:00:00 | 95.66 |
| 547 | 2009-05-05?04:00:00 | 107.63 |
| 548 | 2009-05-05?05:00:00 | 91.15 |
| 549 | 2009-05-05?06:00:00 | 97.17 |
| 550 | 2009-05-05?07:00:00 | 94.23 |
| 551 | 2009-05-05?08:00:00 | 91.22 |
| 552 | 2009-05-05?09:00:00 | 101.37 |
| 553 | 2009-05-05?10:00:00 | 101.37 |
| 554 | 2009-05-05?11:00:00 | 93.91 |
| 555 | 2009-05-05?12:00:00 | 108.12 |
| 556 | 2009-05-05?13:00:00 | 105.98 |
| 557 | 2009-05-05?14:00:00 | 93.94 |
| 558 | 2009-05-05?15:00:00 | 106.87 |
| 559 | 2009-05-05?16:00:00 | 103.81 |
| 560 | 2009-05-05?17:00:00 | 107.57 |
| 561 | 2009-05-05?18:00:00 | 95.06 |
| 562 | 2009-05-05?19:00:00 | 102.82 |
| 563 | 2009-05-05?20:00:00 | 95.43 |
| 564 | 2009-05-05?21:00:00 | 107.52 |
| 565 | 2009-05-05?22:00:00 | 104.44 |
| 566 | 2009-05-05?23:00:00 | 102.44 |
| 567 | 2009-05-06?00:00:00 | 101.96 |
| 568 | 2009-05-06?01:00:00 | 90.91 |
| 569 | 2009-05-06?02:00:00 | 101.02 |
| 570 | 2009-05-06?03:00:00 | 108.67 |
| 571 | 2009-05-06?04:00:00 | 92.62 |
| 572 | 2009-05-06?05:00:00 | 105.25 |
| 573 | 2009-05-06?06:00:00 | 90.32 |
| 574 | 2009-05-06?07:00:00 | 90.13 |
| 575 | 2009-05-06?08:00:00 | 104.93 |
| 576 | 2009-05-06?09:00:00 | 92.29 |
| 577 | 2009-05-06?10:00:00 | 96.40 |
| 578 | 2009-05-06?11:00:00 | 101.29 |
| 579 | 2009-05-06?12:00:00 | 94.73 |
| 580 | 2009-05-06?13:00:00 | 102.54 |
| 581 | 2009-05-06?14:00:00 | 105.21 |
| 582 | 2009-05-06?15:00:00 | 93.51 |
| 583 | 2009-05-06?16:00:00 | 109.69 |
| 584 | 2009-05-06?17:00:00 | 91.47 |
| 585 | 2009-05-06?18:00:00 | 96.34 |
| 586 | 2009-05-06?19:00:00 | 101.47 |
| 587 | 2009-05-06?20:00:00 | 108.39 |
| 588 | 2009-05-06?21:00:00 | 107.22 |
| 589 | 2009-05-06?22:00:00 | 109.91 |
| 590 | 2009-05-06?23:00:00 | 99.31 |
| 591 | 2009-05-07?00:00:00 | 96.81 |
| 592 | 2009-05-07?01:00:00 | 108.85 |
| 593 | 2009-05-07?02:00:00 | 105.53 |
| 594 | 2009-05-07?03:00:00 | 90.88 |
| 595 | 2009-05-07?04:00:00 | 103.95 |
| 596 | 2009-05-07?05:00:00 | 104.63 |
| 597 | 2009-05-07?06:00:00 | 100.20 |
| 598 | 2009-05-07?07:00:00 | 108.50 |
| 599 | 2009-05-07?08:00:00 | 108.79 |
| 600 | 2009-05-07?09:00:00 | 109.82 |
| 601 | 2009-05-07?10:00:00 | 102.09 |
| 602 | 2009-05-07?11:00:00 | 104.49 |
| 603 | 2009-05-07?12:00:00 | 100.06 |
| 604 | 2009-05-07?13:00:00 | 93.15 |
| 605 | 2009-05-07?14:00:00 | 106.97 |
| 606 | 2009-05-07?15:00:00 | 90.02 |
| 607 | 2009-05-07?16:00:00 | 100.97 |
| 608 | 2009-05-07?17:00:00 | 91.53 |
| 609 | 2009-05-07?18:00:00 | 94.17 |
| 610 | 2009-05-07?19:00:00 | 105.50 |
| 611 | 2009-05-07?20:00:00 | 100.77 |
| 612 | 2009-05-07?21:00:00 | 102.26 |
| 613 | 2009-05-07?22:00:00 | 109.07 |
| 614 | 2009-05-07?23:00:00 | 96.95 |
| 615 | 2009-05-08?00:00:00 | 104.82 |
| 616 | 2009-05-08?01:00:00 | 92.18 |
| 617 | 2009-05-08?02:00:00 | 108.85 |
| 618 | 2009-05-08?03:00:00 | 102.75 |
| 619 | 2009-05-08?04:00:00 | 105.21 |
| 620 | 2009-05-08?05:00:00 | 93.08 |
| 621 | 2009-05-08?06:00:00 | 98.46 |
| 622 | 2009-05-08?07:00:00 | 105.12 |
| 623 | 2009-05-08?08:00:00 | 103.84 |
| 624 | 2009-05-08?09:00:00 | 102.82 |
| 625 | 2009-05-08?10:00:00 | 93.65 |
| 626 | 2009-05-08?11:00:00 | 90.65 |
| 627 | 2009-05-08?12:00:00 | 109.62 |
| 628 | 2009-05-08?13:00:00 | 101.42 |
| 629 | 2009-05-08?14:00:00 | 97.96 |
| 630 | 2009-05-08?15:00:00 | 94.37 |
| 631 | 2009-05-08?16:00:00 | 101.93 |
| 632 | 2009-05-08?17:00:00 | 101.66 |
| 633 | 2009-05-08?18:00:00 | 90.51 |
| 634 | 2009-05-0819:00:00 | 91.61 |
| 635 | 2009-05-08?20:00:00 | 101.99 |
| 636 | 2009-05-08?21:00:00 | 103.34 |
| 637 | 2009-05-08?22:00:00 | 91.51 |
| 638 | 2009-05-08?23:00:00 | 92.16 |
| 639 | 2009-05-09?00:00:00 | 104.21 |
| 640 | 2009-05-09?01:00:00 | 90.86 |
| 641 | 2009-05-09?02:00:00 | 102.31 |
| 642 | 2009-05-09?03:00:00 | 100.95 |
| 643 | 2009-05-09?04:00:00 | 109.18 |
| 644 | 2009-05-09?05:00:00 | 103.17 |
| 645 | 2009-05-09?06:00:00 | 106.91 |
| 646 | 2009-05-09?07:00:00 | 99.77 |
| 647 | 2009-05-09?08:00:00 | 90.42 |
| 648 | 2009-05-09?09:00:00 | 95.80 |
| 649 | 2009-05-09?10:00:00 | 91.80 |
| 650 | 2009-05-09?11:00:00 | 94.31 |
| 651 | 2009-05-09?12:00:00 | 96.52 |
| 652 | 2009-05-09?13:00:00 | 104.06 |
| 653 | 2009-05-09?14:00:00 | 90.99 |
| 654 | 2009-05-09?15:00:00 | 100.94 |
| 655 | 2009-05-09?16:00:00 | 100.75 |
| 656 | 2009-05-09?17:00:00 | 106.94 |
| 657 | 2009-05-09?18:00:00 | 93.11 |
| 658 | 2009-05-09?19:00:00 | 97.60 |
| 659 | 2009-05-09?20:00:00 | 99.90 |
| 660 | 2009-05-09?21:00:00 | 101.07 |
| 661 | 2009-05-09?22:00:00 | 97.43 |
| 662 | 2009-05-09?23:00:00 | 93.10 |
| 663 | 2009-05-10?00:00:00 | 94.23 |
| 664 | 2009-05-10?01:00:00 | 104.05 |
| 665 | 2009-05-10?02:00:00 | 95.74 |
| 666 | 2009-05-10?03:00:00 | 99.40 |
| 667 | 2009-05-10?04:00:00 | 90.43 |
| 668 | 2009-05-10?05:00:00 | 96.65 |
| 669 | 2009-05-10?06:00:00 | 106.93 |
| 670 | 2009-05-10?07:00:00 | 100.99 |
| 671 | 2009-05-10?08:00:00 | 99.53 |
| 672 | 2009-05-10?09:00:00 | 103.05 |
| 673 | 2009-05-10?10:00:00 | 101.05 |
| 674 | 2009-05-10?11:00:00 | 98.63 |
| 675 | 2009-05-10?12:00:00 | 91.49 |
| 676 | 2009-05-10?13:00:00 | 98.23 |
| 677 | 2009-05-10?14:00:00 | 92.03 |
| 678 | 2009-05-10?15:00:00 | 100.55 |
| 679 | 2009-05-10?16:00:00 | 95.43 |
| 680 | 2009-05-10?17:00:00 | 92.98 |
| 681 | 2009-05-10?18:00:00 | 94.41 |
| 682 | 2009-05-10?19:00:00 | 93.95 |
| 683 | 2009-05-10?20:00:00 | 109.14 |
| 684 | 2009-05-10?21:00:00 | 95.89 |
| 685 | 2009-05-10?22:00:00 | 108.43 |
| 686 | 2009-05-10?23:00:00 | 95.18 |
| 687 | 2009-05-11?00:00:00 | 108.08 |
| 688 | 2009-05-11?01:00:00 | 97.19 |
| 689 | 2009-05-11?02:00:00 | 96.63 |
| 690 | 2009-05-11?03:00:00 | 97.60 |
| 691 | 2009-05-11?04:00:00 | 95.34 |
| 692 | 2009-05-11?05:00:00 | 106.04 |
| 693 | 2009-05-11?06:00:00 | 99.73 |
| 694 | 2009-05-11?07:00:00 | 95.58 |
| 695 | 2009-05-11?08:00:00 | 108.23 |
| 696 | 2009-05-11?09:00:00 | 95.65 |
| 697 | 2009-05-11?10:00:00 | 91.00 |
| 698 | 2009-05-11?11:00:00 | 98.08 |
| 699 | 2009-05-11?12:00:00 | 102.16 |
| 700 | 2009-05-11?13:00:00 | 99.03 |
| 701 | 2009-05-11?14:00:00 | 102.73 |
| 702 | 2009-05-11?15:00:00 | 96.45 |
| 703 | 2009-05-11?16:00:00 | 93.95 |
| 704 | 2009-05-11?17:00:00 | 104.86 |
| 705 | 2009-05-11?18:00:00 | 91.65 |
| 706 | 2009-05-11?19:00:00 | 100.66 |
| 707 | 2009-05-11?20:00:00 | 96.09 |
| 708 | 2009-05-11?21:00:00 | 92.67 |
| 709 | 2009-05-11?22:00:00 | 100.18 |
| 710 | 2009-05-11?23:00:00 | 108.33 |
As can be seen from Table 4, this monitor was tested 24 times from every day on May 11st, 12 days 1 April in 2009, did not break down, and MTBF (average non-failure operation time) 720 hours satisfies the requirement of company standard fully.
Claims (9)
1. reagent constant volume method is characterized in that: adopt the constant volume cup of band constant volume line, the place of flushing is provided with the reagent refluxing opening in constant volume line horizontal direction, and the above reagent of constant volume line is derived from refluxing opening, and remaining reagent promptly is the reagent that passes through constant volume in the constant volume cup; The outlet of adopting the delivery of therapeutic agents conduit will need the reagent of constant volume to import in the constant volume cup as refluxing opening during constant volume, guarantee that liquid level surpasses the constant volume line; Again the reagent more than the constant volume line is derived from refluxing opening.
2. reagent constant volume method according to claim 1 is characterized in that: will need the reagent of constant volume to import the constant volume cup from the reagent storage bottle by the reagent delivery conduit, and again the reagent more than the constant volume line be led back the reagent corresponding storage bottle.
3. reagent constant volume method according to claim 2 is characterized in that: adopt many raceways peristaltic pump delivery of therapeutic agents.
4.CODcr monitoring method is characterized in that may further comprise the steps:
A, each described constant volume method of employing claim 1～3 are with water sample to be measured, potassium dichromate digestion solution, catalyzer constant volume in constant volume cup separately; Described catalyzer is the mixed liquor of the silver sulfate and the concentrated sulphuric acid;
Each reagent through constant volume in b, the constant volume cup is delivered to mixing reactor, and reaction back colorimetric estimation Cr is cleared up in heating
3+Content, thus converse CODcr.
5. CODcr monitoring method according to claim 4 is characterized in that: the temperature that reaction is cleared up in the heating of b step is 165 ± 2 ℃, colorimetric estimation Cr
3+At wavelength 610nm.
6. CODcr monitoring method according to claim 5 is characterized in that may further comprise the steps:
A, assembling: will react the entrance point that required each reagent storage bottle is connected peristaltic pump by the constant volume conduit, the constant volume cup is connected the endpiece of peristaltic pump by the constant volume conduit;
B, set the volume clear up required each reagent of reaction respectively; Constant volume cup to each reagent carries out volume calibration, marks the constant volume line at the constant volume wall of cup, and the constant volume conduit outlet is flushed with constant volume line separately;
C, peristaltic pump are just changeing in each reagent importing constant volume cup separately, guarantee that each reagent liquid level surpasses constant volume line separately, by peristaltic pump counter-rotating the reagent more than the constant volume line is led back separately reagent reservoir bottle then, remaining reagent promptly is the reagent that passes through constant volume in the constant volume cup;
Each reagent through constant volume in d, the constant volume cup is delivered to mixing reactor by the reaction conduit, is heated to 165 ± 2 ℃ and fully clears up reaction, Cr
6+Be reduced to Cr
3+, at wavelength 610nm place, colorimetric estimation Cr
3+Content, thus converse CODcr.
7. CODcr monitoring method according to claim 6 is characterized in that: react required reagent and also comprise distilled water.
8. CODcr monitoring method according to claim 7 is characterized in that: described peristaltic pump is 4 raceway peristaltic pumps, carries water sample to be measured, potassium dichromate digestion solution, catalyzer, distilled water simultaneously.
9.CODcr online automatic monitor, comprise one 4 raceway peristaltic pump, water sample to be measured, potassium dichromate digestion solution, catalyzer, distilled water reagent storage bottle separately and corresponding separately constant volume cup, 1 reactor, and 1 colorimetric estimation system and computer control system; Wherein on each constant volume wall of cup the constant volume line is arranged, each reagent storage bottle and corresponding separately constant volume cup are connected on the 4 raceway peristaltic pumps by the constant volume conduit respectively, and the constant volume conduit outlet flushes with the constant volume line, and each constant volume cup is delivered to reactor by the reaction conduit respectively; Adopt the colorimetric estimation system to detect titration end-point, by computer system control colorimetric titration system and calculate CODcr.
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| KR101869090B1 (en) | 2013-08-08 | 2018-06-20 | 일루미나, 인코포레이티드 | Fluidic system for reagent delivery to a flow cell |
| CN105067543A (en) * | 2015-07-29 | 2015-11-18 | 安徽古井贡酒股份有限公司 | Method for determining COD of pot bottom water through rapid unsealed catalytic digestion |
| CN106289432B (en) * | 2016-08-08 | 2023-12-12 | 江苏省农业科学院 | Digestion liquid batch transfer constant volume device for wet digestion and control module thereof |
| CN110726717A (en) * | 2019-09-27 | 2020-01-24 | 厦门金越电器有限公司 | Rapid semi-quantitative detection method for COD in wastewater |
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