CN102253232B - Automatic analyzer and analysis method for water soluble total phosphorus - Google Patents
Automatic analyzer and analysis method for water soluble total phosphorus Download PDFInfo
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Abstract
The invention discloses a full-automatic analyzer and an analysis method for water soluble total phosphorus. The analyzer comprises a sample injection device and a color development detection device, wherein the sample injection device comprises an automatic sample injection device, a multi-way valve and a first peristaltic pump; the first peristaltic pump is provided with a first pump pipe; and the color development detection device comprises a second peristaltic pump, a first container bottle, a second container bottle, a third container bottle, a fourth container bottle, a fifth container bottle, a sampling ring, a first knitted reactor, a first three-way valve, a high temperature online heating module, a second three-way valve, a second knitted reactor, a first two-way valve, an ultraviolet digestion module, a third three-way valve, a third knitted reactor, a fourth three-way valve, a low temperature online heating module, a flowing pool, a detector, a data connection cable, a computer processing system, a waste liquid trough, a second backpressure adjuster and a plurality of capillaries. By the automatic analyzer and the analysis method for the water soluble total phosphorus, samples can be tested automatically and continuously, and the test is accurate and quick.
Description
Technical field
The present invention relates to a kind of full-automatic flow injection analyzer and analytical approach thereof, relate in particular to fully-automatic analyzer and the analytical approach thereof of dissolubility total phosphorus in a kind of water.
Background technology
The analysis of dissolubility total phosphorus in water, in national standard method GB11893-89, use pressure cooker to clear up rear ammonium molybdate spectrophotometric method, this method need to be used high pressure steam boiler in advance in the time of 120 ℃, after sample is heated to 30min, the phosphate of various forms in water sample is cleared up for being measured after orthophosphate, in the process of mensuration, progressively be added ascorbic acid solution and molybdate solution, after at room temperature placing 15 minutes, under the 700nm wavelength, measure absorbance.Sample of methods analyst in GB at least needs the time of 45min, and a big chunk time loss is in the pre-treatment of sample; In the process of measuring, if room temperature is lower, also need to promote with the water-bath of 20～30 ℃ the generation of chromogenic reaction.
Simple, convenient with it for Flow Injection Analysis, easily realize robotization and can carry out online the characteristics of pre-treatment to sample, be widely used at present (Ruzicka J, Hansen E H in chemical analysis, Flow Injection Analysis, Wiley, NewYork, 1981; Fang Zhaolun, flow injection analysis, Beijing: Science Press, 1999).With the dissolubility total phosphorus in flow injection methods analyst water, commercial import instrument is arranged at present, but its method detection limit higher (generally in 100 μ g/L left and right), and the Environmental Protection in China monitoring requires detection limit to be less than 20 μ g/L, its import instrument can not meet the demand of actual monitoring work.
Summary of the invention
The purpose of this invention is to provide and a kind ofly continuously and automatically sample is tested, test accurately fast, detectability is less than fully-automatic analyzer and the analytical approach thereof of dissolubility total phosphorus in the water of 20 μ g/L.
Full-automatic flow injection analyzer provided by the present invention, comprise sampling device and color developing detection device;
Described sampling device comprises automatic sampling apparatus, the first peristaltic pump, described the first peristaltic pump is provided with the first pump line, the sample introduction needle of described automatic sampling apparatus is connected with the F port of multiport valve by described the first pump line, and the A port of described multiport valve is connected with waste liquid tank by the first back pressure regulator;
Described color developing detection device, comprise the second peristaltic pump, the first container bottle, the second container bottle, the 3rd container bottle, the 4th container bottle, the 5th container bottle, sampling ring, multiport valve, the first knitting reactor, the first T-valve, high temperature on-line heating module, the second T-valve, the second knitting reactor, the first two-way valve, the ultraviolet digestion module, the 3rd T-valve, the 3rd knitting reactor, the 4th T-valve, low temperature on-line heating module, flow cell, detecting device, data stube cable and computer processing system, waste liquid tank, the second back pressure regulator and some kapillaries, the second peristaltic pump is provided with the second pump line, the 3rd pump line, the 4th pump line, the 5th pump line, the 6th pump line, the first container bottle, the second pump line, the D port of multiport valve connects by kapillary successively, the C port of multiport valve, the first knitting reactor, an import of the first T-valve connects by kapillary successively, the outlet of the first T-valve, high temperature on-line heating module, an import of the second T-valve connects by kapillary successively, the outlet of the second T-valve, the second knitting reactor, the first two-way valve, the ultraviolet digestion module, an import of the 3rd T-valve connects by kapillary successively, the outlet of the 3rd T-valve, the 3rd knitting reactor, an import of the 4th T-valve connects by kapillary successively, the outlet of the 4th T-valve, low temperature on-line heating module, flow cell, the second back pressure regulator, waste liquid tank connects by kapillary successively, detecting device, the data stube cable is connected successively with computer processing system, and the two ends of sampling ring are connected to B port and the E port of multiport valve, second container bottle, the 3rd pump line, another import of the first T-valve connects by kapillary successively, the 3rd container bottle, the 4th pump line, another import of the second T-valve connects by kapillary successively, the 4th container bottle, the 5th pump line, another import of the 3rd T-valve connects by kapillary successively, the 5th container bottle, the 6th pump line, another import of the 4th T-valve connects by kapillary successively.
Full-automatic flow injection analyzer of the present invention, wherein, described high temperature on-line heating module or described low temperature on-line heating module comprise heating rod, be sleeved on the outer good aluminium body of heat transfer property of heating rod, be wrapped in the teflon heated capillary and the thermometric thermal resistance that form the reaction pipeline of heating on the aluminium body, and being coated on the external muff of aluminium, thermal resistance is ceramic platinum resistance Pt100 or copper resistance Cu50 etc.
Full-automatic flow injection analyzer of the present invention, wherein, described ultraviolet solution is cleared up module, and ultraviolet lamp tube is arranged on the ultraviolet lamp socket, and kapillary is wrapped in outside ultraviolet lamp tube, and ultraviolet lamp tube is electrically connected to power supply.
Full-automatic flow injection analyzer of the present invention, wherein, described automatic sampling apparatus comprises sample introduction needle, test tube, sample disc, sample introduction needle service sink and pipeline-cleaning pond; The upper end of described sample introduction needle is connected with the capillary connecting pipe with described the first pump line.
Full-automatic flow injection analyzer of the present invention, wherein, the internal diameter of described the first pump line, described the second pump line, described the 3rd pump line, described the 4th pump line, described the 5th pump line and described the 6th pump line is 0.38～1.85mm.
Full-automatic flow injection analyzer of the present invention, wherein, the capillary pipe length of described the first knitting reactor is 0.5～1.5m; The capillary pipe length of described the second knitting reactor is 2～5m; The capillary pipe length of described the 3rd knitting reactor is 0.5～3m; The capillary pipe length of described high temperature on-line heating module is 5～15m; The capillary pipe length of described ultraviolet digestion module is 2～10m; The capillary pipe length of described low temperature on-line heating module is 1～5m; The capillary pipe length of described sampling ring is 1～4m.
In water provided by the present invention, the full-automatic Flow Injection Analysis Method of dissolubility total phosphorus, comprise the steps:
Testing sample mixes with 100～150 ℃ of volumn concentration 5～20% sulfuric acid solutions;
Mixed solution and 20～30g/L potassium persulfate solution hybrid reaction;
Reacted solution carries out the ultraviolet digestion reaction, the reacted solution of ultraviolet digestion and chromogenic reagent solution hybrid reaction;
After the developer hybrid reaction, with 50～100g/L ascorbic acid solution, mix, after mixing, 30～50 ℃ are reacted, and reacted liquid carries out colorimetric estimation at 700～880nm place;
The solution that described developer is ammonium molybdate, potassium antimony tartrate and NaOH potpourri, described ammonium molybdate concentration is 5～12g/L, and the concentration of described potassium antimony tartrate is 0.1～0.4g/L, and the concentration of described NaOH is 65～105g/L.
In water of the present invention, the automatic analyzer of dissolubility total phosphorus and analytical approach thereof, with the dissolubility total phosphorus in flow injection methods analyst water, can be tested sample continuously and automatically, detect and are limited to 2 μ g/L, and test accurately fast.
The accompanying drawing explanation
The structural representation that Fig. 1 is the fully-automatic analyzer of dissolubility total phosphorus in water of the present invention.
The structural representation that Fig. 2 is high temperature on-line heating module or low temperature on-line heating module.
Fig. 3 is the structural representation that the ultraviolet solution is cleared up module.
Embodiment
Automatic analyzer below in conjunction with Figure of description to dissolubility total phosphorus in water of the present invention is described further.
Referring to Fig. 1, the automatic analyzer of dissolubility total phosphorus in water of the present invention, comprise sampling device and color developing detection device;
Sampling device comprises automatic sampling apparatus 1, multiport valve 20, the first peristaltic pump 11, described the first peristaltic pump 11 is provided with the first pump line 12, the sample introduction needle 5 of automatic sampling apparatus is connected with the F port of multiport valve 20 by the first pump line 12, and the A port of multiport valve 20 is connected with waste liquid tank 36 by the first back pressure regulator 37.
Automatic sampling apparatus 1 comprises sample introduction needle 5, sample disc 4, sample introduction needle service sink 3 and pipeline-cleaning pond 2;
The color developing detection device, comprise the second peristaltic pump 18, the first container bottle 38, second container bottle 7, the 3rd container bottle 8, the 4th container bottle 9, the 5th container bottle 10, sampling ring 19, the first knitting reactor 21, the first T-valve 22, high temperature on-line heating module 23, the second T-valve 24, the second knitting reactor 25, the first two-way valve 26, ultraviolet digestion module 27, the 3rd T-valve 28, the 3rd knitting reactor 29, the 4th T-valve 30, low temperature on-line heating module 31, flow cell 32, detecting device 33, data stube cable 35 and computer processing system 34, waste liquid tank 36, the second back pressure regulator 39 and some kapillaries.The second peristaltic pump is provided with the second pump line 13, the 3rd pump line 14, the 4th pump line 15, the 5th pump line 16, the 6th pump line 17.The first container bottle 38, the second pump line 13, the D port of multiport valve 20 connects by kapillary successively, the C port of multiport valve 20, the first knitting reactor 21, an import of the first T-valve 22 connects by kapillary successively, the outlet of the first T-valve 22, high temperature on-line heating module 23, an import of the second T-valve 24 connects by kapillary successively, the outlet of the second T-valve 24, the second knitting reactor 25, the first two-way valve 26, ultraviolet digestion module 27, an import of the 3rd T-valve 28 connects by kapillary successively, the outlet of the 3rd T-valve 28, the 3rd knitting reactor 29, an import of the 4th T-valve 30 connects by kapillary successively, the outlet of the 4th T-valve 30, low temperature on-line heating module 31, flow cell 32, the second back pressure regulator 39, waste liquid tank 36 connects by kapillary successively, detecting device 33, data stube cable 35 is connected successively with computer processing system 34, and the two ends of sampling ring 19 are connected to B port and the E port of multiport valve 20, second container bottle 7, the 3rd pump line 14, another import of the first T-valve 22 connects by kapillary successively, the 3rd container bottle 8, the 4th pump line 15, another import of the second T-valve 24 connects by kapillary successively, the 4th container bottle 9, the 5th pump line 16, another import of the 3rd T-valve 28 connects by kapillary successively, the 5th container bottle 10, the 6th pump line 17, another import of the 4th T-valve 28 connects by kapillary successively.
High temperature on-line heating module 23 or low temperature on-line heating module 31 are with reference to Fig. 2, comprise heating rod 46, be sleeved on the outer good aluminium body 44 of heat transfer property of heating rod, be wrapped in the teflon heated capillary 48 and the thermometric thermal resistance 45 that form the reaction pipeline of heating on the aluminium body, and being coated on the external muff of aluminium 47, thermal resistance 45 is ceramic platinum resistance Pt100 or copper resistance Cu50 etc.
Ultraviolet is cleared up module 27 structures with reference to Fig. 3 in solution, and ultraviolet lamp tube 52 is arranged on ultraviolet lamp socket 53, and kapillary 51 is wrapped in outside ultraviolet lamp tube 52, and ultraviolet lamp tube 52 is electrically connected to power supply.The wavelength of uviol lamp is 254nm, and power is 8-24W.
The first peristaltic pump 11, the second peristaltic pump 18 pump line internal diameters are 0.38～1.85mm, and pump speed is 15～60 rev/mins.The first knitting reactor 21 capillary pipe lengths are 0.5～1.5m; The second knitting reactor 25 capillary pipe lengths are 2～5m, are wrapped on the bobbin winder bracket of metal; The 3rd knitting reactor 29 capillary pipe lengths are 0.5～3m; The capillary pipe length of high temperature on-line heating module 23 is 5～15m, and the capillary pipe length of ultraviolet digestion module 27 is 2～10m, and the capillary pipe length of low temperature on-line heating module 31 is 1～5m; The capillary pipe length of sampling ring 19 is 1～4m.The temperature of high temperature on-line heating module 23 is 100～150 ℃, and the temperature of low temperature on-line heating module 31 is 30～50 ℃, and the wavelength of ultraviolet digestion module 27 is 200～300nm, and power is 8～20w.The present invention's internal diameter capillaceous used is 0.5～1.0mm, and multiport valve is the multiport valve with 6～24 ports, and the light path of flow cell is 10～50mm, and the detection wavelength of detecting device is 700～880nm.
Fill deionized water in the first container bottle 38; Dress Sulfuric-Acid Digestion liquid in second container bottle 7, the concentration of sulfuric acid is 5～20% (volumn concentrations); Fill potassium persulfate solution in the 3rd container bottle 8, the concentration of potassium persulfate is 20～30g/L; Fill developer in the 4th container bottle 9, the solution that developer is ammonium molybdate, potassium antimony tartrate and NaOH potpourri, ammonium molybdate concentration is 5～12g/L, the concentration that the concentration of potassium antimony tartrate is 0.1～0.4g/L, NaOH is 65～105g/L; The concentration that fills ascorbic acid solution, ascorbic acid in the 5th container bottle 10 is 50～100g/L.
In water of the present invention, the course of work of the automatic analyzer of dissolubility total phosphorus is as follows:
Sample after filtering is placed in sample hose 6, by automatic sampling apparatus 1 under the effect of peristaltic pump 11 through the first pump line 12, enter the sampling ring 19 connected on six-way valve 20, sampling ring 19 is full of by the direct waste discharge of the first back pressure regulator 37 and enters waste liquid bottle 36.After sampling process finishes, six-way valve 20 turns to the state shown in dotted line in figure, peristaltic pump 18 pumps into current-carrying solution, sample in sampling ring 19 is released, in the first knitting reactor 21, mix, enter in the first T-valve 22 and converge with sulfuric acid solution, in high temperature on-line heating module 23, mixed, mixed solution converges with potassium persulfate solution in the second T-valve 24, reaction in the second knitting reactor 25, reacted solution is through the first two-way valve 26, enter ultraviolet digestion module 27, reacted solution advances in the 3rd T-valve 28 and converges with chromogenic reagent solution, reaction in the 3rd knitting reactor 29, entering the 4th T-valve 30 after mixing converges with ascorbic acid solution, enter after mixing in low temperature on-line heating module 31 and reacted, reacted liquid is in the pond 32 that circulates, carry out colorimetric estimation by detecting device 33 at 700～880nm place, the liquid flowed out directly enters waste liquid bottle 36 through the second back pressure regulator 39.
In using water of the present invention during the automatic analyzer of dissolubility total phosphorus, standard solution and sample are poured into respectively in the sample hose of automatic sampling apparatus, get final product automatic analysis, do typical curve according to absorbance peak height or the peak area of the standard solution recorded, absorbance peak height value or peak area value per sample can calculate the content of dissolubility total phosphorus in sample on typical curve.
Adopt automatic analyzer of the present invention to be tested, the sample fillup valve is six-way valve, the capillary inner diameter of stream is 0.8mm, in the analyzing and testing stream, the capillary pipe length of the first knitting reactor 21 is 1m, the capillary pipe length of the second knitting reactor 25 is 3m, the capillary pipe length of the 3rd knitting reactor 29 is 2.5m, and the length of other capillary connecting pipe is 0.5m, and the length of sampling ring 19 is 1m.The light path of flow cell 32 is 10mm, and in high-temperature heating module 23, capillary pipe length is 4m, 125 ℃ of heating-up temperatures; In low-temperature heat module 31, capillary pipe length is 4m, 37 ℃ of heating-up temperatures, and the capillary pipe length of ultraviolet digestion module is 6m, power is 8W, at the 880nm place, is measured.
1, the preparation of standard specimen
Preparation of standard sample: take 4.396g in 110 ℃ of dry 2h the anhydrous potassium dihydrogenphosphate (KH that lets cool in exsiccator
2pO
4), shifting and be settled to the 1000ml volumetric flask after water dissolves, the phosphorus storing solution that is mixed with 1000mg P/L is standby.
By the phosphorus storing solution deionized water stepwise dilution of 1000mg/L, be configured to 0.0,0.01,0.02,0.05,0.1,0.2,0.4, the 1.0mg/L standard series.
2, the preparation of reagent
In the present embodiment, testing sample mixes with 125 ℃ of volumn concentration 10% sulfuric acid solutions;
Mixed solution and 23.78g/L potassium persulfate solution hybrid reaction;
Reacted solution carries out the ultraviolet digestion reaction, the reacted solution of ultraviolet digestion and chromogenic reagent solution hybrid reaction;
Mix with the 80g/L ascorbic acid solution after the developer hybrid reaction, mix latter 47.5 ℃ and reacted, reacted liquid carries out colorimetric estimation at the 880nm place;
The solution that described developer is ammonium molybdate, potassium antimony tartrate and NaOH potpourri, described ammonium molybdate concentration is 7g/L, and the concentration of described potassium antimony tartrate is 0.34g/L, and the concentration of described NaOH is 90g/L.
Agents useful for same all adopts domestic reagent, and the purity of reagent is minimum pure for analyzing.
3, sample introduction
Draw sample in the sample hose 6 of sample introduction needle 5 from be inserted in sample disc 4, sample pumps into sample fillup valve 20 by peristaltic pump, and after sample is full of sampling ring 19, unnecessary sample enters waste liquid tank 36.
4, response measurement
Sample after filtering is placed in sample hose 6, by automatic sampling apparatus 1 under the effect of peristaltic pump 11 through the first pump line 12, enter the sampling ring 19 connected on six-way valve 20, sampling ring 19 is full of by the direct waste discharge of the first back pressure regulator 37 and enters waste liquid bottle 36.After sampling process finishes, six-way valve 20 turns to the state shown in dotted line in figure, peristaltic pump 18 pumps into current-carrying solution, sample in sampling ring 19 is released, in the first knitting reactor 21, mix, enter in the first T-valve 22 and converge with sulfuric acid solution, in high temperature on-line heating module 23, mixed, mixed solution converges with potassium persulfate solution in the second T-valve 24, reaction in the second knitting reactor 25, reacted solution is through the first two-way valve 26, enter ultraviolet digestion module 27, reacted solution advances in the 3rd T-valve 28 and converges with chromogenic reagent solution, reaction in the 3rd knitting reactor 29, entering the 4th T-valve 30 after mixing converges with ascorbic acid solution, enter after mixing in low temperature on-line heating module 31 and reacted, reacted liquid is in the pond 32 that circulates, carry out colorimetric estimation by detecting device 33 at 700～880nm place, the liquid flowed out directly enters waste liquid bottle 36 through the second back pressure regulator 39.
The test result that table 1 is standard model, the test result that table 2 is actual sample, the Precision test result that table 3 is measured for actual sample.
The test result of table 1. standard model
Dissolubility total phosphorus content measurement result in table 2. actual sample
| Concentration (μ g/L) recovery (%) tap water 11.8 10.0 21.1 92.9 surface water 66.3 10.0 75.9 95.6 underground water 4.2 10.0 14.0 97.3 sewage (diluting 10 times) 273.5 400.0 663.1 97.4 after sample title sample concentration (μ g/L) mark-on concentration (μ g/L) mark-on |
Dissolubility total phosphorus content measurement result in table 3. actual sample
| RSD measures the number of times absorbance, (peak height) absorbance, (peak area) returns and calculates concentration, (μ g/L) 1 0.0105 3.655 101.411 2 0.0106 3.677 101.961 3 0.0104 3.634 100.885 4 0.0105 3.663 101.603 5 0.0106 3.633 100.84 6 0.0104 3.632 100.825 7 0.0104 3.648 101.222 |
The range of linearity of method is 0.01～2.0mg P/L, and linearly dependent coefficient r >=0.999 detects and is limited to 0.002mg P/L, and the recovery of standard addition of actual water sample is 90%～110%; Precision is high, and the sample relative standard deviation of 0.1mg P/L is 0.43%.
Above embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (7)
1. the fully-automatic analyzer of dissolubility total phosphorus in a water, is characterized in that: comprise sampling device and color developing detection device;
Described sampling device comprises automatic sampling apparatus (1), the first peristaltic pump (11) and multiport valve (20), described the first peristaltic pump (11) is provided with the first pump line (12), the sample introduction needle (5) of described automatic sampling apparatus (1) is connected with the F port of multiport valve (20) by described the first pump line (12), and the A port of described multiport valve (20) is connected with waste liquid tank (36) by the first back pressure regulator (37);
Described color developing detection device, comprise the second peristaltic pump (18), the first container bottle (38), second container bottle (7), the 3rd container bottle (8), the 4th container bottle (9), the 5th container bottle (10), sampling ring (19), the first knitting reactor (21), the first T-valve (22), high temperature on-line heating module (23), the second T-valve (24), the second knitting reactor (25), the first two-way valve (26), ultraviolet digestion module (27), the 3rd T-valve (28), the 3rd knitting reactor (29), the 4th T-valve (30), low temperature on-line heating module (31), flow cell (32), detecting device (33), data stube cable (35) and computer processing system (34), waste liquid tank (36), the second back pressure regulator (39) and some kapillaries, the second peristaltic pump is provided with the second pump line (13), the 3rd pump line (14), the 4th pump line (15), the 5th pump line (16), the 6th pump line (17), the first container bottle (38), the second pump line (13), the D port of multiport valve (20) connects by kapillary successively, the C port of multiport valve (20), the first knitting reactor (21), an import of the first T-valve (22) connects by kapillary successively, the outlet of the first T-valve (22), high temperature on-line heating module (23), an import of the second T-valve (24) connects by kapillary successively, the outlet of the second T-valve (24), the second knitting reactor (25), the first two-way valve (26), ultraviolet digestion module (27), an import of the 3rd T-valve (28) connects by kapillary successively, the outlet of the 3rd T-valve (28), the 3rd knitting reactor (29), an import of the 4th T-valve (30) connects by kapillary successively, the outlet of the 4th T-valve (30), low temperature on-line heating module (31), flow cell (32), the second back pressure regulator (39), waste liquid tank (36) connects by kapillary successively, detecting device (33), data stube cable (35) is connected successively with computer processing system (34), and the two ends of sampling ring (19) are connected to B port and the E port of multiport valve (20), second container bottle (7), the 3rd pump line (14), another import of the first T-valve (22) connects by kapillary successively, the 3rd container bottle (8), the 4th pump line (15), another import of the second T-valve (24) connects by kapillary successively, the 4th container bottle (9), the 5th pump line (16), another import of the 3rd T-valve (28) connects by kapillary successively, the 5th container bottle (10), the 6th pump line (17), another import of the 4th T-valve (28) connects by kapillary successively.
2. fully-automatic analyzer according to claim 1, it is characterized in that: described high temperature on-line heating module (23) and described low temperature on-line heating module (31) include heating rod (46), be sleeved on the outer good aluminium body of heat transfer property (44) of heating rod (46), be wrapped in upper teflon heated capillary (48) and the thermometric thermal resistance (45) that forms the reaction pipeline of heating of aluminium body (44), and being coated on the outer muff (47) of aluminium body (44), thermal resistance (45) is ceramic platinum resistance Pt100 or copper resistance Cu50.
3. fully-automatic analyzer according to claim 1 and 2, it is characterized in that: the ultraviolet lamp tube (52) of described ultraviolet digestion module (27) is arranged on ultraviolet lamp socket (53), be wound with kapillary (51) outside described ultraviolet lamp tube (52), described ultraviolet lamp tube (52) is electrically connected to power supply.
4. fully-automatic analyzer according to claim 3 is characterized in that: described automatic sampling apparatus (1) comprises sample introduction needle (5), sample disc (4), sample introduction needle service sink (3), test tube (6) and pipeline-cleaning pond (2); The upper end of described sample introduction needle (5) is connected with kapillary with described the first pump line (12).
5. fully-automatic analyzer according to claim 4, it is characterized in that: the internal diameter of described the first pump line (12), described the second pump line (13), described the 3rd pump line (14), described the 4th pump line (15), described the 5th pump line (16) and described the 6th pump line (17) is 0.38 ~ 1.85mm.
6. fully-automatic analyzer according to claim 5, it is characterized in that: in described the first knitting reactor, capillary pipe length is 0.5 ~ 1.5m; In described the second knitting reactor, capillary pipe length is 2 ~ 5m; In described the 3rd knitting reactor, capillary pipe length is 0.5 ~ 3m; In described high temperature on-line heating module, capillary pipe length is 5 ~ 15m; In described ultraviolet digestion module, capillary pipe length is 2 ~ 10m; In described low temperature on-line heating module, capillary pipe length is 1 ~ 5m; In described sampling ring, capillary pipe length is 1 ~ 4m.
7. by the method that in claim 1 to 6, arbitrary described fully-automatic analyzer divides dissolubility total phosphorus in bleed, comprise the steps:
Testing sample mixes with 100 ~ 150 ℃ of volumn concentration 5 ~ 20% sulfuric acid solutions;
Mixed solution and 20 ~ 30g/L potassium persulfate solution hybrid reaction;
Reacted solution carries out the ultraviolet digestion reaction, the reacted solution of ultraviolet digestion and chromogenic reagent solution hybrid reaction;
After the developer hybrid reaction, with 50 ~ 100g/L ascorbic acid solution, mix, after mixing, 30 ~ 50 ℃ are reacted, and reacted liquid carries out colorimetric estimation at 700 ~ 880nm place;
The solution that described developer is ammonium molybdate, potassium antimony tartrate and NaOH potpourri, described ammonium molybdate concentration is 5 ~ 12g/L, and the concentration of described potassium antimony tartrate is 0.1 ~ 0.4g/L, and the concentration of described NaOH is 65 ~ 105g/L.
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| CN109406426A (en) * | 2018-11-22 | 2019-03-01 | 北京城市排水集团有限责任公司 | Total phosphorus reagent in a kind of quickly measurement sewage, and its preparation method and application |
| CN109470674A (en) * | 2018-12-28 | 2019-03-15 | 清华大学 | A kind of detection device and detection method of dissolved organic matter molecular weight distribution |
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| CN101592670A (en) * | 2008-05-29 | 2009-12-02 | Bltec韩国株式会社 | Automatic analysis quantitatively measure method and automatic analysis quantitatively measure apparatus |
| CN201364308Y (en) * | 2009-01-21 | 2009-12-16 | 马三剑 | On-line automatic monitoring device of water total phosphorus |
| CN201392314Y (en) * | 2009-03-18 | 2010-01-27 | 马三剑 | Automatic on-line analyzing device for total phosphorus in water body |
| CN101661027A (en) * | 2008-08-26 | 2010-03-03 | 上海雷磁环保工程有限公司 | Process for online monitoring and sampling of waste water |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101592670A (en) * | 2008-05-29 | 2009-12-02 | Bltec韩国株式会社 | Automatic analysis quantitatively measure method and automatic analysis quantitatively measure apparatus |
| CN101661027A (en) * | 2008-08-26 | 2010-03-03 | 上海雷磁环保工程有限公司 | Process for online monitoring and sampling of waste water |
| CN201364308Y (en) * | 2009-01-21 | 2009-12-16 | 马三剑 | On-line automatic monitoring device of water total phosphorus |
| CN201392314Y (en) * | 2009-03-18 | 2010-01-27 | 马三剑 | Automatic on-line analyzing device for total phosphorus in water body |
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| JP特开2009-288228A 2009.12.10 |
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