CN102375073B - Fully automatic fluorine analyzer and analytical method thereof - Google Patents
Fully automatic fluorine analyzer and analytical method thereof Download PDFInfo
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- CN102375073B CN102375073B CN2010102529581A CN201010252958A CN102375073B CN 102375073 B CN102375073 B CN 102375073B CN 2010102529581 A CN2010102529581 A CN 2010102529581A CN 201010252958 A CN201010252958 A CN 201010252958A CN 102375073 B CN102375073 B CN 102375073B
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Abstract
The invention relates to a fully automatic analyzer for analyzing fluoride ions in environmental water. The analyzer which comprises an automatic injection device (1), a peristaltic pump (19), a detector (11), a computer processing system (17), and an online processing assembly is characterized in that: the automatic injection device (1) comprises a sample injection needle (4), a sample disc (20), a sample injection needle cleaning cell (3), and a pipeline cleaning cell (2); the detector (11) is inserted into a flow cell (12), and the outlet of the flow cell (12) is communicated with a liquid waste cell (16) through a second backpressure regulator (14) by capillary connecting tubes; and the detector (11) is connected with the computer processing system (17) through a signal line (18). By combining an electrode method with a sequential injection analysis method, the analyzer of the invention has the advantages of realization of the automation of the whole process, avoiding of personal errors, detection precision improvement, reagent amount saving, and realization of the timely monitoring of water quality.
Description
Technical field
The present invention relates to a kind of automatical analysis of Environmental Water intermediate ion, particularly a kind of fully-automatic analyzer and the method for using fluorine ion in this analyser automatic analysis Environmental Water of measuring fluorine ion in Environmental Water with sequentical injection analysis.
Background technology
Measure at present the fluoride ion electrode in water, mainly adopt the fluoride ion selective electrode mensuration, fluoride ion selective electrode is the electrode that can correctly measure fluorine ion activity in solution.It mainly is comprised of film, interior reference solution and internal reference electrode three parts, and fluoride ion selective electrode coordinates contrast electrode to connect potential difference meter simultaneously, can measure different kinds of ions concentration, and this assay method is the fluoride ion electrode method.
But the method has the following disadvantages:
1, because need manually-operated, so, have artificial error, and each consumed amount of reagent is more.
2, needing manually-operated, is not to carry out automation mechanized operation, can not be applicable to the real-time monitoring to water quality.
Summary of the invention
The object of the present invention is to provide a kind of sensitivity and accuracy of mensuration high, and simple to operate, and analysis speed is fast, the automatic analytical instrument of fluorine ion in Environmental Water steady in a long-term.
Another object of the present invention has been to provide the automatic analysis method of fluorine ion in a kind of Environmental Water.
The fully-automatic analyzer of fluorine ion in a kind of Environmental Water, comprise automatic sampling apparatus, peristaltic pump, detecting device, computer processing system, online processing components, and automatic sampling apparatus comprises sample introduction needle, sample disc, sample introduction needle service sink, pipeline-cleaning pond, wherein, detecting device inserts flow cell, and the outlet of flow cell is communicated with waste liquid tank by the second back pressure regulator with the capillary connecting pipe, detecting device is connected with computer processing system by signal wire, online processing components comprises sample fillup valve, reagent introduction valve, syringe, capillary connecting pipe, peristaltic pump pump line, the sample fillup valve has the interface more than 6, and two states are arranged: sample introduction state and detected state, when A interface and B interface connection, C interface and D interface connection, E interface and F interface are communicated with, are the sample introduction state, when A interface and F interface connection, B interface and C interface connection, D interface and E interface are communicated with, it is detected state, the interface F of sample fillup valve successively with peristaltic pump on pump line, the upper end of sample introduction needle is communicated with the capillary connecting pipe, the lower end of this sample introduction needle can be stretched in sample bottle, the interface B of sample fillup valve is connected with the two ends of sampling ring respectively with the capillary connecting pipe with interface E, the interface A of sample fillup valve is communicated with waste liquid tank by the first back pressure regulator with the capillary connecting pipe, the interface D of sample fillup valve is connected with the flow cell entrance with the capillary connecting pipe, the interface C of sample fillup valve is connected with reagent introduction valve interface A with the capillary connecting pipe, the reagent introduction valve is 3 valves, two states are arranged: reagent is drawn and reagent discharges, when A interface and S interface are logical, the state that syringe is drawn in downward work reagent, when B interface and S interface are logical, syringe is in the reagent release conditions of upwards working, sample fillup valve C interface is communicated with reagent introduction valve A interface, when the reagent introduction valve during in the reagent release conditions, sample in sampling ring is injected in flow cell, the A interface of sample fillup valve, the outlet of flow cell is connected with the second back pressure regulator respectively, the other end of the second back pressure regulator is communicated with waste liquid tank, back pressure regulator is used for regulating the pressure in stream, suppress the bubble formation in stream, improve accuracy in detection, the kapillary be connected with the interface B of reagent introduction valve is communicated with reagent bottle, the interface B of reagent introduction valve is communicated with reagent bottle by the capillary connecting pipe, reagent introduction valve S interface and syringe join.
The fully-automatic analyzer of fluorine ion in Environmental Water of the present invention, the circulate among pond is hollow structure, it is pmma material.
The fully-automatic analyzer of fluorine ion in Environmental Water of the present invention, the length of capillary connecting pipe wherein is 0.1～1m, and the length of sampling ring is 1～4m, and the syringe volume is 1～5ml
The fully-automatic analyzer of fluorine ion in Environmental Water of the present invention, the dead volume of flow cell wherein is 10～100 μ l.
Use the fully-automatic analyzer of fluorine ion in Environmental Water of the present invention to detect the method for fluorine ion in water, wherein, sample enters peristaltic pump by automatic sampling apparatus, sample pumps into the sample fillup valve by peristaltic pump, after sampling ring is full of, unnecessary sample enters waste liquid tank through interface A and back pressure regulator; The reagent introduction valve is upwards worked and is drawn release reagent downwards by syringe, the dislocation of sample fillup valve, the dislocation of reagent introduction valve, syringe is released the sample be full of in sampling ring, the pond that circulates, and unnecessary sample enters waste liquid tank through back pressure regulator, detecting device detects the potential value of solution in flow cell, and it is transferred to computer processing system, computer processing system, according to the position of potential value on typical curve of sample, calculates the content of fluorine ion in test fluid.
For this automatic analyzer, can change corresponding ion-selective electrode (as chlorion, iodide ion, magnesium ion, calcium ion, cyanide ion, anionic surfactant are selected electrode), supporting flow cell and corresponding current-carrying reagent, be used for measuring corresponding ion.
Advantage of the present invention is: the present invention adopts electrode method and sequentical injection analysis coupling, has realized the robotization of whole process, has avoided personal error, can improve the precision of test, saves amount of reagent and can realize the timely monitoring for water quality.
The accompanying drawing explanation
Fig. 1 is the structure diagram of the automatic analyzer of fluorine ion in Environmental Water provided by the invention.
Embodiment
Below by embodiment, further the present invention will be described.
The fully-automatic analyzer of fluorine ion in embodiment 1 Environmental Water
The automatic analyzer of fluorine ion in Environmental Water as shown in Figure 1, comprise automatic sampling apparatus 1, peristaltic pump 19, detecting device 11, computer processing system 17, online processing components, automatic sampling apparatus comprises sample introduction needle 4, sample disc 20, sample introduction needle service sink 3, pipeline-cleaning pond 2, detecting device 11 inserts flow cell 12, and flow cell 12 is the protruding structure of middle concave side, and the dead volume of flow cell is 10～100 μ l, and it is pmma material, and the outlet of flow cell 12 is communicated with waste liquid tank 16 by the second back pressure regulator 14 with the capillary connecting pipe, detecting device 11 is connected with computer processing system 17 by signal wire 18, online processing components comprises sample fillup valve 8, reagent introduction valve 9, syringe 10, capillary connecting pipe, peristaltic pump pump line 6, syringe 10 volumes are 1-5ml, capillary connecting pipe length is 0.1-1m, sample fillup valve 8 tools have A, B, C, D, E, six interfaces of F, the interface F of sample fillup valve 8 successively with peristaltic pump 19 on pump line 6, the upper end of sample introduction needle 4 is communicated with the capillary connecting pipe, the lower end of this sample introduction needle 4 can be stretched in sample hose 5, the interface B of sample fillup valve 8 is connected with the two ends of sampling ring 7 with interface E, the length of sampling ring 7 is 1～4m, the interface A of sample fillup valve 8 is communicated with waste liquid tank 16 by the first back pressure regulator 13 with the capillary connecting pipe, the interface D of sample fillup valve 8 is connected with flow cell 12 entrances with the capillary connecting pipe, the interface C of sample fillup valve 8 is connected with reagent introduction valve 9 interface A with the capillary connecting pipe, reagent introduction valve 9 is 3 valves, the interface B of reagent introduction valve 9 is communicated with reagent bottle 15 by the capillary connecting pipe, reagent bottle 15 reagent introduction valve 9S interfaces and syringe 10 join.
The course of work of automatic analyzer is:
Sample enters peristaltic pump by automatic sampling apparatus 1, sample pumps into sample fillup valve 8 by peristaltic pump, now, when the A interface of sample fillup valve 8 and B interface connection, C interface and D interface connection, E interface and F interface are communicated with, for the sample introduction state, after sampling ring 7 is full of, unnecessary sample enters waste liquid tank 16 through interface A and back pressure regulator 13; When the B interface of reagent introduction valve 9 and S interface lead to, syringe 10 is in drawing current-carrying from reagent bottle 15 downwards; When reagent introduction valve 9A interface and S interface are logical, syringe 10 is in the reagent release conditions of upwards working, the C interface of sample fillup valve 8 is communicated with reagent introduction valve A interface, now, the A interface of sample fillup valve 8 and F interface connection, B interface and C interface connection, D interface and E interface are communicated with, and sample is injected in flow cell, the pressure that back pressure regulator 13,14 is used for regulating in stream, suppress the bubble formation in stream, improve accuracy in detection.Detecting device 11 detects the potential value of solution in flow cell 12, and it is transferred to computer processing system 17, and computer processing system 17, according to the position of potential value on typical curve of sample, calculates the content of fluorine ion in test fluid.
In the Environmental Water that embodiment 2 is used in embodiment 1, the fully-automatic analyzer of fluorine ion is measured the method for fluorine ion in water
(1) preparation of standard specimen
11 preparation of standard samples: take 0.2210g benchmark sodium fluoride (NaF) (in advance prior to 105～110 ℃ of dry 2h, or in 500～600 ℃ of dry 40min, cooling), water proceeds in the 1000ml volumetric flask after dissolving, and is diluted to graticule, shakes up.Be transferred in the polyethylene bottle of dried and clean at once and store.(100mg/L is (with F for the fluoride standard reserving solution
-Meter)).
1.2 by equal-volume TISAB solution stepwise dilution for fluoride standard reserving solution 100mg/L, be configured to 0.2,0.5,1.0,2.0,5.0,10.0, the 20.0mg/L standard series.
1.3 in total ionic strength adjustment buffer degree buffer solution (being called for short TISAB solution), the sodium chloride volumetric molar concentration is 1.5mol/L, the sodium acetate volumetric molar concentration is 1.5mol/L, the sodium citrate volumetric molar concentration is 0.5mol/L, and 36% acetic acid volumetric molar concentration is 0.5mol/L, with deionized water, is diluted to 1L.
1.4 being isopyknic TISAB solution, mixes with water current-carrying.
Need to use domestic reagent in use procedure, the purity of reagent is minimum pure for analyzing.
Adopt the automatic analyzer shown in Fig. 1 to be tested.
(2) sample introduction
Sample is pumped to sampling ring 7, after sampling ring 7 is full of, enters waste liquid tank 16.
(3) response measurement
Reagent introduction valve 9 is drawn to syringe 10 by current-carrying, and current-carrying is released the sample in sampling ring 7, and the pond 12 that circulates is detected, and the data of generation can be recorded.Do typical curve according to the potential value of the standard solution recorded, calculate the content of fluorine ion according to the suction potential value of sample on typical curve.
The test result of table 1 standard model:
| Concentration known mg/L | logC | Potential value (mv) | Return and calculate concentration mg/L |
| 0.2 | -0.69897 | 197.6 | 0.208 |
| 0.5 | -0.30103 | 176.6 | 0.481 |
| 1 | 0 | 158.7 | 0.982 |
| 2 | 0.30103 | 140.8 | 2.005 |
| 5 | 0.69897 | 117.7 | 5.041 |
| 10 | 1 | 100.3 | 10.092 |
The test result of the different samples of table 2 (n=3)
From this embodiment, adopt this method to record result accurate.
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 those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (7)
1. the fully-automatic analyzer of fluorine ion in an Environmental Water, comprise automatic sampling apparatus (1), peristaltic pump (19), detecting device (11), computer processing system (17), online processing components, described automatic sampling apparatus comprises sample introduction needle (4), sample disc (20), sample introduction needle service sink (3), pipeline-cleaning pond (2), it is characterized in that, described detecting device (11) inserts flow cell (12), and the outlet of flow cell (12) is communicated with waste liquid tank (16) by the second back pressure regulator (14) with the capillary connecting pipe, detecting device (11) is connected with computer processing system (17) by signal wire (18), described online processing components comprises sample fillup valve (8), reagent introduction valve (9), syringe (10), capillary connecting pipe, peristaltic pump pump line (6), described sample fillup valve (8) has the interface more than 6, the interface F of sample fillup valve (8) successively with peristaltic pump (19) on pump line (6), the upper end of sample introduction needle (4) is communicated with the capillary connecting pipe, the interface B of sample fillup valve (8) is connected with the two ends of sampling ring (7) respectively with interface E, the interface A of sample fillup valve (8) is communicated with waste liquid tank (16) by the first back pressure regulator (13) with the capillary connecting pipe, the interface D of sample fillup valve (8) is connected with flow cell (12) entrance with the capillary connecting pipe, the interface C of sample fillup valve (8) is connected with reagent introduction valve (9) interface A with the capillary connecting pipe, reagent introduction valve (9) is 3 valves, the interface B of reagent introduction valve (9) is communicated with reagent bottle (15) by the capillary connecting pipe, the S interface of reagent introduction valve (9) and syringe (10) join.
2. the fully-automatic analyzer of fluorine ion in Environmental Water as claimed in claim 1 is characterized in that: circulate among pond (12) are the protruding structure of middle concave side, and it is pmma material.
3. the fully-automatic analyzer of fluorine ion in Environmental Water as claimed in claim 1 or 2, it is characterized in that: the length of described capillary connecting pipe is 0.1～1m, and the length of sampling ring (7) is 1～4m, and the syringe volume is 1～5ml.
4. the fully-automatic analyzer of fluorine ion in Environmental Water as claimed in claim 1 or 2, it is characterized in that: the dead volume of described flow cell (12) is 10～100 μ l.
5. right to use requires the fully-automatic analyzer of fluorine ion in 1 or 2 described Environmental Water to detect the method for fluorine ion in water, it is characterized in that, sample enters peristaltic pump by automatic sampling apparatus (1), sample pumps into sample fillup valve (8) by peristaltic pump, after sampling ring (7) is full of, unnecessary sample enters waste liquid tank (16) through interface A and back pressure regulator (13); The sample release that reagent introduction valve (9) is upwards worked downwards and will be full of in sampling ring (7) by syringe, pond circulates, unnecessary sample enters waste liquid tank (16) through back pressure regulator (14), detecting device (11) detects the potential value of solution in flow cell, and it is transferred to computer processing system (17), according to the position of potential value on typical curve of sample, computer processing system (17) calculates the content of fluorine ion in test fluid.
6. right to use requires the fully-automatic analyzer of fluorine ion in 3 described Environmental Water to detect the method for fluorine ion in water, it is characterized in that, sample enters peristaltic pump by automatic sampling apparatus (1), sample pumps into sample fillup valve (8) by peristaltic pump, after sampling ring (7) is full of, unnecessary sample enters waste liquid tank (16) through interface A and back pressure regulator (13); Reagent introduction valve (9) is upwards worked and is drawn release reagent downwards by syringe, sample fillup valve (8) dislocation, reagent introduction valve (9) dislocation, syringe is released the sample be full of in sampling ring (7), pond circulates, unnecessary sample enters waste liquid tank (16) through back pressure regulator (14), detecting device (11) detects the potential value of solution in flow cell, and it is transferred to computer processing system (17), computer processing system (17), according to the position of potential value on typical curve of sample, calculates the content of fluorine ion in test fluid.
7. right to use requires the fully-automatic analyzer of fluorine ion in 4 described Environmental Water to detect the method for fluorine ion in water, sample enters peristaltic pump by automatic sampling apparatus (1), sample pumps into sample fillup valve (8) by peristaltic pump, after sampling ring (7) is full of, unnecessary sample enters waste liquid tank (16) through interface A and back pressure regulator (13); Reagent introduction valve (9) is upwards worked and is drawn release reagent downwards by syringe, sample fillup valve (8) dislocation, reagent introduction valve (9) dislocation, syringe is released the sample be full of in sampling ring (7), pond circulates, unnecessary sample enters waste liquid tank (16) through back pressure regulator (14), detecting device (11) detects the potential value of solution in flow cell, and it is transferred to computer processing system (17), computer processing system (17), according to the position of potential value on typical curve of sample, calculates the content of fluorine ion in test fluid.
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| CN103267795B (en) * | 2013-05-02 | 2015-04-22 | 中国科学院合肥物质科学研究院 | On-line monitoring analyzer for fluorinion in water and detection method thereof |
| CN103776889A (en) * | 2013-11-20 | 2014-05-07 | 北京华安奥特科技有限公司 | Automatic ion electrode detection module |
| CN104764861B (en) * | 2015-04-16 | 2017-02-01 | 肖巍 | Analyzing and metering device and liquid analysis system |
| CN104730216B (en) * | 2015-04-16 | 2016-12-07 | 肖巍 | A kind of analysis metering device and liquid analysis system |
| CN105738361B (en) * | 2016-05-03 | 2018-09-07 | 北京宝德仪器有限公司 | Permanganate index automatic analyzer and analysis method in water |
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| CN101692093A (en) * | 2009-09-28 | 2010-04-07 | 北京吉天仪器有限公司 | Automatic analyzer for anionic surfactant in water and automatic analysis method |
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| KR100935703B1 (en) * | 2008-01-14 | 2010-01-07 | 대한민국 | Device and method analyzing milk for field |
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| CN101692093A (en) * | 2009-09-28 | 2010-04-07 | 北京吉天仪器有限公司 | Automatic analyzer for anionic surfactant in water and automatic analysis method |
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