CN102565443A - Simplified automatic sample feeding system of total organic carbon (TOC) analyzer - Google Patents
Simplified automatic sample feeding system of total organic carbon (TOC) analyzer Download PDFInfo
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Abstract
The invention aims at providing a simplified automatic sample feeding system of a total organic carbon (TOC) analyzer. Two peristaltic pumps are used for respectively collecting a water sample and a reagent which enter an acidifier and an oxidation reactor together, wherein the reagent is formed by mixing acid solution and persulfate solution according to proportion. Therefore, the quantity of the peristaltic pumps and reagent dosage are reduced, and the failure probability of the instrument is lowered.
Description
Technical field
The invention belongs to TOC analyser equipment technical field, specifically relate to a kind of TOC analyser automatic sample handling system of simplification.
Background technology
In automatic water quality monitoring, have unrivaled advantage owing to adopt total organic carbon (TOC) to analyze, thereby generally adopted by developed country or area than COD (COD) analysis and biological requirement (BOD) analysis.Along with the continuous enhancing of China's economic strength and the raising day by day of sustainable development consciousness, be that the organic contaminant automatic continuous monitoring system of core just comes into one's own and is widely used in recent years with TOC.
On Dec 8th, 2000, in the notice of State Environmental Protection Administration's issue " environment supervision instrument development guide ", first " organic contaminant automatic continuous monitoring system " classified as the instrument of primary study." 15 " national high-tech research development plans (863 Program)---" automatic water quality monitoring system gordian technique and integrated equipment development " item is classified the TOC automatic analyzer one of as research contents down first.On February 28th, 2003 State Planning Commission, the Ministry of Finance, State Environmental Protection Administration, State Economic and Trade Commission unite the issue the 31st command " collection of drainage dues standard management way " stipulate " chemical oxygen demand COD in the same floss hole, biochemical oxygen demand (BOD first
5) and total organic carbon (TOC), only impose one ".
For this reason, from last century Mo beginning, each big TOC analyser class producer of the world moves into China one after another, and the import TOC automatic analyzer of various models has occupied the market of China more than 90%.Meanwhile, domestic part Study unit and manufacturer have also carried out the development work of pertinent instruments, but majority still is in foundry or imitated stage.
In numerous imports or imitated various TOC analyser models, the variation of sample mode is the maximum differential between them automatically, also is one of main constraints and gordian technique of influencing instrument failure rate and availability thereof.
Existing TOC automatic analyzer can be divided into combustion oxidation method (dry method) and chemical oxidization method (wet method), and the former utilizes high temperature to make the organic substance in the water that burning generation CO take place
2, then through surveying CO
2The concentration of total organic carbon in the cubage water outlet; The latter is oxidized to CO with the organic substance in the water with ultraviolet ray (UV), ozone, persulfate, permanganate, dichromate etc.
2, survey then.Before oxidation of organic compounds, all need pass through certain way, remove the interference of inorganic carbon in anhydrating earlier.In view of firing method needs expensive chemical catalyst, therefore present most TOC automatic analyzers adopt wet oxidation, and generally adopt UV+ persulfate method.
In wet method TOC analyser,, can be divided into microsyringe, semi-automatic microsyringe, slide-valve, rotating disk location automatic sampler, XYZ three-dimensional location automatic sampler, peristaltic pump and quantitative cross-over valve etc. according to sample mode.Wherein, the micro syringe situation of water is per sample adjusted the sample position at any time or water sample is handled, but the difficult control of repeatability; The characteristics of semi-automatic micro syringe are manual samplings, after syringe needle is inserted the sample introduction head, touch the sample introduction key, and water sample injects reaction tube automatically, measure but can only be used for batch (-type); The slide-valve injector is made up of valve body, cylinder, reversing solenoid valve and controller, and advantage is simple in structure, but sample size can not be regulated; The rotating disc injector is made up of parts such as motor, rotating disk, location, sampling, sample presentation, controllers; Characteristics are can be to tens water sample sequencings; Automatically sampling, sample introduction generally only are used for the analysis of laboratory to batch samples, are not suitable for online auto monitoring; Quantitatively cross-over valve is made up of parts such as quantity tube, motor, cross-over valves, is characterized in that sample size can regulate, and both can be used for the laboratory and also can be used for automatic on-line and monitor; Peristaltic pump is made up of pump line, pump head and motor, and characteristics are that simple in structure, sample introduction is stable, can sample incessantly, sample introduction, therefore is specially adapted to on-line automatic continuous monitoring.
For this reason, present TOC automatic analyzer adopts peristaltic pump as injector more.But in existing wet-way analysis appearance, sampling system generally needs 4 peristaltic pumps, and one is used to extract water sample, one and is used to draw fluid after sour reagent, one are used to carry acidifying, one and is used to extract oxygenant.The concrete course of work is: water sample to be measured is inhaled into through injection port 0 under the suction of first peristaltic pump, after filtrator 1 filters, gets into the acidifying coil pipe, and phosphoric acid or the sulphate reagent drawn at this and second peristaltic pump mix mutually.If in water sample, contain the carbonate of inorganic states, can generate CO with sour reagent reacting
2, separate through moisture trap 8 subsequently, and discharge from exhausr port 9.Fluid after the acidifying gets into oxidation reactor 10 under the ordering about of the 3rd peristaltic pump, meanwhile, and with oxygenant (persulfate) solution of the 4th peristaltic pump pumps.This moment, oxygen also got into oxidation reactor.In oxidation reactor 10, the organism in the water sample all is converted into CO under the synergy of ultraviolet light, oxygenant and oxygen
2, and under the promotion of carrier gas, getting into condensation hydroextractor 12, remaining liquid is then discharged through surplus liquid delivery pipe 19.In condensation hydroextractor 12, steam is condensed into water, and is flowed out by drainpipe 13, removes the dry gas behind the moisture, getting into CO after eliminating interfering ions through ion trap 14
2Detecting device 15.CO
2The signal that detecting device 15 obtains is handled through data processor 16, just can obtain the content of total organic carbon in the water sample (TOC), is directly showing on the instrument display screen 17 or is sending on the master server of monitoring department through data transmitter 18 then.
Yet find that in use mainly there is the deficiency of following three aspects in this system: the one, sampling pump is too much.Wherein any one instrument just can not normally move if fault, and the more probabilities that break down that just mean of quantity increase; The 2nd, acidification reactor pipeline easy blocking.Because mostly acidification reactor is coiled, acidifying coil pipe distance is grown (20-30cm), internal diameter less (0.2-0.3mm), in case acidification reaction product (like calcium phosphate, magnesium phosphate etc.) precipitates on tube wall, is easy to make line clogging; The 3rd, oxygenant and acidulant consumption are more.Because acidulant, oxygenant and organic duration of contact very short (1-2s) in this system; In order to improve acidifying, degree of oxidation; Often need add excessive acidulant and oxygenant; For example the auto TOC1950 analyser of U.S. Zell Weger company is dissolved with the 357g sodium peroxydisulfate as oxygenant in 1 premium on currency, and 58ml phosphoric acid is made acidulant; The TOC2001 analyser use concentration as the 178.6g sodium peroxydisulfate make oxygenant, 60ml phosphoric acid is made acidulant; The TOC2100 analyser of U.S. Rosemount company is dissolved with the 140g sodium peroxydisulfate in 1 premium on currency; The TOC2000 of France Seres uses 60ml phosphoric acid to make acidulant.Acidulant and the too much easy generation of secondary pollution of oxygenant consumption, and cause the instrument volume excessive or the cycle of changing dressings is too short.
Summary of the invention
To the deficiency of prior art, the purpose of this invention is to provide a kind of TOC analyser automatic sample handling system of simplification.
Scheme of the present invention is that a kind of TOC analyser automatic sample handling system of simplification mainly comprises injection port, reagent bottle, carrier gas bottle and acidification reactor.Injection port links to each other with acidification reactor through filtrator, electronic flow-meter, peristaltic pump, and reagent bottle passes through electronic flow-meter, peristaltic pump links to each other with acidification reactor, and after carrier gas bottle was divided into two-way through T-valve, wherein one the tunnel was connected with acidification reactor.
Described TOC analyser automatic sample handling system, preferred scheme is that the teflon hose of internal diameter 0.2-0.3mm is adopted in the water route.
Described TOC analyser automatic sample handling system, preferred scheme is that gas circuit adopts the silicon rubber hose of internal diameter 0.5-0.8mm.
Described TOC analyser automatic sample handling system, preferred scheme is that said peristaltic pump is established two.One is used to aspirate water sample, and another is used to extract reagent.
Described TOC analyser automatic sample handling system, preferred scheme be, said reagent bottle fills acidulant and oxygenant in 1: 4-4: the solution that 1 ratio is processed.Described acidulant is phosphoric acid or sulfuric acid.Described oxygenant is sodium peroxydisulfate, potassium persulfate or ammonium persulfate.
Described TOC analyser automatic sample handling system, preferred scheme is that described acidification reactor adopts the four-way hollow glass spherical structure of internal diameter 1.0-3.0mm.
Described TOC analyser automatic sample handling system, preferred scheme is that carrier gas is oxygen or carbon-free air.
The general water sample that adopts after 4 sampling pumps are gathered water sample, acidulant, oxidizing agent solution and acidifying respectively of the sampling system of present wet method TOC automatic analyzer.The native system appearance adopts 2 sampling pumps to gather the mixed solution of water sample and acidulant+oxygenant respectively, can realize auto injection.
Technical advantage of the present invention is:
1. native system is mixed with mixed solution with acidulant (phosphoric acid, sulfuric acid etc.) and oxygenant (sodium peroxydisulfate, potassium persulfate, ammonium persulfate etc.) according to the water sample situation in advance by a certain percentage; Transmit with a peristaltic pump, and the fluid after the acidifying directly relies on carrier gas to promote to move ahead.Saved 2 peristaltic pumps thus, and these 2 peristaltic pumps same motor-driven can be used, thereby the probability that instrument breaks down can be significantly reduced.
2. the acidification reactor of native system has adopted the four-way glass bead structure of an internal diameter 1.0-3.0mm.Under the strong agitation effect of carrier gas, the acidification reaction product is not easy deposition.Even precipitate,, also be difficult for stopping up also because the volume of this reactor is bigger.And because of the perspective effect of glass bead, can check the internal precipitate situation intuitively,, can in time unload and clean or change in case find to have the outlet of sediment blocking pipeline.
3. because the duration of contact of acidulant and oxygenant and inorganic carbon and organic carbon is longer, so the consumption of acidulant and oxygenant can significantly reduce, thereby can prolong the interpolation cycle of reagent greatly, the while has also alleviated reagent to second environmental pollution.Be the water sample of 0～150mg.C/L for example, only dissolve 20g sodium peroxydisulfate and 5mL phosphoric acid in every 1L reagent, can satisfy 1 month measuring period for pH=7, TOC content.
Description of drawings
Fig. 1 is the structural representation of embodiment 1TOC analyser automatic sample handling system.Wherein, 0-injection port; The 1-filtrator; The 2-electronic flow-meter; The 3-peristaltic pump; The 4-acidification reactor; The 5-reagent bottle; The 6-carrier gas bottle; The 7-T-valve; The 8-moisture trap; The 9-exhausr port; The 10-oxidation reactor; The 11-uviol lamp; 12-condensation hydroextractor; The 13-drainpipe; The 14-ion trap; 15-CO
2Detecting device; The 16-data processor; The 17-display; The 18-data transmitter; The surplus liquid vent pipe of 19-.The solid arrow express liquid flows among the figure, and empty arrow is represented gas flow.
Fig. 2 is the TOC typical curve of Potassium Hydrogen Phthalate distilled water solution.
Embodiment
Specify technical scheme of the present invention below in conjunction with embodiment and accompanying drawing, but protection domain is not by this restriction.
The TOC analyser automatic sample handling system of 1 one kinds of simplification of embodiment; Structure can be with reference to figure 1; Mainly comprise injection port 0, reagent bottle 5, carrier gas bottle 6 and acidification reactor 4, injection port 0 links to each other with acidification reactor 4 through filtrator 1, electronic flow-meter 2, peristaltic pump 3, and reagent bottle 5 links to each other with acidification reactor 4 through electronic flow-meter 2, peristaltic pump 3; Carrier gas bottle 6 gas circuits are divided into two-way through T-valve 7, and wherein one the tunnel is connected with acidification reactor 4.The teflon hose of internal diameter 0.2-0.3mm is adopted in the water route.Gas circuit adopts the silicon rubber hose of internal diameter 0.5-0.8mm.Said reagent bottle fills acidulant (phosphoric acid or sulfuric acid) and oxygenant (sodium peroxydisulfate, potassium persulfate or ammonium persulfate) in 1: 4-4: the solution that 1 ratio is processed.Described acidification reactor adopts the four-way hollow glass spherical structure of internal diameter 1.0-3.0mm.
Thus; Native system has adopted a kind of 2 pump sampling systems; Its course of work is: water sample to be measured sucks from injection port 0 under the swabbing action of peristaltic pump 3; Get into acidification reactors 4 through filtrator 1 and flowmeter 2, meanwhile, with the mixed solution of phosphoric acid and persulfate from reagent bottle 5 by another peristaltic pump suction acidification reactor 4.In acidification reactor, inorganic carbon in the water sample and phosphatase reaction generate CO
2Oxygen in the carrier gas bottle 6 or carbon-free air are divided into two-way through T-valve 7 after the bottleneck ejection, wherein one the tunnel get into acidification reactor 4.Fluid after the acidifying is inflow moisture trap 8 under the promotion of carrier gas, isolated inorganic CO
2Discharged by exhausr port 9, the liquid part then gets in the oxidation reactor 10.In oxidation reactor 10, the organic carbon in the water sample is broken down and oxidized under the double action of uviol lamp 11 and persulfate and is CO
2, and under the promotion of the second tunnel carrier gas, getting into condensation hydroextractor 12 from upper cavity, the raffinate part is then discharged through surplus liquid vent pipe 19.In the condensation hydroextractor, steam becomes liquid water because of condensation takes place, and is flowed out by drainpipe 13, and is rich in CO
2Dry gas then get into ion trap 14, at this to CO
2Detect and produce the Cl that disturbs
-Be fixed purer subsequently CO
2With O as carrier gas
2Get into infrared CO
2Detecting device 15 is according to CO
2Concentration data and electronic flow-meter obtain data on flows, can calculate the content of total organic carbon in the water sample (TOC) by data processor 16 according to certain calculation procedure.Computational data can directly show on instrument and meter dish 17, also can and monitor IDNet Inter Departmental Net through data transmitter 18.
Experimental example 1 is chosen Potassium Hydrogen Phthalate, and (molecular formula is C
8H
5KO
4, relative molecular weight 204.22) and as the standard substance of organic carbon.Take by weighing the 2.125g Potassium Hydrogen Phthalate, put into volumetric flask and be settled to 1000mL, be mixed with the standard mother liquor of 1000mg/L.With distilled water mother liquor is mixed with the standard solution of 0mg/L, 100mg/L, 200mg/L respectively, its TOC is demarcated the typical curve of gained instrument such as table 1 and Fig. 2 with this system.
Table 1TOC typical curve is demarcated
This shows that when measuring total organic carbon TOC with this sampling system, the linearly dependent coefficient of its typical curve reaches 0.99965, shows to have good rectilinearity.
The Potassium Hydrogen Phthalate standard mother liquor of experimental example 2 usefulness 1000mg/L is prepared the standard solution of 25mg/L, 50mg/L, 75mg/L, 100mg/L, 150mg/L, 200mg/L respectively, it is carried out TOC measure result such as table 2.
The TOC of table 2 Potassium Hydrogen Phthalate distilled water standard solution measures result (mg/L)
Test findings shows, when measuring total organic carbon TOC with this sampling system, system all less than 0.5%, explains that native system is very high to the measured value stability of water quality TOC to the relative deviation RSD of Potassium Hydrogen Phthalate standard solution TOC measured value, and reappearance is better.
Experimental example 3 is for having chosen phenol, aniline, glutamic acid, glycocoll, DTPA five kinds of representative organism such as (diethylene triamine pentacetic acid (DTPA)s) respectively as standard substance; Be mixed with five kinds of organic carbon contents earlier and contain the standard mother liquor that TOC is 1000mg/L; Become the standard solution of 50mg/L more respectively with distilled water diluting; Carry out TOC with this system then and measure, and measured value and actual value are compared its result such as table 3.
Table 3 is measured result (mg/L) to the TOC of other representative organism standard solution
Can find out that through test this system all has multiple organism and well detects effect, recall rate is higher, and the scope of application is wider, can be used for the monitoring analysis of complicated water quality.
Claims (7)
1. the TOC analyser automatic sample handling system of a simplification; It is characterized in that; Mainly comprise injection port, reagent bottle, carrier gas bottle and acidification reactor, injection port links to each other with acidification reactor through filtrator, electronic flow-meter, peristaltic pump, and reagent bottle links to each other with acidification reactor through electronic flow-meter, peristaltic pump; After carrier gas bottle was divided into two-way through T-valve, wherein one the tunnel was connected with acidification reactor.
2. TOC analyser automatic sample handling system according to claim 1 is characterized in that, the teflon hose of internal diameter 0.2-0.3mm is adopted in the water route.
3. TOC analyser automatic sample handling system according to claim 1 is characterized in that, gas circuit adopts the silicon rubber hose of internal diameter 0.5-0.8mm.
4. TOC analyser automatic sample handling system according to claim 1 is characterized in that said peristaltic pump is established two, and one is used to gather water sample, and another is used to gather reagent.
5. TOC analyser automatic sample handling system according to claim 1 is characterized in that, said reagent bottle fills acidulant and oxygenant in 1: 4-4: the solution that 1 ratio is processed.
6. TOC analyser automatic sample handling system according to claim 5 is characterized in that described acidulant is phosphoric acid or sulfuric acid.
7. TOC analyser automatic sample handling system according to claim 5 is characterized in that described oxygenant is sodium peroxydisulfate, potassium persulfate or ammonium persulfate.
TOC analyser automatic sample handling system according to claim 1; It is characterized in that described acidification reactor adopts the four-way glass bead structure of internal diameter 1.0-3.0mm.
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Cited By (6)
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| CN103196896A (en) * | 2013-04-16 | 2013-07-10 | 四川大学 | Continuous flow analysis method for detecting total organic carbon in water sample |
| CN103884572A (en) * | 2012-12-20 | 2014-06-25 | 韦石 | Full-automatic diluting instrument |
| CN104730267A (en) * | 2015-03-31 | 2015-06-24 | 烟台大学 | Continuous, synchronous and online monitoring method and instrument for concentration and total quantity of TOC (total organic carbon), TN (total nitrogen) and TP (total phosphorus) |
| CN104764740A (en) * | 2015-03-31 | 2015-07-08 | 烟台大学 | Method and instrument for synchronously, continuously and automatically measuring total organic carbon and total phosphorus |
| US20160018376A1 (en) * | 2014-05-23 | 2016-01-21 | Hach Company | Measurement of total organic carbon |
| CN107037040A (en) * | 2017-06-05 | 2017-08-11 | 同济大学 | A kind of preparation of quick detection agent for determining monitoring water quality total organic carbon and application method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103884572A (en) * | 2012-12-20 | 2014-06-25 | 韦石 | Full-automatic diluting instrument |
| CN103196896A (en) * | 2013-04-16 | 2013-07-10 | 四川大学 | Continuous flow analysis method for detecting total organic carbon in water sample |
| US20160018376A1 (en) * | 2014-05-23 | 2016-01-21 | Hach Company | Measurement of total organic carbon |
| US9791430B2 (en) * | 2014-05-23 | 2017-10-17 | Hach Company | Measurement of total organic carbon |
| CN104730267A (en) * | 2015-03-31 | 2015-06-24 | 烟台大学 | Continuous, synchronous and online monitoring method and instrument for concentration and total quantity of TOC (total organic carbon), TN (total nitrogen) and TP (total phosphorus) |
| CN104764740A (en) * | 2015-03-31 | 2015-07-08 | 烟台大学 | Method and instrument for synchronously, continuously and automatically measuring total organic carbon and total phosphorus |
| CN104730267B (en) * | 2015-03-31 | 2016-10-05 | 烟台大学 | TOC, TN, TP concentration and total amount continuous synchronization on-line monitoring method and instrument |
| CN104764740B (en) * | 2015-03-31 | 2017-04-26 | 烟台大学 | Method and instrument for synchronously, continuously and automatically measuring total organic carbon and total phosphorus |
| CN107037040A (en) * | 2017-06-05 | 2017-08-11 | 同济大学 | A kind of preparation of quick detection agent for determining monitoring water quality total organic carbon and application method |
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Application publication date: 20120711 |