CN105466754A - Water sample pretreatment method and device thereof - Google Patents
Water sample pretreatment method and device thereof Download PDFInfo
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- CN105466754A CN105466754A CN201510814810.5A CN201510814810A CN105466754A CN 105466754 A CN105466754 A CN 105466754A CN 201510814810 A CN201510814810 A CN 201510814810A CN 105466754 A CN105466754 A CN 105466754A
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- water sample
- water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
Abstract
The invention provides a water sample pretreatment method, which comprises the following steps: a water sample to be tested is extracted into an original sample water bottle; primary treatment is carried out on the water sample by adding a digesting agent into the original sample water bottle; and a separating agent is added into the digested water sample to be tested such that suspended solids in the water sample to be tested and the separating agent undergo emulsion and layering of the water sample to be tested happens, and the water sample to be tested after separation is pumped into a clean water sample bottle for use. By the water sample pretreatment method provided by the invention, turbidity of a water sample with high turbidity can be greatly reduced. After pretreatment by the method, testing of high-turbidity wastewater will not be disturbed. According to the water sample pretreatment device, water samples are input into and extracted out of the original sample water bottle respectively through an input pump and an extraction pump, thus realizing full automation of the whole operating process. Manual operation process is less, and water sample pretreatment efficiency is raised.
Description
Technical field
The present invention relates to water sample analysis technical field, specifically relate to a kind of water sample preprocess method.In addition, the present invention also provides a kind of water sample preprocessing apparatus.
Background technology
Chemical analysis as a kind of important means judging the good and bad degree of water body, is evaluated the ecological risk in water body and basin exactly, is seemed very important with the Real-Time Monitoring carrying out priority pollutant in environmental monitoring.In the process of chemical analysis water sample, main flow process has: sample collection, Sample storage, sample pretreatment, analysis and detection, data processing and data evaluation.In whole sample chemical is analyzed, the pre-service of sample is very important sport technique segment in whole flow process, is directly connected to the accuracy of later stage water sample test.In pre-service, the Problems of Turbidity of water sample becomes the important threshold together hindering Correct Analysis water sample data, and existing turbidity processing mode is mainly taked to filter, centrifugal, strong acid High-temperature Digestion and algorithm deduction turbidity.In these methods, filter the turbidity can effectively removed in water sample and test the impact brought, this mode is also one of conventional laboratory facilities; Strong acid High-temperature Digestion, mainly by being cleared up by the fine grained suspension in water sample under high-temperature strong acid condition, removes the object of turbidity to reach; And algorithm deduction turbidity uses less in the lab, be generally used for instrument and automatically calculate deduction, this turbidity deduction mode, by the theoretical curve of turbidity in matching water sample, carries out calculating deduction according to the interference that theoretical curve equation calculating turbidity brings in whole test process.
In traditional preprocessing process, realize robotization except clearing up to be close to, all the other modes are difficult to realize robotization, or it is very high to realize cost.For a person skilled in the art, how designing a kind of method that can realize automatically being separated solute in water sample fast, is the current technical issues that need to address.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of water sample preprocess method, comprising:
Water sample to be measured is drawn in former state water bottle;
Add digestion agent in described former state water bottle, clear up the particle in water sample;
Water sample to be measured after clearing up adds separating agent, and the suspension generation emulsion in separating agent and water sample to be measured, the suspension in water sample to be measured is separated with water sample to be measured, and the water sample to be measured after separation is pumped in clean water sample bottle for use.
Alternatively, carry out heating after water sample to be measured mixes with digestion agent and constantly stir, fully mixing with digestion agent; After adding separating agent after water sample cooling to be measured, after stratification, pump to described clean water sample bottle.
Alternatively, in described clean water sample bottle, pass into gas, separating agent small part being dissolved in water sample to be measured is taken away.
Alternatively, judge that described former state water bottle adds the turbidity of the water sample to be measured after separating agent; If higher than preset value, repeat to add digestion agent and separating agent; If lower than preset value, pump in described clean water sample bottle.
Alternatively, digestion agent is acid solution; Separating agent is the organic liquid immiscible with water, density and aqueous phase difference larger.
A kind of water sample preprocessing apparatus, comprising:
For holding the former state water bottle of water sample to be measured;
The front pump of water delivery in described former state water bottle, the drawing pump drawn water from described former state water bottle; Described front pump can carry water sample to be measured, digestion agent and separating agent in described former state water bottle;
Be connected to the clean water sample bottle of described drawing pump rising pipe.
Alternatively, in described former state water bottle, stirring apparatus is set, water sample to be measured is mixed with digestion agent; In described former state water bottle, heating arrangement is set.
Alternatively, also gas-holder is set, air or inert gas can be carried from bottom to top in described clean water sample bottle.
Alternatively, the bottom of described former state water bottle is inverted cone shape, bottom connected drainage valve; Described front pump and described drawing pump are all connected to the middle part of described former state water bottle.
Alternatively, described front pump connecting tee valve, is communicated with conveying water sample to be measured, digestion agent and separating agent, respectively by the connecting pipeline of front pump described in electric control system controls; Described former state water bottle also arranges turbidity detection device.
Water sample preprocess method provided by the present invention, is first drawn into water sample to be measured in former state water bottle, then adds digestion agent in former state water bottle, clears up the particulate matter in water sample to be measured; Add separating agent to water sample to be measured again, separating agent is by the turbidity material emulsification in water sample to organic layer, and separating agent, due to water insoluble, can form lamination.Have passed through the water sample to be measured clearing up process and separating treatment to be transported in clean water sample bottle for use.Water sample preprocess method provided by the present invention, can make water sample and turbidity separating substances, eliminates the interference that turbidity brings in the test of matrix water sample.Water sample preprocessing apparatus provided by the present invention, by front pump and drawing pump respectively to the input in former state water bottle with extract water sample out, achieve the full-automation of whole operating process, the process of manual operation is few, improve the pretreated efficiency of water sample, pre-service can be carried out to water sample fast automaticly.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of specific embodiment of water sample preprocess method provided by the invention;
Fig. 2 is the another kind of specific embodiment of water sample preprocess method provided by the invention;
Fig. 3 is a kind of concrete structure of water sample preprocessing apparatus provided by the invention.
Wherein:
Former state water bottle 1, tapping valve 11, clean water sample bottle 2, front pump 3, drawing pump 4, gas-holder 5.
Embodiment
Core of the present invention is to provide a kind of water sample preprocess method and device, and can clear up water sample to be measured fast and be separated, whole process can realize robotization, improves the pretreated efficiency of water sample.
In order to make those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing and concrete embodiment, water sample preprocess method provided by the present invention and device are described in detail.
As depicted in figs. 1 and 2, the process flow diagram of water sample preprocess method provided by the present invention two kinds of embodiments is respectively.First be drawn in former state water bottle 1 by water sample to be measured, heat in former state water bottle 1 to water sample to be measured, be generally the highlyest heated to 100 DEG C, certainly, the process of heating is also nonessential, and object is the speed accelerating to clear up.In former state water bottle 1, add digestion agent, digestion agent can adopt acid solution usually, clears up the particulate matter in water sample to be measured simultaneously.Usual employing nitric acid dissolve, because acid is cleared up limited in one's ability, in water sample, still partial suspended thing can be there is, after adding a certain amount of separating agent, because separating agent can with the suspension generation emulsion in water sample to be measured, thus make suspension be separated with water sample to be measured.Particularly, the separating agent adopted in the present invention is the liquid immiscible with water, as: the organic solvents such as toluene, cyclohexane, normal hexane, its density is larger with aqueous phase difference, when separating agent and water sample to be measured mix, make separating agent fully contact concurrent raw emulsion with the suspension in water sample to be measured, meeting secondary clearing again, if the density of separating agent is greater than water sample, then can sink to bottom, if density is less than water sample, can top be floated to, finally can form lamination with water sample.Large particulate matter in water sample can sink to bottom; And little suspension and separating agent generation emulsion, float or sink to top or the bottom of water sample, realizing and being separated of water sample.Have passed through the water sample to be measured cleared up with detachment process, if the density of separating agent is less than water, then center section water sample is comparatively clear, and suspension is removed; If the density of separating agent is greater than water, then the water sample of the superiors is comparatively clear, and suspension is removed.Now the clean row eliminating particle can be surveyed water sample to extract out, water sample to be measured be sent and is extracted in clean water sample bottle 2, for follow-up use.
A whole set of water sample preprocess method provided by the present invention, can realize the pretreatment operation to water sample to be measured, and have passed through the water sample to be measured cleared up with detachment process, suspension wherein can be sufficiently removed.Organic solvent is have employed as separating agent in this method, can well by the particle removal in water sample, efficient and convenient.
Particularly, water sample preprocess method provided by the present invention, also needs constantly to stir, can mix more abundant with digestion agent and water sample to be measured after digestion agent mixes with water sample to be measured.The process stirred is undertaken by the drive unit be arranged in former state water bottle 1, does not need human intervention.
Separating agent is added after water sample cooling to be measured, first both to be made to mix through stirring, the suspension in water sample to be measured and separating agent is made fully to contact concurrent raw emulsion, need after stirred to close stirring apparatus, and carry out a period of time leave standstill, general about 2min, makes water sample to be measured and separating agent be separated from each other, and separating agent can float to top or sink to bottom.The middle level water sample to be measured that have passed through after leaving standstill can be pumped in clean water bottle 2, and the organic solvent contained by water sample now in clean water sample bottle 2 is relatively less.Time of repose may cause organic separating cannot be separated completely with water sample not.
After in the present invention, water sample to be measured is transported to clean water sample bottle, in order to a small amount of organic solvent contained in water sample to be measured is removed, gas can be passed in clean water sample bottle 2, air or inert gas can be adopted, bottom-uply to pass into, organic solvent in water sample is taken out of, makes separating agent depart from the complete clean water sample of pre-service completely, reduce the impact on subsequent analysis result as far as possible.
After former state water bottle 1 adds separating agent, before pumping to clean water sample bottle 2, first Turbidity measurement is carried out to the water sample to be measured that have passed through single treatment, if turbidity is equal to or less than preset value, then pump directly in clean water sample bottle 2, if turbidity is higher than preset value, then in former state water bottle 2, again add digestion agent and separating agent, again repeat to clear up and detachment process, until the turbidity of water sample to be measured in former state water bottle 1 meets the demands, then proceed next step operation.
Water sample preprocess method provided by the present invention, first pumps to water sample to be measured in former state water bottle 1, then in former state water bottle 1, adds digestion agent and heat, and is constantly uniformly mixed liquid and makes it abundant mixing, clear up the particulate matter in water sample.After cooling, continue to add separating agent in former state water bottle 1, stop after stirring a period of time, the suspension in water sample and separating agent generation emulsion, separating agent and water sample layering to be measured, make other particles remove from water sample.After have passed through above-mentioned two steps operation, detect the turbidity of water sample to be measured, if turbidity is less than or equal to preset value, be extracted in clean water sample bottle 2, if higher than preset value, repeat to add digestion agent and separating agent, until turbidity meets the demands.
As shown in Figure 3, present invention also offers a kind of water sample preprocessing apparatus, this device includes former state water bottle 1, for holding pending water sample, in former state water bottle 1, be also provided with heating arrangement, can heat water sample, should be noted that, heating arrangement nonessential device, in order to accelerate the oxidation rate of digestion agent.Former state water bottle 1 is connected with front pump 3 and drawing pump 4, and drawing pump 4 extracts water sample out from former state water bottle 1, and front pump 3 inputs water sample to be measured, digestion agent and separating agent in former state water bottle 1.At the rising pipe of drawing pump 4, clean water sample bottle 2 is set.
Water sample preprocessing apparatus provided by the present invention, in former state water bottle 1, water sample to be measured and digestion agent is inputted by front pump 3, and by heating arrangement, water sample to be measured is heated, digestion agent is enable to clear up particulate matter in water sample to be measured better, after have passed through digestion process, the mixed solution of water sample to be measured and digestion agent is cooled, in former state water bottle 1, separating agent is added again again by front pump 3, general employing organic liquid, water insoluble, such as toluene can be adopted, cyclohexane, normal hexane etc., separating agent can with the suspension generation emulsion in water sample to be measured, with water sample layering to be measured after emulsification, separating agent density is greater than bottom then sinking down into of water, what separating agent density was less than water then floats up to top, and the large particulate matter in water sample to be measured can sink down into bottom, finally can make to form clean water sample in the middle of the mixing material in former state water bottle 1, now can from wherein extracting.Therefore when the density of separating agent used is less than water, front pump 3 and drawing pump 4 are all connected to the middle part of former state water bottle 1 sidewall, are positioned at the position with crown center bottom former state water bottle 1 from vertical direction; And drawing pump 4 is connected to position top in the middle part of former state water bottle 1 sidewall when the density of separating agent is greater than water.The water sample now entering clean water sample bottle 2 from former state water bottle 1 is relatively more clean.
Water sample preprocessing apparatus provided by the present invention, can realize inputting water sample to be measured fast automaticly, clear up, be separated and the step such as extraction, whole process is without the need to artificial manipulation, and automaticity is high, and instrument can process automatically, and speed is fast.Pretreated efficiency is high, and digestion agent can clear up the particulate matter in water sample, separating agent can with the suspension generation emulsion of water sample, thus remove the particle of water sample.Cost compare is low, and general only needs adds a kind of specific separating agent, and within 24 hours, constantly can process water sample online.The aqueous ingredient finally obtained is reliable, can not affect lasting analysis and detect.
In order to make the digestion agent in former state water bottle 1 and water sample to be measured mix better, in former state water bottle 1, also will stirring apparatus be set, can constantly to the liquid agitation in former state water bottle 1 by the stirring apparatus of Electronic control.Stirring apparatus can adopt the blade of fan page shape, and the Area comparison contacted with solution is large, and the speed of stirring is without the need to excessive.Also arrange tapping valve 11 in the bottom of former state water bottle 1, after adding separating agent, separating agent and water sample to be measured achieve layering, density are greater than to the separating agent of water, can sink to bottom, now discharge by tapping valve 11.The main effect of tapping valve 11 is after water sample to be measured is pumped to clean water sample bottle 2, also can there is certain remaining liq, discharge by tapping valve 11.More thorough when discharging to make liquid, therefore the bottom of former state water bottle 1 can be set to inverted cone shape, tapping valve 11 is arranged on the position of cone point.
For the water sample pumped in clean water sample bottle 2, can arrange gas-holder 5 bottom it, gas-holder 5 can carry gas in clean water sample bottle 2, wherein can adopt air or inert gas.The a small amount of separating agent be dissolved in water sample can be taken out of by the gas be passed in clean water sample bottle 2, the water sample further in the clean water sample bottle 2 of purification.If be air, can install the pump housing and bleed between gas-holder and clean water sample bottle 2, if adopt inert gas, between gas-holder and clean water sample bottle 2, mounted valve controls opening and closing.
In former state water bottle 1, input water sample to be measured, digestion agent and separating agent because front pump 3 needs to meet simultaneously, with front pump 3 input end, can T-valve be set, connect three pipelines respectively, be connected to water sample to be measured, digestion agent and separating agent.By the pipeline that electric control system controls front pump 3 is communicated with.
In addition, in former state water bottle 1, be also provided with turbidity detection device, whether the turbidity that can detect the water sample to be measured of former state water bottle 1 inside meets pre-provisioning request, pumps water sample when turbidity is less than preset value by drawing pump 4 in clean water sample bottle 2; If when turbidity is greater than preset value, can't directly be used, now need to open front pump 3 continue input resolution agent in former state water bottle 1 and heat, and then pass into separating agent and be separated, and again detect turbidity, until the numerical value detected meets preset value, next step operation can be carried out.
Water sample preprocessing apparatus provided by the present invention, inputs water sample to be measured by front pump 3 in former state water bottle 1; Water sample amount enough after carry out digestion process by front pump 3 to input resolution agent in former state water bottle 1 again, carry out heating and stirring, to accelerate oxidation rate simultaneously; Cleared up rear cooling, and added separating agent in former state water bottle 1, separating agent through stirring after static placement, to be separated dose with water sample layering to be measured after the water sample to be measured being arranged in center section can be extracted into clean water sample bottle 2 by drawing pump 4.Gas-holder 5 passes into gas in clean water sample bottle 2, to be taken out of by a small amount of separating agent dissolved in clean water sample bottle 2, purifies water sample further.
After whole preprocessing process completes, in water sample preprocessing apparatus provided by the present invention, pass into clear water, and complete above-mentioned whole flow process, just can realize the cleaning to this device.The operation of the automatic control inputs pump 3 of electric-control system, drawing pump 4, exhaust valve 11, stirring apparatus and gas-holder 5 and opening and closing, and control heating devices heat water sample.This device is completed automatic sampling by electric-control system, is automatically cleared up and the operation be separated, automatically clean, and without the need to manual operation, greatly saves manpower, and improves treatment effeciency.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein, can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a water sample preprocess method, is characterized in that, comprising:
Water sample to be measured is drawn in former state water bottle (1);
Add digestion agent in described former state water bottle (1), clear up the particle in water sample;
Water sample to be measured after clearing up adds separating agent, and the suspension generation emulsion in separating agent and water sample to be measured, the suspension in water sample to be measured is separated with water sample to be measured, and the water sample to be measured after separation is pumped in clean water sample bottle (2) for use.
2. water sample preprocess method according to claim 1, is characterized in that, carries out heating and constantly stirs, fully mix with digestion agent after water sample to be measured mixes with digestion agent; After adding separating agent after water sample cooling to be measured, after stratification, pump to described clean water sample bottle (2).
3. water sample preprocess method according to claim 2, is characterized in that, in described clean water sample bottle (2), pass into gas, separating agent small part being dissolved in water sample to be measured is taken away.
4. the water sample preprocess method according to any one of claims 1 to 3, is characterized in that, judges that described former state water bottle (1) adds the turbidity of the water sample to be measured after separating agent; If higher than preset value, repeat to add digestion agent and separating agent; If be equal to or less than preset value, pump in described clean water sample bottle (2).
5. water sample preprocess method according to claim 4, is characterized in that, digestion agent is acid solution; Separating agent is the organic liquid immiscible with water, density and aqueous phase difference larger.
6. a water sample preprocessing apparatus, is characterized in that, comprising:
For holding the former state water bottle (1) of water sample to be measured;
The front pump (3) of water delivery in described former state water bottle (1), the drawing pump (4) drawn water from described former state water bottle (1); Described front pump (3) can carry water sample to be measured, digestion agent and separating agent in described former state water bottle (1);
Be connected to the clean water sample bottle (2) of described drawing pump (4) rising pipe.
7. water sample preprocessing apparatus according to claim 6, is characterized in that, arranges stirring apparatus, water sample to be measured is mixed with digestion agent in described former state water bottle (1); In described former state water bottle (1), heating arrangement is set.
8. water sample preprocessing apparatus according to claim 7, is characterized in that, also arranges gas-holder (5), can carry air or inert gas from bottom to top in described clean water sample bottle (2).
9. water sample preprocessing apparatus according to claim 8, is characterized in that, the bottom of described former state water bottle (1) is inverted cone shape, bottom connected drainage valve (11); Described front pump (3) and described drawing pump (4) are all connected to the middle part of described former state water bottle (1).
10. water sample preprocessing apparatus according to claim 9, it is characterized in that, described front pump (3) connecting tee valve, is communicated with conveying water sample to be measured, digestion agent and separating agent, respectively by the connecting pipeline of front pump described in electric control system controls (3); Described former state water bottle (1) also arranges turbidity detection device.
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| CN201510814810.5A CN105466754A (en) | 2015-11-20 | 2015-11-20 | Water sample pretreatment method and device thereof |
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| CN201510814810.5A CN105466754A (en) | 2015-11-20 | 2015-11-20 | Water sample pretreatment method and device thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106053751A (en) * | 2016-08-11 | 2016-10-26 | 力合科技（湖南）股份有限公司 | Water quality monitoring system |
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Application publication date: 20160406 |