CN102967495B - Sample pretreatment device and sample treatment method - Google Patents
Sample pretreatment device and sample treatment method Download PDFInfo
- Publication number
- CN102967495B CN102967495B CN201210477497.7A CN201210477497A CN102967495B CN 102967495 B CN102967495 B CN 102967495B CN 201210477497 A CN201210477497 A CN 201210477497A CN 102967495 B CN102967495 B CN 102967495B
- Authority
- CN
- China
- Prior art keywords
- sample
- solvent
- extraction column
- valve
- column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention relates to a sample pretreatment device and a sample treatment method. The sample pretreatment device comprises a solvent pump and a solid-phase extraction device, wherein one end of the solvent pump is connected with the sample introduction end of the solid-phase extraction device, the other end of the solvent pump is connected with a multi-way sample introduction selection valve, and the multi-way sample introduction selection valve is connected with a test sample storage device or a multi-solvent storage device; the collecting end of the solid-phase extraction device is connected with a multi-way collection selection valve, and the multi-way collection selection valve is connected with a component collector; and the solid-phase extraction device is provided with a plurality of extraction columns which can be sequentially communicated in series, and two ends of each extraction column are respectively provided with a two-way reversing valve capable of connecting or disconnecting the extraction column with the sample introduction end and the collecting end. By using the sample pretreatment device provided by the invention, the manual treatment of samples in a laboratory is simplified, influences brought by the environment are minimized, and the sample pretreatment time is shortened.
Description
Technical field
The present invention relates to a kind of sample extraction and purification preprocessing system and disposal route, especially a kind of sample pretreatment device that can dioxin in sample and polychlorinated biphenyl be extracted and be purified and disposal route, it can replace manual extraction and purification process, realize automatically selecting and adding solvent, the sample pretreatment device of automatically collecting.
Background technology
Dioxin, polychlorinated biphenyl, palycyclic aromatic and residues of pesticides etc. are the environment contaminant trace species being subject to common concern in recent years, belong to persistence organic pollutant (Persistent Organic Pollutants is called for short POPs).For the detection of dioxin and polychlorinated biphenyl persistence organic pollutant, because its environmental content is generally below pg (1pg=10-12g) level or PPT (10-12) level, its pre-treatment means become an important and the key link in testing.
At analysis field, in order to the dioxin in the samples such as testing environment, pollution by polychlorinated biphenyles thing, carry out a large amount of Researching and practicing.Especially for the polychlorinated biphenyl in environment, pharmacy, biological sample, dioxin etc., because its content is lower, the disturbing effect brought by other materials in matrix is larger, therefore steps such as carrying out a series of comparatively complicated extraction, purifying, fractionation, concentrate is needed, sample pretreatment process is very complicated, causes testing cost to rise.Meanwhile, current every country government and authoritative institution are for dioxin, and monitoring, the testing requirement of pollution by polychlorinated biphenyles thing are also more and more stricter, and Detection task also sharply increases.Therefore, the extracting and purifying efficiency of sample pre-treatments system, robotization, high flux become the important indicator of developing direction, and sample purification system needs to reliability and commercial utility development.
Current, pre-treatment means for the persistence organic pollutant such as dioxin, polychlorinated biphenyl examination criteria mainly rely on manual operation to go, not only work workload is large, the sample purification cycle is long, and due to the addition of solvent or sample accurately can not be controlled, usually obtain inaccurate examining report, the reliability of quantitative testing result cannot be ensured.Manual operation is not only numerous and diverse, owing to not being airtight operation, easily to human body and environmental danger.
Given this, the present inventor, according to the Production design experience being engaged in this area and association area for many years, develops sample pretreatment device of the present invention and disposal route, with harm reduction, simplifies the operation, and improves sample pre-treatments efficiency.
Summary of the invention
The object of this invention is to provide a kind of sample pretreatment device and disposal route, especially a kind of sample pretreatment device and disposal route that can extract, purify dioxin and polychlorinated biphenyl in sample.
For this reason, sample pretreatment device of the present invention, it comprises: solvent pump, solid-phase extraction device, described solvent pump energy quantitatively output solvent, its one end is connected with the sample introduction end of described solid-phase extraction device, the other end is connected with many logical sample introduction selector valves, and described many logical sample introduction selector valves are connected with test sample storage device or multi-solvents memory storage; The collecting terminal of described solid-phase extraction device is logically collected selector valve with many and is connected, and describedly manyly logically collects selector valve connection fraction collector; Described solid-phase extraction device has the multiple extraction columns can contacted successively and be communicated with, and the two ends of each described extraction column are respectively equipped with the two way selected valve that described extraction column and sample introduction end can be connected with collecting terminal or disconnect.
Sample pretreatment device as above, wherein, the extraction column arranged near described collecting terminal is acticarbon filled column, and the two-port valve of four bridge-type connections forms solvent and flows to switching device shifter, makes solvent can flow through described acticarbon filled column forward or backwards; Described switching device shifter two corresponding end are wherein connected with the two ends of described acticarbon filled column respectively, and other two corresponding end of described switching device shifter are connected with the described two way selected valve being arranged on described acticarbon filled column two ends respectively.
Sample pretreatment device as above, wherein, described extraction column also has silica filler post and alumina packing post.
Sample pretreatment device as above, wherein, is provided with the pressure transducer that can control to enter treating apparatus internal solvent pressure between described solvent pump and solid-phase extraction device.
Sample pretreatment device as above, wherein, is provided with filtrator between described sample storage device and many logical sample introduction selector valves.
Sample pretreatment device as above, wherein, the outer setting of described sample pretreatment device casing has multiple fixed support, and each described extraction column card is established and is fixed on described fixed support, is connected with the two way selected valve be arranged in described casing by flexible pipe and hose adapter.
Sample pretreatment device as above, wherein, described two way selected valve, many logical sample introduction selector valves, many logical collection selector valves and switching device shifter are electrically-controlled valve.
The present invention also provides a kind of sample-pretreating method, adopts sample pretreatment device as above, comprising:
1) by two way selected valve, each described extraction column is connected respectively successively with collecting terminal with the sample introduction end of described sample pretreatment device, many logical sample introduction selector valves select activating solvent successively, by solvent pump, described activating solvent is delivered to the described extraction column be connected with stream, one by one each described extraction column is activated, and through many logical selector valves of collecting, the activating solvent waste liquid after activating each described extraction column is delivered in the waste collection bottle of fraction collector;
2) by how, logical sample introduction selector valve is chosen as and is connected with sample storage device, disconnect the extraction column be connected with switching device shifter, and by described two way selected valve, other at least one described extraction column is connected with stream, by solvent pump by described sample delivery extremely described extraction column, described sample is collected in the waste collection bottle of fraction collector after flowing through many logical collection selector valves;
3) how drip washing solvent selected successively by logical sample introduction selector valve, and by described two way selected valve, at least one described extraction column is connected with stream, by solvent pump, described drip washing solvent is transported to described extraction column successively, drip washing is carried out to it, to make in sample chaff interference from drip washing extraction column; The object in sample is made to enter in fraction collector in corresponding Fraction collection bottle through many logical selector valves of collecting together with eluent solution, or making the object in sample be transferred on the next stage extraction column of series connection, described drip washing solvent to be selected to enter in fraction collector in corresponding Fraction collection bottle through many logical selector valves of collecting;
4) extraction column described in other is disconnected, the extraction column be connected with switching device shifter is only made to be connected with stream, and this extraction column is in reverse connected state, eluting solvent selected by described many logical sample introduction selector valves, make this eluting solvent reverse direction flow through described extraction column, reverse wash-out is carried out to it, is collected in Fraction collection bottle that the object in described eluting solvent and eluted sample to be collected in fraction collector by selector valve by many logical.
Sample-pretreating method as above, wherein, described step 1) also comprise how multiple activating solvent selected successively by logical sample introduction selector valve, repeatedly activation process is carried out to extraction column described at least one.
Sample-pretreating method as above, wherein, in described step 1), step 3), the extraction column be connected with switching device shifter is in forward connected state.
Sample pretreatment device of the present invention and disposal route, simplify the in vitro manual handle of sample, minimize the impact that environment brings, decrease the time of sample pre-treatments.Adopt outside extraction column being arranged on apparatus housing, by the fixed support of casing outer setting, being established by each extraction column card is fixed on each fixed support, and by flexible pipe and hose adapter by each extraction column respectively be arranged on two way selected valve corresponding in casing and be connected, simple to operation, user directly can buy or carry out filling special purification extraction column as required, conventional dioxin purification separation post or the special trace organic substance decontaminating column of user can be connected, and can according to the actual requirements, three groups or any two groups of purification separation posts arbitrarily combinationally use.Namely, open port design, while can realizing three purification separation solid-phase extraction columns such as silica filler post, alumina packing post and acticarbon filled column, series connection uses, or any two or the purification separation post that are used alone wherein, instrument flow path designs has the forward of solid-phase extraction column, reverse isolation of purified function.The present invention also adapts to the extracting and purifying system expanding to other pollutants.
Accompanying drawing explanation
The following drawings is only intended to schematically illustrate the present invention and explain, not delimit the scope of the invention.Wherein,
Fig. 1 is the syndeton schematic diagram of each parts of sample pretreatment device of the present invention, is shown as each extraction column off position in figure;
Fig. 2 is the syndeton schematic diagram of each parts of sample pretreatment device of the present invention, and it is all in running order to be shown as each extraction column in figure.
Drawing reference numeral illustrates:
1, solvent pump 2, solid-phase extraction device 21, sample introduction end 22, collecting terminal
23, silica filler post 24, alumina packing post 25, switching device shifter
251,252,253,254, two-port valve
26,261,262,263,264,265,266 two way selected valves 27, acticarbon filled column
3, many logical sample introduction selector valve 4, sample storage device 5, multi-solvents memory storage
6, many logical collection selector valve 7, fraction collector 8, pressure transducer 9, filtrator
Embodiment
The sample pretreatment device that the present invention proposes comprises: solvent pump, solid-phase extraction device, described solvent pump energy quantitatively output solvent, its one end is connected with the sample introduction end of described solid-phase extraction device, the other end is connected with many logical sample introduction selector valves, and described many logical sample introduction selector valves are connected with test sample storage device or multi-solvents memory storage; The collecting terminal of described solid-phase extraction device is logically collected selector valve with many and is connected, and describedly manyly logically collects selector valve connection fraction collector; Described solid-phase extraction device has the multiple extraction columns can contacted successively and be communicated with, and the two ends of each described extraction column are respectively equipped with the two way selected valve that described extraction column and sample introduction end can be connected with collecting terminal or disconnect.
In addition, the present invention also proposes a kind of sample-pretreating method, utilizes above-mentioned sample pretreatment device, comprises the following steps:
1) by two way selected valve, each described extraction column is connected respectively successively with collecting terminal with the sample introduction end of described sample pretreatment device, many logical sample introduction selector valves select activating solvent successively, by solvent pump, described activating solvent is delivered to the described extraction column be connected with stream, one by one each described extraction column is activated, and through many logical selector valves of collecting, the activating solvent waste liquid after activating each described extraction column is delivered in the waste collection bottle of fraction collector;
2) by how, logical sample introduction selector valve is chosen as and is connected with sample storage device, disconnect the extraction column be connected with switching device shifter, and by described two way selected valve, other at least one described extraction column is connected with stream, by solvent pump by described sample delivery extremely described extraction column, described sample is collected in the waste collection bottle of fraction collector after flowing through many logical collection selector valves;
3) how drip washing solvent selected successively by logical sample introduction selector valve, and by described two way selected valve, at least one described extraction column is connected with stream, by solvent pump, described drip washing solvent is transported to described extraction column successively, drip washing is carried out to it, to make in sample chaff interference from drip washing extraction column; The object in sample is made to enter in fraction collector in corresponding Fraction collection bottle through collecting selector valve together with eluent solution, or making the object in sample be transferred on the next stage extraction column of series connection, described drip washing solvent is selected to enter in fraction collector in corresponding Fraction collection bottle through collecting selector valve;
4) extraction column described in other is disconnected, the extraction column be connected with switching device shifter is only made to be connected with stream, and this extraction column is in reverse connected state, eluting solvent selected by described many logical sample introduction selector valves, make this eluting solvent reverse direction flow through described extraction column, reverse wash-out is carried out to it, is collected in Fraction collection bottle that the object in described eluting solvent and eluted sample to be collected in fraction collector by selector valve by many logical.
Sample pretreatment device of the present invention and disposal route, simplify the in vitro manual handle of sample, considerably reduce greatly the impact on environment, decrease the time of sample pre-treatments, also substantially increase repeatability and the accuracy of testing result simultaneously, accelerate sample pre-treatments speed, and reduce sample pre-treatments reagent cost.The present invention is not only applicable to the objectionable impuritiess such as dioxin in fast purification sample and polychlorinated biphenyl, adapts to the extracting and purifying that expansion is used for other pollutants yet.
In order to there be understanding clearly to technical characteristic of the present invention, object and effect, below in conjunction with accompanying drawing and preferred embodiment, to the embodiment of inventive samples pretreating device and disposal route, structure, method characteristic and effect, be described in detail as follows.In addition, by the explanation of embodiment, when can to the present invention for the technological means reaching predetermined object and take and effect are goed deep into concrete understanding more, but institute's accompanying drawing be only to provide with reference to and use is described, is not used for being limited the present invention.
As shown in Figure 1, the sample pretreatment device that the present invention proposes comprises: solvent pump 1, solid-phase extraction device 2, one end of described solvent pump 1 is connected with the sample introduction end 21 of described solid-phase extraction device 2, the other end is connected with many logical sample introduction selector valves 3, and described many logical sample introduction selector valves 3 are connected with test sample storage device 4 or multi-solvents memory storage 5; The collecting terminal 22 of described solid-phase extraction device 2 is logically collected selector valve 6 with many and is connected, and described many logical collection selector valves 6 connect fraction collector 7; Described solid-phase extraction device 2 has the multiple extraction columns can contacted successively and be communicated with, and the two ends of each described extraction column are respectively equipped with the two way selected valve 26 that described extraction column and sample introduction end 21 can be connected with collecting terminal 22 or disconnect.Described solvent pump 1 can quantitative output solvent, and setting pumps volume, to guarantee the accuracy of sample and solvent delivery amount as requested.
Wherein, two-port valve shown in figure 251,252,253,254, two way selected valve 26, what be positioned at schematic diagram top position is one, lower position be two.That is, one that 1. represents two-port valve 251,252,253,254 or two way selected valve 26 shown in figure, two of two-port valve 251,252,253,254 or two way selected valve 26 are 2. represented.
Further, the extraction column arranged near described collecting terminal 22 is that the two-port valve formation solvent that acticarbon filled column 27, four bridge-types connect flows to switching device shifter 25, makes solvent can flow through described acticarbon filled column 27 forward or backwards.Described switching device shifter 25 two corresponding end are wherein connected with the two ends of described acticarbon filled column 27 respectively, and other two corresponding end of described switching device shifter 25 are connected with the two way selected valve 265,266 that described acticarbon filled column 27 can be made to be connected with sample introduction end 21, collecting terminal 22 or disconnect respectively.As shown in the figure, switching device shifter 25 is made up of four interconnective two-port valves 251,252,253,254, wherein, two-port valve 251,253 is connected with the two ends of acticarbon filled column 27 respectively, and two-port valve 252,254 is connected with two way selected valve 265,266 respectively.When two-port valve 251 shown in figure, 252 is in one, when two-port valve 254,253 is in two, then solvent flows through acticarbon filled column 27 along the direction of front A; When two-port valve 251,252 is in two, when two-port valve 254,253 is in one, then solvent flows through acticarbon filled column 27 along the direction of front B, thus it is dynamic to realize the lower reflux of solvent on acticarbon filled column 27, extract is all collected in grouping gatherer 7, the accuracy of warranty test.
The extraction column arranged between sample introduction end 21 and acticarbon filled column 27 also comprises silica filler post 23 and alumina packing post 24 successively.Wherein, the two ends of silica filler post 23 are connected with two way selected valve 261,262 respectively; The two ends of alumina packing post 24 are connected with two way selected valve 263,264 respectively.
Wherein, extraction column is not limited to active carbon filler post 27, silica filler post 23 and alumina packing post 24, different according to the sample of process, can expand to other extraction columns.
In a specific embodiment, the pressure transducer 8 that can control to enter treating apparatus internal solvent pressure is provided with between described solvent pump 1 and solid-phase extraction device 2.
In addition, between sample storage device 4 and many logical sample introduction selector valves 3, filtrator 9 can also be set, with the impurity in elimination sample.
The extraction column of sample pretreatment device of the present invention is the outside being arranged on apparatus housing, namely multiple fixed support is had in the outer setting of casing, each extraction column can block to establish and is fixed on each fixed support, and by flexible pipe and hose adapter be arranged on two way selected valve 26 corresponding in casing and be connected.
Wherein, above-mentioned two way selected valve 26, many logical sample introduction selector valves 3, many logical collection selector valves 7 and switching device shifter 25 are electrically-controlled valve, and sample pretreatment device of the present invention can realize Automatic Control.
The sample-pretreating method that the present invention proposes, adopts above-mentioned sample pretreatment device, comprising:
1) by two way selected valve, each described extraction column is connected respectively successively with collecting terminal 22 with the sample introduction end 21 of described sample pretreatment device, many logical sample introduction selector valves 3 select activating solvent successively, by solvent pump 1, described activating solvent is delivered to the described extraction column be connected with stream, one by one each described extraction column is activated, and through many logical selector valves 6 of collecting, the activating solvent waste liquid after activating each described extraction column is delivered in the waste collection bottle of fraction collector 7;
2) by how, logical sample introduction selector valve 3 is chosen as and is connected with sample storage device 4, disconnect the extraction column be connected with switching device shifter 25, and by two way selected valve, other at least one extraction column is connected with stream, by solvent pump 1 by described sample delivery to this extraction column, sample is collected in the waste collection bottle of fraction collector 7 after flowing through many logical collection selector valves 6;
3) how different drip washing solvents selected successively by logical sample introduction selector valve 3, and by two way selected valve, at least one extraction column is connected with stream, the drip washing solvent being removed chaff interference by solvent pump 1 is transported to this extraction column or crosscurrent extraction post successively, drip washing is carried out to it, to make in sample chaff interference from drip washing extraction column, and enter in Fraction collection bottle corresponding in fraction collector 7 through many logical selector valves 6 of collecting with this drip washing solvent.After eliminating chaff interference, solvent pump 1 can carry the drip washing solvent delivery of object to this extraction column or crosscurrent extraction post, drip washing is carried out to it, the object in sample is made to enter in fraction collector 7 in corresponding Fraction collection bottle through many logical selector valves 6 of collecting together with this eluent solution, or making the object in sample be transferred on the next stage extraction column of series connection, described drip washing solvent to be selected to enter in fraction collector 7 in corresponding Fraction collection bottle through many logical selector valves 6 of collecting;
4) other extraction column is disconnected, the extraction column be connected with switching device shifter 25 is only made to be connected with stream, and this extraction column is in reverse connected state, eluting solvent selected by many logical sample introduction selector valves 3, make this eluting solvent reverse direction flow through described extraction column, reverse wash-out is carried out to it, is collected in Fraction collection bottle that the object in described eluting solvent and eluted sample to be collected in fraction collector 7 by selector valve 6 by many logical.
Described step 1) further comprise: by how multiple activating solvent selected successively by logical sample introduction selector valve 3, repeatedly activation process is carried out at least one extraction column.
In addition, in described step 1), step 3) in, the extraction column be connected with switching device shifter 25 is in forward connected state.
Principle of work of the present invention is: many logical sample introduction selector valves 3 are selected to be connected with a kind of solvent in sample storage device 4 or multi-solvents memory storage 5, by solvent pump 1 by sample or solvent delivery to solid-phase extraction device 2.According to the need of by sample or solvent delivery to each root extraction column, select each two way selected valve 261,262,263,264,265,266 be in shown in Fig. 1 or be in two shown in Fig. 2.When two way selected valve 26 is all in two as shown in Figure 2, then each extraction column is sequentially connected in series, then sample and solvent are transported to each extraction column by solvent pump 1, the final regulation place being collected fraction collector through many logical collection selector valves 6.
The present invention can be used for the Solid-Phase Extraction pre-treatment of sample, Solid-Phase Extraction analyzing and processing needs sample (analyzing component containing band) to be transported on the solid-phase extraction column of regulation usually, then by controlling many logical sample introduction selector valves 3, the solvent of regulation is transported on selected extraction column successively, solid-phase extraction column performs activation, loading, drip washing, the steps such as wash-out, and control stream by many logical selector valves 6 of collecting, different component or waste liquid are collected collections place different in fraction collector respectively, then each component that analyst can collect fraction collector is carried out next step and is analyzed.
In the present invention, guarantee that Solid-Phase Extraction is carried out, to improve the accuracy of test under the pressure and flow velocity of regulation by arranging pressure transducer 8.
Below for the extraction of dioxin and polychlorinated biphenyl with purify, further illustrate technical scheme of the present invention.
In this specific embodiment, set gradually three solid-phase extraction columns, be respectively silica filler post 23, alumina packing post 24 and acticarbon filled column 27.Extraction solvent normal hexane, toluene, ethyl acetate and toluene mixture liquid (50: 50 is stored respectively in multi-solvents memory storage 5, v/v), the mixed solvent (98: 2 of methylene chloride and normal hexane, and normal hexane and methylene chloride mixed solvent (50: 50, v/v) v/v).
First, activate solid-phase extraction column, two way selected valve 261,262 is arranged on two, 263,264,265,266 one is all arranged on, normal hexane solvent selected by many logical sample introduction selector valves 3, by solvent pump 1 by this normal hexane solvent delivery to solid-phase extraction device, activated silica gel filled column 23.Two way selected valve 263,264 is arranged on two, and 261,262,265,266 are all arranged on one, and normal hexane solvent selected by many logical sample introduction selector valves 3, by solvent pump 1 by this normal hexane solvent delivery to solid-phase extraction device, activated alumina filled column 24.Two way selected valve 265,266 is arranged on two, 261,262,263,264 one is all arranged on, two-port valve 251,252 in switching device shifter 25 is in one, and two-port valve 253,254 is in two, normal hexane solvent selected by many logical sample introduction selector valves 3, by solvent pump 1 by this normal hexane solvent delivery to solid-phase extraction device, make solvent energy forward (direction along front A) flow through carbon column 27.Then, the two way selected valve state of step in maintenance, toluene solvant selected by many logical sample introduction selector valves 3, by solvent pump 1, this toluene solvant is transported to acticarbon filled column 27 by two way selected valve 265, switching device shifter 5, activates this acticarbon filled column.The two way selected valve state of step in maintenance, namely acticarbon filled column 27 is only made to be connected with solvent pump 1, many logical sample introduction selector valves 3 select ethyl acetate and benzene to mix liquid (50: 50v/v), by solvent pump 1, this ethyl acetate and benzene are mixed liquid (50: 50v/v) and be delivered to acticarbon filled column 27, it is activated; Select normal hexane and methylene chloride to mix liquid (50: 50v/v) again, be delivered to acticarbon filled column 27 by solvent pump, this acticarbon filled column is activated; Afterwards, select normal hexane solvent, be transported to acticarbon filled column 27 by solvent pump 1, this acticarbon filled column 27 is activated.Above-mentioned activated solution is selected to enter in the component f of gatherer 7 through collecting selector valve 6.
Carry out loading step after completing above-mentioned steps, many logical sample introduction selector valves 3 are selected to be connected with sample storage device 4, simultaneously, two way selected valve 261,262,263,264 is made to be in two, and two way selected valve 265,266 is in one, that is, acticarbon filled column 27 and stream are disconnected.Described sample, after filter 9 filters, is transported to silica filler post 23 and alumina packing post 24 by solvent pump 1, after flowing through many logical collection selector valves 6, is collected in the component f of sample component gatherer 7, namely in waste collection bottle.
Then, normal hexane solvent selected by many logical sample introduction selector valves 3, by solvent pump 1, it is transported to silica filler post 23 and alumina packing post 24 successively, carries out drip washing, dioxin is transferred on alumina packing post 24 to silica filler post 23 and alumina packing post 24.Solvent is selected to enter in the component f in fraction collector 7 through collecting selector valve 6.
Afterwards, many logical sample introduction selector valves 3 select normal hexane and methylene chloride to mix liquid (98: 2, v/v), only make two way selected valve 263,264 be in two, all the other each two way selected valves 26 are all in one, namely simultaneously, only alumina packing post 24 is connected with solvent pump 1, by solvent pump 1, normal hexane and methylene chloride are mixed liquid (98: 2, v/v) and be delivered to alumina packing post 24, drip washing is carried out to it.Leacheate is through collecting in the component a of selector valve 6 selection in fraction collector 7.
Next step, many logical sample introduction selector valves 3 select normal hexane and methylene chloride to mix liquid (50: 50, v/v), make two way selected valve 261,262 remain on one simultaneously, make two way selected valve 263,264,265,266 be in two, the two-port valve 251,252 in switching device shifter 25 is in one, and two-port valve 253,254 is in two, make alumina packing post 24, acticarbon filled column 27 and fluid communication, and make solvent can flow through acticarbon filled column 27 along the direction of front A; By solvent pump 1, normal hexane and methylene chloride are mixed liquid (50: 50, v/v) alumina packing post 24 is delivered to, carry out drip washing to it, make dioxin be transferred on acticarbon filled column, leacheate is then collected in the components b of selector valve 6 selection in fraction collector 7 through lead to more.
Again by how logical sample introduction selector valve 3 selects ethyl acetate and benzene to mix liquid (50: 50v/v), only make two way selected valve 265,266 be in two simultaneously, all the other each two way selected valves 261,262,263,264 are in one, namely acticarbon filled column 27 is only made to be connected with solvent pump 1, by solvent pump 1, ethyl acetate and benzene are mixed liquid (50: 50v/v) and be delivered to acticarbon filled column 27, drip washing is carried out to it, now, solvent flows through acticarbon filled column 27 along the direction of front A.Leacheate is through collecting in the amount of component b of selector valve 6 selection in fraction collector 7.
In maintenance, the stream of step is constant, that is, only make acticarbon filled column 27 be connected with solvent pump 1.Normal hexane selected by described many logical sample introduction selector valves 3, by solvent pump 1, normal hexane is delivered to acticarbon filled column 27, carries out drip washing to it.Leacheate is through collecting in the component d of selector valve 6 selection in fraction collector 7.
Finally, acticarbon filled column 27 is only made to be connected with solvent pump 1, disconnect other filled column, meanwhile, switching device shifter 25 is commutated, namely two-port valve 251,252 is in two, two-port valve 253,254 is in one, and toluene selected by many logical sample introduction selector valves 3, by solvent pump 1, toluene is delivered to acticarbon filled column 27, reverse wash-out is carried out to it, is collected in component e that dioxin to be collected in fraction collector 7 by selector valve 6 by many logical.Then analyst can carry out next step analysis to the component of collecting.
Sample pretreatment device of the present invention all adopts electrically-controlled valve due to each valve, Automatic Control can be carried out to it by computing machine, pre-treatment step full automation can be realized for organic micro-pollutant sample solutions such as dioxin, polychlorinated biphenyl, palycyclic aromatic and residues of pesticides, eliminate the error that manual pre-treatment dioxin sample causes, substantially increase repeatability and the accuracy of testing result, accelerate sample pre-treatments speed, and reduce sample pre-treatments reagent cost.
The present invention is by loading different control module, by autoelectrinic Vavle switching, without the need to manual intervention, realize that automatic on multiple decontaminating columns such as special acidifying silicagel column, alkali alumina post and carbon column of sample solution is separated, purifying, not only provide safeguard for realizing the accurate quantitative analysis of contaminant trace species in sample, and save the input of time, artificial and reagent aspect.
Sample pretreatment device of the present invention adopts outside extraction column being arranged on apparatus housing, by the fixed support of casing outer setting, being established by each extraction column card is fixed on each fixed support, and by flexible pipe and hose adapter by each extraction column respectively be arranged on two way selected valve 26 corresponding in casing and be connected, simple to operation, user directly can buy or carry out filling special purification extraction column as required, conventional dioxin purification separation post or the special trace organic substance decontaminating column of user can be connected, and can be according to the actual requirements, three groups or any two groups of purification separation posts arbitrarily combinationally use.Namely, open port design, while can realizing three purification separation solid-phase extraction columns such as silica filler post 23, alumina packing post 24 and acticarbon filled column 27, series connection uses, or any two or the purification separation post that are used alone wherein, instrument flow path designs has the forward of solid-phase extraction column, reverse isolation of purified function.The present invention is totally-enclosed system, automatically completes sample amounts sample introduction and quantitative collection.Sample can realize activation, drip washing and wash-out in purification separation process, and automatically completes the switching of 5 kinds of solvents; Native system adopts the design of solid-phase extraction column interface opening formula,
In the present embodiment, fraction collector 7 has 6 passages, and a passage is for collecting waste liquid, and other five passages are used for Fraction collection, are communicated with one of them passage by 6 channel selector valves.And each expanding channels one receiving flask, namely can comprise multiple receiving flask in fraction collector 7, wherein component a to component f is respectively 6 receiving flasks, and in the present embodiment, setting component f is waste collection bottle.Therefore each sample can realize continuous 5 sections of quantitative collections, obtains 5 kinds of components after purification separation for subsequent analysis.
The foregoing is only the schematic embodiment of the present invention, and be not used to limit scope of the present invention.Any those skilled in the art, the equivalent variations done under the prerequisite not departing from design of the present invention and principle and amendment, all should belong to the scope of protection of the invention.And it should be noted that, each ingredient of the present invention is not limited in above-mentioned overall applicability, the each technical characteristic described in instructions of the present invention can select one to adopt separately or select the multinomial use that combines according to actual needs, therefore, the present invention covers other relevant with this case inventive point in the nature of things and combines and embody rule.
Claims (9)
1. a sample pretreatment device, it is characterized in that, described sample pretreatment device comprises: solvent pump, solid-phase extraction device, described solvent pump energy quantitatively output solvent, its one end is connected with the sample introduction end of described solid-phase extraction device, the other end is connected with many logical sample introduction selector valves, and described many logical sample introduction selector valves are connected with test sample storage device or multi-solvents memory storage; The collecting terminal of described solid-phase extraction device is logically collected selector valve with many and is connected, and describedly manyly logically collects selector valve connection fraction collector; Described solid-phase extraction device has the multiple extraction columns can contacted successively and be communicated with, and the two ends of each described extraction column are respectively equipped with the two way selected valve that described extraction column and sample introduction end can be connected with collecting terminal or disconnect; The extraction column arranged near described collecting terminal is acticarbon filled column, and the two-port valve of four bridge-type connections forms solvent and flows to switching device shifter, makes solvent can flow through described acticarbon filled column forward or backwards; Described switching device shifter two corresponding end are wherein connected with the two ends of described acticarbon filled column respectively, and other two corresponding end of described switching device shifter are connected with the described two way selected valve that described acticarbon filled column can be made to be connected with sample introduction end, collecting terminal or disconnect respectively.
2. sample pretreatment device as claimed in claim 1, it is characterized in that, described extraction column also has silica filler post and alumina packing post.
3. sample pretreatment device as claimed in claim 1, is characterized in that, be provided with the pressure transducer that can control to enter treating apparatus internal solvent pressure between described solvent pump and solid-phase extraction device.
4. sample pretreatment device as claimed in claim 1, is characterized in that, is provided with filtrator between described sample storage device and many logical sample introduction selector valves.
5. sample pretreatment device as claimed in claim 1, it is characterized in that, the outer setting of described sample pretreatment device casing has multiple fixed support, each described extraction column card is established and is fixed on described fixed support, is connected with the two way selected valve be arranged in described casing by flexible pipe and hose adapter.
6. the sample pretreatment device as described in any one of claim 1 to 5, is characterized in that, described two way selected valve, many logical sample introduction selector valves, many logical collection selector valves and switching device shifter are electrically-controlled valve.
7. a sample-pretreating method, is characterized in that, described sample-pretreating method utilizes the sample pretreatment device described in any one of claim 1 to 6, comprising:
1) by two way selected valve, each described extraction column is connected respectively successively with collecting terminal with the sample introduction end of described sample pretreatment device, many logical sample introduction selector valves select activating solvent successively, by solvent pump, described activating solvent is delivered to the described extraction column be connected with stream, one by one each described extraction column is activated, and through many logical selector valves of collecting, the activating solvent waste liquid after activating each described extraction column is delivered in the waste collection bottle of fraction collector;
2) by how, logical sample introduction selector valve is chosen as and is connected with sample storage device, disconnect the extraction column be connected with switching device shifter, and by described two way selected valve, other at least one described extraction column is connected with stream, by solvent pump by described sample delivery extremely described extraction column, described sample is collected in the waste collection bottle of fraction collector after flowing through many logical collection selector valves;
3) how drip washing solvent selected successively by logical sample introduction selector valve, and by described two way selected valve, at least one described extraction column is connected with stream, by solvent pump, described drip washing solvent is transported to described extraction column successively, drip washing is carried out to it, to make in sample chaff interference from drip washing extraction column; The object in sample is made to enter in fraction collector in corresponding Fraction collection bottle through many logical selector valves of collecting together with eluent solution, or making the object in sample be transferred on the next stage extraction column of series connection, described drip washing solvent to be selected to enter in fraction collector in corresponding Fraction collection bottle through many logical selector valves of collecting;
4) extraction column described in other is disconnected, the extraction column be connected with switching device shifter is only made to be connected with stream, and this extraction column is in reverse connected state, eluting solvent selected by described many logical sample introduction selector valves, make this eluting solvent reverse direction flow through described extraction column, reverse wash-out is carried out to it, is collected in Fraction collection bottle that the object in described eluting solvent and eluted sample to be collected in fraction collector by selector valve by many logical.
8. sample-pretreating method as claimed in claim 7, is characterized in that, described step 1) also comprise how multiple activating solvent selected successively by logical sample introduction selector valve, repeatedly activation process is carried out to extraction column described at least one.
9. sample-pretreating method as claimed in claim 7, is characterized in that, in described step 1), step 3), the extraction column be connected with switching device shifter is in forward connected state.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210477497.7A CN102967495B (en) | 2012-11-21 | 2012-11-21 | Sample pretreatment device and sample treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210477497.7A CN102967495B (en) | 2012-11-21 | 2012-11-21 | Sample pretreatment device and sample treatment method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102967495A CN102967495A (en) | 2013-03-13 |
| CN102967495B true CN102967495B (en) | 2015-04-01 |
Family
ID=47797787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210477497.7A Active CN102967495B (en) | 2012-11-21 | 2012-11-21 | Sample pretreatment device and sample treatment method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102967495B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048947B (en) * | 2014-05-23 | 2017-02-22 | 孟令启 | Method for detecting dioxin content in food |
| CN104316381B (en) * | 2014-11-05 | 2017-06-20 | 中国科学院生态环境研究中心 | The method of sample extraction, purification and concentration integrated device and sample pre-treatments |
| CN105092875A (en) * | 2015-09-24 | 2015-11-25 | 北京楚翔飞科技开发有限责任公司 | Full-automatic gas-liquid multi-purpose sample injector |
| CN105527147B (en) * | 2015-11-23 | 2018-05-22 | 浙江省海洋水产研究所 | A kind of seawater sample Extraction of Heavy Metals device |
| CN106018613B (en) * | 2016-06-23 | 2018-12-07 | 西安交通大学 | It can switch online and realize the concatenated solid-phase extraction device of multicolumn and its extracting process |
| CN111732149B (en) * | 2020-06-30 | 2023-06-23 | 自然资源部第四海洋研究所(中国—东盟国家海洋科技联合研发中心) | Seawater heavy metal multichannel pretreatment device and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1890562A (en) * | 2003-12-05 | 2007-01-03 | 财团法人杂贺技术研究所 | Method of analyzing organic chemical substance and apparatus for analysis |
| US20080209983A1 (en) * | 2003-12-05 | 2008-09-04 | Saika Technological Institute Foundation | Method of Analyzing Organic Chemical Substances and Apparatus for Analysis |
| CN101871856A (en) * | 2010-06-04 | 2010-10-27 | 陈小波 | Solid phase extraction and concentration system |
| CN102166433A (en) * | 2011-01-21 | 2011-08-31 | 北京莱伯泰科仪器有限公司 | Multichannel parallel automatic solid phase extraction device |
| CN202886166U (en) * | 2012-11-21 | 2013-04-17 | 北京普立泰科仪器有限公司 | Sample pretreatment device |
-
2012
- 2012-11-21 CN CN201210477497.7A patent/CN102967495B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1890562A (en) * | 2003-12-05 | 2007-01-03 | 财团法人杂贺技术研究所 | Method of analyzing organic chemical substance and apparatus for analysis |
| US20080209983A1 (en) * | 2003-12-05 | 2008-09-04 | Saika Technological Institute Foundation | Method of Analyzing Organic Chemical Substances and Apparatus for Analysis |
| CN101871856A (en) * | 2010-06-04 | 2010-10-27 | 陈小波 | Solid phase extraction and concentration system |
| CN102166433A (en) * | 2011-01-21 | 2011-08-31 | 北京莱伯泰科仪器有限公司 | Multichannel parallel automatic solid phase extraction device |
| CN202886166U (en) * | 2012-11-21 | 2013-04-17 | 北京普立泰科仪器有限公司 | Sample pretreatment device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102967495A (en) | 2013-03-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102967495B (en) | Sample pretreatment device and sample treatment method | |
| CN102078705B (en) | Tandem nano fiber solid phase extraction column | |
| CN103822999B (en) | A kind of full-automatic QuEChERS pre-treatment all-in-one and pre-treating method | |
| EP2807410A2 (en) | Liquid sampling valve | |
| CN203941163U (en) | A kind of glycolated hemoglobin analysis liquid road | |
| CN101206205B (en) | Method and isolated device for micro flux liquid chromatogram on-line large volume sample injection | |
| Quintana et al. | Online coupling of bead injection lab-on-valve analysis to gas chromatography: application to the determination of trace levels of polychlorinated biphenyls in solid waste leachates | |
| CN204255916U (en) | Gas chromatograph | |
| CN201161989Y (en) | Multicenter protein compatible chromatography purification instrument | |
| CN202886166U (en) | Sample pretreatment device | |
| CN108845056A (en) | A kind of on-line automatic pretreating device of aflatoxin based on flow path switching | |
| CN211877889U (en) | Chromatograph-mass spectrometer | |
| CN205175977U (en) | Take high -efficient gas chromatograph of antifouling device | |
| CN208636264U (en) | A kind of on-line automatic pretreating device of aflatoxin based on flow path switching | |
| CN102323433B (en) | Reagent precise quantitative sample-injection method and system | |
| CN103293253B (en) | Efficient purification-analysis system for biotechnological medicine and medicine separation detection method thereof | |
| CN212159315U (en) | Device for automatically enriching red tide toxins in concentrated seawater | |
| CN101329310A (en) | Full-automatic pressurization capillary electric chromatogram system | |
| CN103323560B (en) | Component separating preparation instrument | |
| CN202083677U (en) | Back-washing stream system for glycosylated hemoglobin analyzer | |
| CN108548879A (en) | A kind of quick detection device of automation | |
| CN208171864U (en) | Semiautomatic plant and detection device based on Solid Phase Extraction | |
| CN201993349U (en) | Semi-automatic gel permeation purification device | |
| CN208607187U (en) | A kind of online purification devices for liquid chromatogram | |
| CN204065037U (en) | A kind of full-automatic matrix dispersive solid-phase extraction pre-treatment all-in-one |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |