CN106289925A - A kind of combination bleeder two English pretreating device - Google Patents
A kind of combination bleeder two English pretreating device Download PDFInfo
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- CN106289925A CN106289925A CN201510274870.2A CN201510274870A CN106289925A CN 106289925 A CN106289925 A CN 106289925A CN 201510274870 A CN201510274870 A CN 201510274870A CN 106289925 A CN106289925 A CN 106289925A
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Abstract
The invention discloses a kind of combination bleeder two English pretreating device, comprising: the first cylindrical container, it has entrance and exit, and the top of described first cylindrical container is provided with expanding structure, is provided with purification filled column in the lower section of expanding structure in described first cylindrical container；Second cylindrical container, it has entrance and exit, the entrance of described second cylindrical container and the exit seal of the first cylindrical container connect, and the top of described second cylindrical container also is provided with expanding structure, are provided with separating filler post in the lower section of expanding structure in described second cylindrical container；Three way cock, the exit seal of its first interface and the second cylindrical container connects, and second interface of three way cock is in order to export processed liquid；Air extractor, it is connected with the 3rd interface of described three way cock.Combination bleeder two English pretreating device of the present invention is capable of completing the separation of two English samples, purification fast and efficiently, thus improves the efficiency of two English sample pretreatments.
Description
Technical field
The present invention relates to a kind of pretreatment unit for quickly analyzing, particularly relate to a kind of for organic contamination
The pretreatment unit that thing is quickly analyzed.
Background technology
Dioxins be many chloros dibenzo two English (Polychlorinated dibenzo-p-dioxins,
PCDDs) and the general name of polychlorinated dibenzofurans (Polychlorinated-dibenzofuran, PCDFs), it is
It is currently known one of maximum compound of toxicity.Owing to the dosage of dioxins is low, difficult degradation, appearance
Easily biological concentration, therefore, detection and analysis for dioxins receive significant attention.About holding
" Convention of Stockholm " of property organic pollution (POPs) formally existed on November 11st, 2004 for a long time
China comes into force." pact " should require that contracting party needed the chemicals in list appended by pact from coming into force
Matter is studied and controls, and wherein, two English just arrange at this.
Two English and the like have more isomer, and they are usual with ultra trace water in environmental sample
Flat (pg level) exists.The analysis of this type of material belongs to ultra trace, multi-component analysis, its for specificity,
The requirement of selectivity and sensitivity is high, so, analysis, detection to two English and the like are also rings
The difficult point of border analysis field.
Publication No. CN102062762A, publication date is on May 18th, 2011, entitled " the most pre-
Process the method for pedotheque for two English detections " Chinese patent literature disclose and a kind of have containing trace
The preprocess method of the sample of organic pollutants two English.This preprocess method includes: by pedotheque and oxidation
Aluminum, the copper powder mix homogeneously of 5:5:1 in mass ratio；Mixture is transferred to accelerated solvent extractor instrument abstraction pool
In, add two English and extract standard specimens and purify standard specimen, then with dichloromethane and normal hexane mixed solution as molten
Agent；Carry out soda acid silica column purification after sample concentration, again concentrate and transfer to the sample bottle with interpolation pipe
The nitrogen that middle use is eased up is blown to 20 μ about l, adds before after concentration, sample carries out the online mensuration of high-resolution chromaticness
Two English of 1000pg enter machine mark.Propose in the method and utilize the Accelerate solvent extraction system of commercialization
Realize the separation of two English samples.This system is used to be only capable of the separation of two English samples, but, purify
Process remains a need for by manual compound silica gel post.It addition, system Meteorological is expensive, cause two English inspections
Survey, analysis cost rises.Additionally, such system is only applicable to the detection of soil matrix sample, to not
It is applicable to the detection of other matrix sample.
Publication No. CN 102109505A, publication date is on June 29th, 2011, entitled " a kind of extraction
Take liquid pretreatment method for purifying " Chinese patent literature describe two English, Polychlorinated biphenyls in a kind of extract
Pretreatment method for purifying with PBDE.The method is included in the extraction module of Full-automatic solid phase extraction instrument
On be provided with compound silica gel post, alkali alumina post and Fu Luoli earth pillar composition decontaminating column, eluent by step
Rapid priority is divided into two kinds, and first step eluent is the mixed liquor of normal hexane and dichloromethane, second step eluent
For dichloromethane；All it is transferred in online concentrator after evaporation and concentration at each purification intercolumniation eluent, then turns
Move to carry out purified treatment on next decontaminating column.The process employs a kind of based on Full-automatic solid phase extraction instrument
In the self-purging sample extraction liquid of (SPE, J2scientific PrepLinc) PCDD/Fs, PCBs and
The analysis pretreatment technology of PBDEs.But, this analysis pretreatment technology is disadvantageous in that and must make
With the equipment (including solid-phase extracting instrument and concentrating instrument) of complete commercialization, and this analysis pre-treatment is for post
The sealing requirements of system is the highest, thus adds the pretreatment cost of two English samples.
Publication No. CN102539548A, publication date is on July 4th, 2012, entitled " one-stage process
The method and device of two English class materials in purification environmental matrices extract " Chinese patent literature disclose one
Plant the method and device of two English class materials in purification environmental matrices extract, comprising: prepare composite chromatography
Post, with normal hexane pre-drip washing composite chromatography post, add environmental matrices extract, successively in compound chromatographic column
With after normal hexane, normal hexane/dichloromethane mixed solution eluting impurity, again with dichloromethane two
Disliking the purifying step of English class material, the filler of described composite chromatography post is from bottom to top followed successively by silanized glass
Cotton, quartz sand, Fu Luoli magnesium silicate, deactivation alkali alumina, neutral silica gel, alkaline silica gel, neutral silicon
Glue, acidic silica gel and anhydrous sodium sulfate.The shortcoming of the method and device is: 1) to sulfur-bearing class chaff interference
Detergent power not enough, the two English samples high to sulfur content are inapplicable.2) due to aluminium oxide, Florey
Soil and compound silica gel are all on a chromatographic column, it is impossible to separate, and final step is when using the dichloro that polarity is the strongest
During methane eluting column system, it is most likely that by chaff interference and two English of target of the residual on compound silica gel post
Elute together, thus affect the testing result of two English, especially to substrate more complicated containing two English samples
Product are not appropriate for.
In patent documentation disclosed in above-mentioned three parts, the method disclosed in first and second parts of patent documentations is necessary
Realize quick two English sample pre-treatments by the expensive instrument of commercialization, so can be greatly improved two
The pre-treatment cost of English sample.3rd part of method and device disclosed in patent documentation to complex matrices two
Chaff interference may be introduced during English sample purification, thus affect the testing result of two English.Because of this it may be desirable to
Obtain the front place for quickly analyzing, detect two English that a kind of low cost, work efficiency are high and easy and simple to handle
Reason device.
Summary of the invention
It is an object of the invention to provide a kind of combination bleeder two English pretreating device, locate before this two English
Reason device can complete the separation of two English samples, purification fast and efficiently, thus improves two English samples
The efficiency of pre-treatment.It addition, the simple in construction of two English pretreating devices of the present invention, input cost
Few.Additionally, two English pretreating devices of the present invention can be greatly reduced the usage amount of organic solvent.
To achieve these goals, the present invention proposes a kind of combination bleeder two English pretreating device, its
Including:
First cylindrical container, it has entrance and exit, and the top of this first cylindrical container is provided with expanding structure,
It is provided with purification filled column in the lower section of expanding structure in first cylindrical container；
Second cylindrical container, it has entrance and exit, and the entrance of this second cylindrical container and the first cylindricality are held
The exit seal of device connects, and the top of the second cylindrical container also is provided with expanding structure, in the second cylindrical container
The lower section of expanding structure is provided with separating filler post；
Three way cock, the exit seal of its first interface and the second cylindrical container connects, the second of three way cock
Interface is in order to export processed liquid；
Air extractor, it is connected with the 3rd interface of three way cock.
Based on technique scheme, the outlet of the first cylindrical container is with the inlet seal of the second cylindrical container even
Connecing, the first interface of three way cock and the exit seal of the second cylindrical container connect, thus, it is desirable to separated,
The sample (or solvent) purified passes sequentially through the first cylindrical container, the second cylindrical container and three way cock, its
In, it is provided with purification filled column in the cylinder below expanding structure in the first cylindrical container to realize sample
Purification, be provided with separating filler post for complete in the cylinder below expanding structure in the second cylindrical container
Dioxin substance in sample is become to separate with other compounds.Here, due to the first cylindrical container and the second post
Describe that device is directly tightly connected, thus avoid liquid switching in different vessels, and then be greatly reduced
The usage amount of organic solvent, and it is effectively improved the response rate of liquid.
The top of the first cylindrical container is provided with expanding structure and can increase the place of single sample (or solvent)
Reason amount, reduces operator and contacts the frequency of harmful sample or solvent.Compare to be not provided with expanding structure, tool
The first cylindrical container having expanding structure can also be effectively prevented sample (or solvent) because of by the first cylindricality
Speed when purifying filled column in container is crossed slow and is made sample (or solvent) entering from the first cylindrical container
The phenomenon that mouth overflows occurs.
Similarly, there is the second cylindrical container of expanding structure, compare to be not provided with the second post of expanding structure
Describing device, it can advantageously avoid sample (or solvent) because of by the separating filler in the second cylindrical container
Speed during post is crossed slow and is caused the anti-situation about overflowing to the first cylindrical container of sample (or solvent) to occur.
Air extractor is connected with the 3rd interface of three way cock, with the two English pretreating devices for the present invention
Bleed so that two English pretreating devices are negative pressure or vacuum shape, thus improve sample (or solvent) and pass through
First cylindrical container and the speed of the second cylindrical container, and then improve the efficiency that device purifies, separates and collect.
Additionally, be positioned at length and the big I of internal diameter of the columnar part below the expanding structure of the first cylindrical container
To be designed according to practical situation, for example, it is possible to according to the kind of contained substance, sample in treated sample
The treating capacity of product is designed.Correspondingly, the columnar part below the expanding structure of the second cylindrical container it is positioned at
Length and internal diameter size can also be designed according to practical situation.
It should be noted that the entrance and exit of the first cylindrical container, the entrance and exit of the second cylindrical container
And second interface of three way cock all can be designed to frosted interface, thus realize the first cylindrical container and
Being tightly connected of two cylindrical containers and being tightly connected of the second cylindrical container and three way cock.Certainly, also may be used
Being tightly connected between said vesse and container, container and joint is realized in the way of taking other；Such as,
In the outlet of the first cylindrical container and the inlet connection of the second cylindrical container, sealing ring is set.
Further, combination bleeder two English pretreating device of the present invention also includes container containing,
Its import is connected with second sealing joint of three way cock, is used for depositing processed liquid.
Further, in combination bleeder two English pretreating device of the present invention, above-mentioned first
The expanding structure of cylindrical container and/or the expanding structure of the second cylindrical container are spherical or almost spherical.
Expanding structure based on technical scheme, the first cylindrical container and/or the second cylindrical container is also
It is not limited to spherical.This expanding structure can also use longitudinal section to be square or trapezoidal structure.
Further, in combination bleeder two English pretreating device of the present invention, above-mentioned first
Cylindrical container and/or the second cylindrical container are glass material or politef material.
Further, in combination bleeder two English pretreating device of the present invention, above-mentioned first
The lower section purifying filled column in cylindrical container is provided with the baffle plate of eye, in order to regulate liquid by the first cylindricality
The speed purifying filled column in container.
It is to say, compare to be not provided with the situation of baffle plate, when the lower section purifying filled column is provided with eye
During baffle plate, flow through and purify the speed of liquid of filled column and can slow down so that liquid can fully with purification
Compound reaction in filled column, thus improve clean-up effect.
Under a kind of embodiment, the eyelet internal diameter of the baffle plate in the first cylindrical container is 2-5mm.
In order to regulation flows through the speed of the liquid purifying filled column more accurately, by the eyelet of above-mentioned baffle plate
Inside diameter ranges is set between 2-5mm.
Under yet other embodiments, the baffle plate in the first cylindrical container and purify between filled column and be provided with glass cotton
Layer, to regulate liquid further by purifying the flow velocity of filled column.
It should be noted that the number of plies of the glass cotton layer being arranged between baffle plate and purification filled column can basis
The size needing flow velocity is set.
Further, in combination bleeder two English pretreating device of the present invention, above-mentioned second post
Describe that the lower section of separating filler post is provided with the baffle plate of eye in device, held by the second cylindricality in order to regulate liquid
The speed of the separating filler post in device.
Similarly, compare to be not provided with the situation of baffle plate, when the lower section of separating filler post is provided with the gear of eye
During plate, the flow velocity of liquid by separating filler post can be reduced so that liquid can fully and separating filler post
In compound reaction, thus improve separating effect.
Under a kind of embodiment, the eyelet internal diameter of the baffle plate in the second cylindrical container is 2-5mm.
Correspondingly, the eyelet inside diameter ranges of the baffle plate in the second cylindrical container is set between 2-5mm
Purpose is more accurately to regulate the flow velocity of the liquid by separating filler post.
Under yet other embodiments, it is provided with glass cotton between the baffle plate in the second cylindrical container and separating filler post
Layer, to regulate the liquid flow velocity by separating filler post further.
Additionally, the number of plies of the glass cotton layer being arranged between baffle plate and separating filler post can flow velocity as required
Size be set.
Closer, in combination bleeder two English pretreating device of the present invention, above-mentioned purification
Filled column includes at least one of which neutral silica gel separate layer and anhydrous with what neutral silica gel separate layer was correspondingly arranged
At least one of sodium sulfate layer, silver nitrate layer of silica gel, acidic silica gel layer and alkaline silica gel layer, wherein,
Neutral silica gel layer is relative to corresponding anhydrous sodium sulfate layer, silver nitrate layer of silica gel, acidic silica gel layer and alkali
At least one of property layer of silica gel is located at below.
Based on technique scheme, it is arranged at the scavenging material purified in filled column and can only include anhydrous slufuric acid
One of them of sodium layer, silver nitrate layer of silica gel, acidic silica gel layer or alkaline silica gel layer, it is also possible to be above-mentioned only
The combination in any of formed material.
It should be noted that anhydrous sodium sulfate layer, silver nitrate layer of silica gel, acidic silica gel layer and alkaline silica gel layer
It is required for arranging neutral silica gel separate layer Deng the lower section of scavenging material.It is to say, which kind of no matter selects purify
Material, the compound mode of scavenging material how, and each scavenging material needs and neutral silica gel separate layer takes interval
Mode is configured.
Preferably, above-mentioned purification filled column includes the most successively: anhydrous sodium sulfate layer, neutral silica gel layer,
Silver nitrate layer of silica gel, neutral silica gel layer, acidic silica gel layer, neutral silica gel layer, alkaline silica gel layer and neutral silicon
Glue-line.
Under a kind of embodiment, the weight of described anhydrous sodium sulfate layer is 1-50g, is positioned at anhydrous sodium sulfate
The weight of the neutral silica gel layer below Ceng is 1-50g, the weight of described silver nitrate layer of silica gel is 1-50g, is positioned at
The weight of the neutral silica gel layer below silver nitrate layer of silica gel is 1-50g, the weight of described acidic silica gel layer is
1-50g, the weight being positioned at the neutral silica gel layer below acidic silica gel layer are 1-50g, described alkaline silica gel layer
Weight is 1-50g, and the weight being positioned at the neutral silica gel layer below alkaline silica gel layer is 1-50g.
Further, in combination bleeder two English pretreating device of the present invention, above-mentioned separation
Filled column includes alkaline oxygenated aluminium lamination or active carbon layer or Florey soil layer.
Further, above-mentioned separating filler post also includes being positioned at alkaline oxygenated aluminium lamination or active carbon layer or not Lip river
In anhydrous sodium sulfate layer above soil layer.
Under a kind of embodiment, the weight of above-mentioned anhydrous sodium sulfate layer is 1-50g.
Under yet other embodiments, the weight of above-mentioned alkaline oxygenated aluminium lamination is 5-50g.
It should be noted that combination bleeder two English pretreating device of the present invention not merely limits to
In the pre-treatment of dioxin substance, it can also carry out pre-treatment to the analog of two English.
Combination bleeder two English pretreating device of the present invention can realize two English efficiently, rapidly
The purification of sample and separation, thus improve the pre-treatment efficiency of two English samples, shorten the pre-treatment time.
It is it addition, the simple structure of combination bleeder two English pretreating device of the present invention, easy and simple to handle,
Do not expend time and manpower.
Additionally, combination bleeder two English pretreating device of the present invention can efficiently reduce solvent
Usage amount, reduce a staff contact harmful substance (including two English sample and organic solvents) time and
The frequency, has good economical and environmentally friendly benefit.
Accompanying drawing explanation
Fig. 1 is that combination bleeder two English pretreating device of the present invention is under a kind of embodiment
Structural representation.
Fig. 2 is that the first cylindrical container in combination bleeder two English pretreating device of the present invention exists
A kind of structural representation under embodiment.
Fig. 3 is that the second cylindrical container in combination bleeder two English pretreating device of the present invention exists
A kind of structural representation under embodiment.
Fig. 4 is that the container containing in combination bleeder two English pretreating device of the present invention is in one
Structural representation under embodiment.
Fig. 5 is that the three way cock in combination bleeder two English pretreating device of the present invention is in one
Structural representation under embodiment.
Fig. 6 is the structural representation under a kind of embodiment of the baffle plate in the first cylindrical container shown in Fig. 2
Figure.
Fig. 7 is the structural representation under a kind of embodiment of the baffle plate in the second cylindrical container shown in Fig. 3
Figure.
Detailed description of the invention
Below in conjunction with Figure of description and specific embodiment to combination bleeder two of the present invention
English pretreating device makes further explanation, but, this explanation and explanation not skill to the present invention
The improper restriction of art forecast scheme configuration.
Fig. 1 shows that combination bleeder two English pretreating device of the present invention is under a kind of embodiment
Structure.Fig. 2, Fig. 3, Fig. 4 and Fig. 5 then respectively illustrate combination bleeder two of the present invention
The first cylindrical container, the second cylindrical container, container containing and three way cock in English pretreating device are in one
Structure under embodiment.
As shown in Figures 1 to 5, the combination bleeder two English pretreating device bag under above-mentioned embodiment
Include first cylindrical container the 1, second cylindrical container 2, three way cock 3, container containing 4 and air extractor (not
Figure 1 illustrates).Wherein, the first cylindrical container 1 has entrance 11 and outlet 12, holds in the first cylindricality
The top of device 1 is provided with expanding structure 13, below expanding structure 13 first in this first cylindrical container 1
Purification filled column (illustrating the most in fig. 1 and 2) it is provided with in cylinder 14；Second cylindrical container 2 have into
Mouth 21 and outlet 22, the entrance 21 of this second cylindrical container 2 seals with the outlet 12 of the first cylindrical container
Connecting, the top of this second cylindrical container 2 also is provided with expanding structure 23, the expansion in the second cylindrical container 2
It is provided with separating filler post (not shown in Fig. 1 and Fig. 3) in the second cylinder 24 below gauge structure 23；
Three way cock 3 has first interface the 31, second interface 32 and the 3rd interface 33, the first of three way cock 3
Interface 31 is tightly connected with the outlet 22 of the second cylindrical container 2；Container containing 4 has import 41 and contains
Dress body 42, second interface 32 of three way cock 3 is tightly connected with the import 41 of container containing 4, in order to
The processed liquid of output；Air extractor is tightly connected with the 3rd interface 33 of three way cock.
Additionally, the entrance of the outlet of the first cylindrical container and the second cylindrical container is frosted interface, thus real
Being tightly connected of existing first cylindrical container and the second cylindrical container.
As shown in Figure 1, Figure 2 and Figure 3, the expanding structure 13 of the first cylindrical container 1 and the second cylindrical container
The expanding structure 23 of 2 all uses spherical structure.
As shown in Figure 1 and Figure 4, the overall structure of container containing 4 is also adopted by being similar to spherical structure.
Here, the first cylindrical container and/or the second cylindrical container can use glass material or politef material
Matter etc. are appropriate to Organic substance purification, the material of lock out operation.Similarly, container containing can also use glass
Glass material or politef material.
The baffle plate that Fig. 6 and Fig. 7 respectively illustrates in the first cylindrical container and the second cylindrical container is implemented in one
Structure under mode.
As shown in Figure 1, Figure 2 with shown in Fig. 6, the lower section purifying filled column in the first cylindrical container 1 is provided with band
The baffle plate 15 of eyelet 16 flows through the speed of purification filled column, the eyelet 16 of this baffle plate 15 in order to regulate liquid
Internal diameter can be set as 2-5mm.It addition, be additionally provided with glass cotton layer between baffle plate 15 and purification filled column
17 (due to glass cotton layer 17 thinner thicknesses, thus fail to illustrate this glass cotton layer the most significantly),
To control liquid further by purifying the flow velocity of filled column.
As shown in Fig. 1, Fig. 3 and Fig. 7, in the second cylindrical container 2, the lower section of separating filler post is provided with band
The baffle plate 25 of eyelet 26 flows through the speed of purification filled column, the eyelet 26 of this baffle plate 25 in order to regulate liquid
The scope of design of internal diameter can be 2-5mm.Additionally, be additionally provided with glass between baffle plate 25 and separating filler post
Glass cotton layer 27 (due to glass cotton layer 27 thinner thickness, thus fails to illustrate this glass the most significantly
Cotton layer), to control the liquid speed by separating filler post further.
Use the combination bleeder two English pretreating device under above-mentioned embodiment, and divide as steps described below
Not pre-treatment do not carries out for 4 environmental samples (flue gas sample) containing two English:
1) load purification filled column: use dry method to fill out post method, the first cylindrical container loads purification and fills out
Stock column, wherein, if this purification filled column include dried layer neutral silica gel separate layer and with neutral silica gel separate layer
Anhydrous sodium sulfate layer, silver nitrate layer of silica gel, acidic silica gel layer and the alkaline silica gel layer being correspondingly arranged, this purification
Filled column includes the most successively: anhydrous sodium sulfate layer-neutral silica gel layer-silver nitrate layer of silica gel-neutral silica gel
Layer-acidic silica gel layer-neutral silica gel layer-alkaline silica gel layer-neutral silica gel layer, the weight of each layer in purification filled column
Amount can be chosen according to actual needs by those skilled in the art in the framework of the present definition；
2) separating filler post is loaded: in the second cylindrical container, load separating filler post, wherein, separate
The filling material of filled column is selected from alkaline oxygenated aluminium lamination or active carbon layer or Florey soil layer, and in alkalescence
The top of alumina layer or active carbon layer or Florey soil layer is filled with corresponding anhydrous sodium sulfate layer, and separation is filled out
The type of each layer in stock column and weight can be by those skilled in the art according to actual needs at these
Choose in the range of bright restriction；
3) preparation of samples: preparing environment sample, after toluene surname extraction, and by above-mentioned sample concentration
To 0.3ml, before sample purification separates, it is quantitatively adding 13C labelling 2,3,7,8-substituted two English toxicity
Congener；
4) pre-drip washing: the normal hexane of 100ml is poured into from the entrance 11 of the first cylindrical container 1, liquid
Flow out from the outlet 22 of the second cylindrical container 2, contain via three way cock 3 and by container containing 4,
In the process, the air extractor being tightly connected with the 3rd interface 33 of three way cock 3 is bled, and accelerates the
The pre-drip washing speed of the separating filler post purified in filled column and the second cylindrical container 2 in one cylindrical container 1
Degree, when the purification filled column in the first cylindrical container 1 and the separating filler post in the second cylindrical container 2 while
After completing pre-drip washing, close air extractor；
5) loading: extract the sample solution after concentrating, falls it from the entrance 11 of the first cylindrical container 1
Enter；
6) purify+separate: open air extractor in order to accelerate sample solution by the first cylindrical container 1 He
The flow velocity of the second cylindrical container 2, thus improve the efficiency of sample purification, separation, pour the just own of 100ml into
Alkane drip washing purifies, and first leacheate is through the purification filled column of the first cylindrical container 1, to remove in sample
Impurity thus complete the purification of sample, then the separating filler post through the second cylindrical container 2, two English and furan
Compounds of muttering is retained on separating filler post, other copline compounds similar to two English structures
(such as, the chlorobenzene of low pole, Polychlorinated biphenyls and terphenyl and many chlorinated diphenyl ethers) is leached,
This part leacheate removes after container containing 4 is collected need not；
7) detection liquid is collected: close air extractor, first remove the first cylindrical container 1, then open and take out
Device of air, with the dichloromethane of 100ml/normal hexane mixed solution (50:50) eluting the second cylindrical container 2
Separating filler post, by under two English being stranded on separating filler post and the complete eluting of furfuran compound
Come, and utilize container containing 4 to be collected；
8) detection liquid is concentrated: after the liquid concentration that will collect, by high-resolution gas chromatogram high-resolution
Magnetic substance spectrum detects.
It should be noted that due in the step (3) chemical property of the 13C label of titration with divided
The chemical property of the component in analysis sample is completely the same, therefore, and the loss in above-mentioned sample pretreatment process
Also it is identical, can characterize, with the response rate of mark substance, the accuracy that dioxin substance is analyzed.
In order to show the technique effect using combination bleeder two English pretreating device of the present invention, right
4 kinds of identical environmental samples are processed by the two English pretreating devices that ratio does not use this case to relate to,
But have employed existing conventional treatment method.
Table 1 lists in each sample after this case embodiment and comparative example process for 4 kinds of environmental samples
The toxic equivalent concentration of 17 kind of two English monomer.
Table 1.
* note: A1-A4 represents each two English lists in the sample after using combination bleeder two English pretreating device of the present invention to process for 4 kinds of environmental samples
The toxic equivalent concentration of body, at B1-B4 all represents that the prior art being provided without combination bleeder two English pretreating device of the present invention is for 4 kinds of environmental samples
The toxic equivalent concentration of each two English monomers in the sample after reason, C1-C4 represents relative standard deviation between embodiment A1-A4 and comparative example B1-B4 respectively.
17 kind of two English monomer in table 1 is 17 kinds of dioxin monomers of EPA standard-required detection, and it is known to those skilled in that art.
As can be seen from Table 1, this case embodiment and prior art comparative example are for two in test environment sample
All≤30%, it meets general international standard, U.S. environment to the relative standard deviation of the detected value of English concentration
The requirement of protection administration (US Environmental Protection Agency is called for short EPA) examination criteria.With
Time, as can also be seen from Table 1, the relative standard deviation all≤10% of two English concentration of major part sample.
Therefore, table 1 indicates and uses combination bleeder two English pretreating device of the present invention to carry out sample
Process is the accuracy that can ensure that testing result.
Table 2 list the embodiment using combination bleeder two English pretreating device of the present invention for
4 kinds of environmental samples carry out processing the response rate of two English monomers of rear 15 kinds of tape labels, and what it characterized is detection
During the extent of damage of sample.
Table 2.
| Dioxin monomer | A1 (%) | A2 (%) | A3 (%) | A4 (%) |
| 13C-2378-TCDD | 74.9 | 100 | 96.3 | 94.6 |
| 13C-12378-PeCDD | 74.1 | 98.9 | 111.6 | 108.7 |
| 13C-123678-HxCDD | 75.5 | 101.9 | 116.1 | 88.2 |
| 13C-1234678-HpCDD | 92.6 | 112.3 | 101.4 | 89.4 |
| 13C-OCDD | 103 | 128.5 | 80.9 | 72.7 |
| 13C-2378-TCDF | 68.8 | 84.3 | 97 | 95.8 |
| 13C-12378-PeCDF | 72.7 | 85.7 | 97.3 | 106.1 |
| 13C-123678-HxCDF | 86.8 | 96 | 99.8 | 89.5 |
| 13C-1234678-HpCDF | 85.5 | 100.6 | 89.7 | 75.5 |
| 37Cl-2378-TCDD | 42.9 | 97.9 | 90.6 | 92.7 |
| 13C-123478-HxCDD | 68.1 | 96.8 | 57.1 | 68.4 |
| 13C-23478-PeCDF | 67 | 93.5 | 93 | 95 |
| 13C-123478-HxCDF | 69.9 | 91.1 | 88.7 | 84.2 |
| 13C-1234789-HpCDF | 91.8 | 109.8 | 71.7 | 53.9 |
| 13C-123789-HxCDF | 82.4 | 96.2 | 68 | 62.3 |
Note: listed by table 2 is according to EPA standard two English monomers of 15 kinds of tape labels of carbon 13 mark substance of addition during detection.
As can be seen from Table 2, use combination bleeder two English pretreating device of the present invention for sample
Product carry out pre-treatment, and the response rate of two English monomers can reach 70～120%, and existing two English are examined
The two English response rate in mark standard require that maximum magnitude is 17-181%, and this explanation employing the technical program can
With the loss of sample during reduction detection, it is far above standard-required.
Additionally, after combination bleeder two English pretreating device in employing above-described embodiment, single sample
The time purify, separated foreshortens to about 60min.Compare to the time required in prior art, purify,
The time separated shortens 50%, thus is effectively improved the efficiency of the pre-treatment of two English sample detection.
It addition, the usage amount of organic solvent is reduced to about 310ml from 520ml, decrease the organic solvent of 40%
Usage amount.Owing to the detection of dioxin substance belongs to ultra trace analysis, organic solvent must use impurity to contain
Measuring few and expensive agriculture residual level organic solvent, therefore, the minimizing of organic solvent usage amount can be effective
Ground reduces the pretreatment process cost of two English samples.
It should be noted that the listed above specific embodiment being only the present invention, it is clear that the invention is not restricted to
Above example, has the similar change of many therewith.If those skilled in the art is open from the present invention
Content all deformation of directly deriving or associating, protection scope of the present invention all should be belonged to.
Claims (17)
1. a combination bleeder two English pretreating device, it is characterised in that including:
First cylindrical container, it has entrance and exit, and the top of described first cylindrical container is provided with expansion
Gauge structure, is provided with purification filled column in the lower section of expanding structure in described first cylindrical container；
Second cylindrical container, it has entrance and exit, the entrance and first of described second cylindrical container
The exit seal of cylindrical container connects, and the top of described second cylindrical container also is provided with expanding structure, institute
It is provided with separating filler post in the lower section of expanding structure in stating the second cylindrical container；
Three way cock, the exit seal of its first interface and the second cylindrical container connects, three way cock's
Second interface is in order to export processed liquid；
Air extractor, it is connected with the 3rd interface of described three way cock.
2. combination bleeder two English pretreating device as claimed in claim 1, it is characterised in that also include
Container containing, its import is connected with second sealing joint of described three way cock.
3. combination bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
The expanding structure of the expanding structure and/or the second cylindrical container of stating the first cylindrical container is spherical or approximation
Spherical.
4. combination bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
State the first cylindrical container and/or the second cylindrical container is glass material or politef material.
5. combination bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
The lower section purifying filled column in stating the first cylindrical container is provided with the baffle plate of eye.
6. combination bleeder two English pretreating device as claimed in claim 5, it is characterised in that described gear
The eyelet internal diameter of plate is 2-5mm.
7. combination bleeder two English pretreating device as claimed in claim 5, it is characterised in that described gear
It is provided with glass cotton layer between plate and purification filled column.
8. combination bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
State the lower section of separating filler post in the second cylindrical container and be provided with the baffle plate of eye.
9. combination bleeder two English pretreating device as claimed in claim 8, it is characterised in that described gear
The eyelet internal diameter of plate is 2-5mm.
10. combination bleeder two English pretreating device as claimed in claim 8, it is characterised in that described gear
Glass cotton layer it is provided with between plate and separating filler post.
11. combination bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
State purification filled column and include at least one of which neutral silica gel separate layer and corresponding with neutral silica gel separate layer
Arrange anhydrous sodium sulfate layer, silver nitrate layer of silica gel, acidic silica gel layer and alkaline silica gel layer at least its
One of, wherein, neutral silica gel layer is relative to corresponding anhydrous sodium sulfate layer, silver nitrate silica gel
At least one of layer, acidic silica gel layer and alkaline silica gel layer is located at below.
12. combine bleeder two English pretreating device as claimed in claim 11, it is characterised in that described
Purify filled column to include the most successively: anhydrous sodium sulfate layer, neutral silica gel layer, silver nitrate silica gel
Layer, neutral silica gel layer, acidic silica gel layer, neutral silica gel layer, alkaline silica gel layer and neutral silica gel layer.
13. combine bleeder two English pretreating device as claimed in claim 12, it is characterised in that described
The weight of anhydrous sodium sulfate layer is 1-50g, be positioned at the weight of neutral silica gel layer below anhydrous sodium sulfate layer
Amount is 1-50g for 1-50g, the weight of described silver nitrate layer of silica gel, is positioned at below silver nitrate layer of silica gel
The weight of neutral silica gel layer be 1-50g, the weight of described acidic silica gel layer is 1-50g, is positioned at acid
The weight of the neutral silica gel layer below property layer of silica gel is 1-50g, the weight of described alkaline silica gel layer is
1-50g, the weight being positioned at the neutral silica gel layer below alkaline silica gel layer is 1-50g.
14. combine bleeder two English pretreating device as claimed in claim 1 or 2, it is characterised in that institute
State separating filler post and include alkaline oxygenated aluminium lamination or active carbon layer or Florey soil layer.
15. combination bleeder two English pretreating device as claimed in claim 14, it is characterised in that described
Separating filler post also includes being positioned at the nothing above alkaline oxygenated aluminium lamination or active carbon layer or Florey soil layer
Aqueous sodium persulfate layer.
16. combine bleeder two English pretreating device as claimed in claim 15, it is characterised in that described
The weight of anhydrous sodium sulfate layer is 1-50g.
17. combination bleeder two English pretreating device as claimed in claim 15, it is characterised in that described
The weight of alkaline oxygenated aluminium lamination is 5-50g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510274870.2A CN106289925A (en) | 2015-05-26 | 2015-05-26 | A kind of combination bleeder two English pretreating device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510274870.2A CN106289925A (en) | 2015-05-26 | 2015-05-26 | A kind of combination bleeder two English pretreating device |
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| CN106289925A true CN106289925A (en) | 2017-01-04 |
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|---|---|---|---|
| CN201510274870.2A Pending CN106289925A (en) | 2015-05-26 | 2015-05-26 | A kind of combination bleeder two English pretreating device |
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| CN110907259A (en) * | 2019-11-21 | 2020-03-24 | 俞峰 | Dioxin purification enrichment column and enrichment method thereof |
| CN115963213A (en) * | 2023-02-08 | 2023-04-14 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107064395A (en) * | 2017-06-09 | 2017-08-18 | 中国环境科学研究院 | Compound silica gel post and the pre-treating method for analyzing organic pollution in sample |
| CN107064395B (en) * | 2017-06-09 | 2018-12-25 | 中国环境科学研究院 | Comprehensive silicon rubber column gel column and pre-treating method for analyzing organic pollutant in sample |
| CN110907259A (en) * | 2019-11-21 | 2020-03-24 | 俞峰 | Dioxin purification enrichment column and enrichment method thereof |
| CN115963213A (en) * | 2023-02-08 | 2023-04-14 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium |
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