CN105758688A - Dispersing liquid-liquid micro extraction kit - Google Patents

Abstract

The invention relates to a dispersing liquid-liquid micro extraction kit, comprising an extraction bottle, an extract collector and a sample injector vial.A bottom opening of the extraction bottle is elliptic cylindrical or cylindrical and is provided with a conical collecting recess (6); the top of the extraction bottle is provided with a screw port and fitted with a seal gasket and a screw cap matching with the screw port to seal the top; the extract collector is used for collecting extract having less extracting solvent density than water and comprises a transparent tube (7) and a collection hood (9) with a handle (8), and maximum outer diameter of the collection hood (9) matches with inner diameter of the upper portion of the extraction bottle; the sample injector vial comprises a body (10) in which a conical tube (11) is arranged.The dispersing liquid-liquid micro extraction kit has the advantages of wide applicable range, processing simplicity, operation simplicity and convenience, high repeatability, high recycling rate, higher determination accuracy, and easiness for enabling automatic batch processing of samples.

Description

A kind of dispersion liquid-liquid micro-extraction external member

Technical field

The present invention relates to extraction equipment.

Background technology

The pollution of water body is on the rise by organic compound in recent years, and its level of pollution increasingly comes into one's own with health effect research.The U.S. in 1977 State Bureau of Environmental Protection (USEPA) is according to the toxicity of organic pollution, biodegradable possibility and the factor such as probability occurred in water body, from 7 Ten thousand kinds of organic compound filter out the pollutant of 65 129 kinds of priority acccess control of class, wherein organic compound 114 kinds, accounts for the 88.4% of sum, bag Include 21 kinds of insecticides, 26 kinds of halogenated aliphatic hydrocarbons, 8 kinds of Polychlorinated biphenyls, 11 kinds of phenol, 7 kinds of nitrous acid and other compound.These compounds itself Having certain biological accumulation, some is own toxic, and some has three-induced effect.Surface water, underground water, Drinking Water, sanitary sewage, work Tremendous influence is there is in the Organic Pollutants In Water residuals such as industry waste water, seawater to production and the life of the mankind.Long Term Contact or drink by mutagenesis, The water that carcinogen pollutes, can make the incidence of disease of cancer in the crowd of drinking increase.Therefore the study on monitoring one to dissimilar Organic Pollutants In Water Straight attention.

In analyzing water body, organic pollution method is a lot.Traditional liquid-liquid extraction method is with low cost, applied widely, but need to use substantial amounts of organic reagent Extracting sample, organic solvent generally has high volatility, high toxicity and combustibility, easily causes secondary environmental pollution and causes security incident； Solid phase extraction purifies while water sample is enriched with, and eliminates Matrix effects impact, improves the degree of accuracy of analysis, and the method is easily achieved Automation, but operating technology difficulty is high, instrument and equipment somewhat expensive；Flow Injection on-line preconcentration, Solid-phase Microextraction, membrane extraction and solid-state Extraction stirring rod technology have do not use or use less organic solvent, simple to operate, amount of samples is few, the detection limit advantage such as low.But above skill at present The aspects such as art is in conceptual phase more, method stability there is also certain problem, is difficult to promote, need to study further.Liquid-liquid micro-extraction method is root According to the liquid-liquid extraction method extracting a small amount of fluid sample with a small amount of organic solvent.The method overcome tradition liquid-liquid extraction sample and extractant consumption be big, The defect that environmental pollution is big, has sample and quick, the degree of accuracy few, simple, convenient of extractant consumption and highly sensitive, no cross contamination And advantages of environment protection, the operation of its extracting and enriching has good compatibility with subsequent detection method, and extraction phase can be used directly gas-chromatography, height Effect liquid phase chromatogram, thin-layer chromatography, gas chromatography-mass spectrum, spectrophotometric, flame atomic absorption spectrometry and Electrothermal atomic absorption spectrometry, to targeted Compound is measured.It is applicable not only to the separation and concentration of trace organic substance, is also applied for the separation and concentration of trace inorganic metal ion, the most successfully It is applied to the separation and concentration of trace components in various bad borders water sample (including high salinity water sample), various beverages, biological sample, coal and mineral samplers, It it is a kind of rising eco-friendly separation and concentration technology.

Dispersion liquid-liquid micro-extraction technique (DLLME) be first be rapidly injected in the centrifuge tube filling sample solution in advance a certain amount of extractant and The mixed liquor of dispersant, sample solution forms the emulsion system of a water/dispersant/extractant, organic extraction after vibrating or be ultrasonically treated gently Contact surface between agent microballon and sample solution is relatively big, and determinand is extracted into rapidly in extractant microballon, and extraction equilibrium is quickly completed, more by centrifugation Or other mode split-phases, direct injected or be analyzed after being dissolved in suitable solvent after taking out with microsyringe and measuring organic extractant volume.Should Method collection separates and is enriched in one, it is to avoid the loaded down with trivial details operating process such as traditional liquid-liquid extraction separates, shifts, concentration, be one easy and simple to handle, Quickly, low cost, bioaccumulation efficiency height and the sample pre-treatments new technology of environmental protection.

The dispersion liquid-liquid micro-extraction device of multi-form differs from one another at present.But these extraction external members are relative complex, with wanting that DLLME simplifies Ask inconsistent.All kinds of dispersion liquid-liquid micro-extraction devices are faced with similar defect and deficiency:

(1) seeing in applicability angle, dispersion liquid-liquid micro-extraction device majority may be only available for the extraction that extractant density is bigger than water, and minority can be real The extraction that existing extractant density is less than water, but extraction equipment is complicated, operation easier is big, fragile, and two kinds of extraction modes can not take into account, extract Stability and poor repeatability.

(2) in terms of effect of extracting angle, dispersion liquid-liquid micro-extraction external member the most on the market, it is usually applicable only to manually shake extraction, it is impossible to realize Automation batch processing sample.

(3) the emulsification problem solution angle easily produced from operating process, centrifugal process is to eliminate the simple effective method of emulsification, but right It is positioned at the design of extraction flask bottom extraction flask (simultaneously also can be as centrifuge tube) in extract, has employing without special collecting pipe, be difficult to draw extraction Liquid；Bottom is had to use opening to add the mode that rubber cushion seals, though the extract bottom easily gathering, but fluid seepage problem when being also susceptible to centrifugal.

Summary of the invention

It is an object of the invention to combine the feature of dispersion liquid-liquid micro-extraction, it is provided that one is applied widely, it is simple, simple to operation, reproducible to process, The rate of recovery is high, measure more accurately and easily be automated the dispersion liquid-liquid micro-extraction external member of batch processing sample.Technical scheme is as follows:

A kind of dispersion liquid-liquid micro-extraction external member, including extraction flask, extract collecting means and three parts of injector bottle, it is characterised in that

Bottleneck profile bottom described extraction flask is elliptical cylinder-shape or cylinder, offers cone-shaped collection groove (6)；Top offers screw socket, and joins There is the sealing gasket and blind nut mated with screw socket, be used for sealing top；

Described extract collecting means, for realizing the collection of the extractant density extract less than water, including transparent pipe (7) with handle (8) collecting hood (9), the maximum outside diameter of collecting hood (9) matches with extraction flask top bottle internal diameter, when collecting extract from extraction flask top Portion stretches into after in extraction flask can be close to bottle inwall；One end of transparent pipe (7) is fixed on handle (8)；

Described injector bottle includes bottle (10), is within it placed with conical pipe (11), by sampling probe from the extraction of extraction flask bottom collection Liquid or from extract collecting means transparent pipe (7) collect extract collection after be placed in the conical pipe of injector bottle.

The present invention compared with prior art has the advantage that

(1) seeing in applicability angle, owing to bottom is provided with taper extract feeder, this device goes for the extraction that extractant density is bigger than water Take the collection of liquid；And the design of extract collecting hood can realize the collection of the extractant density extract less than water, two kinds of extraction modes are taken into account, Extraction stability and reproducible.

(2) in terms of effect of extracting angle, add the design of sealing gasket owing to extraction flask open top end have employed blind nut, be both possible to prevent extraction process to send out Raw leakage, can be replaced by mechanical force again and manually shake extraction, is advantageously implemented automation batch processing sample.

(3) after centrifugal process eliminates emulsification, extract is positioned to the design of extraction flask bottom extraction flask (simultaneously also can be as centrifuge tube), if In respect of special taper extract feeder, it is simple to make extract concentrate, easily draw extract；Outer wall uses circular-arc-shaped design simultaneously, is possible to prevent Extraction flask is made to rupture owing to pressure is relatively big time centrifugal.

(4) this extraction external member structure is simple, be easy to processing, easily operated, sealing gasket and seal lid and select universal material and size.

(5) extract taken out can load in the sample injection bottle being built-in with conical pipe, replaces for the ease of realizing automatic sampler auto-programming sample introduction Hand sampling, improves accuracy and the sample introduction efficiency of sample introduction.For micro-extraction device, extraction liquid measure is trace, if at the bottom of being split in bottle, then adding Sampling greatly difficulty, automatic sampler absorption extract is easy in conical pipe design.

Accompanying drawing explanation

Fig. 1 is the structure chart of the dispersion liquid-liquid micro-extraction bottle of the present invention.

Fig. 2 is the extract collecting means structure chart that extract density is less than water sample.

Fig. 3 is extract sample injection bottle structure chart.

Label declaration in figure: 1 blind nut；2 sealing gaskets；3 polytetrafluorethylecoatings coatings liners；4 screw sockets；5 extraction flasks；6 cone-shaped collection grooves； 7 transparent glass tubes；8 handles；9 collecting hoods；10 automatic sampler bottles；11 conical pipes

Detailed description of the invention

The present invention will be described with embodiment below in conjunction with the accompanying drawings.

See Fig. 1, Fig. 2 and Fig. 3, the dispersion liquid-liquid micro-extraction external member that the present invention provides, specifically include different size glass extraction flask (Fig. 1), The profile of bottom bottleneck is oval, its interior tapered, it is simple to the collection of extract.There is outside extraction flask open top screw socket 4, blind nut 1 He Extract and sample are sealed by the sealing gasket 2 of tool polytetrafluorethylecoatings coatings 3 by blind nut 1.The extract less than water sample for extract density uses Extract collecting means (Fig. 2) is collected, and including transparent glass tube 7 with the collecting hood 9 of handle 8, collecting hood 9 uses polytetrafluoroethylene (PTFE) Material.The outer wall of the collecting hood 9 of extract collecting means can fit tightly by inwall open-topped with extraction flask, and handle facilitates the receipts of extract collecting means Collection operation, transparent glass tube 7 shows position and the extract volume of extract, it is simple to sampling probe extraction extract.Fig. 3 is that internal glass of placing is bored The auto injection bottle of shape pipe, it is simple to after the extract collected is injected conical pipe by sampling probe, with the automatic sampler of analytical instrument according to Loading sequence journey Sequence sample introduction is analyzed.

Concrete operation method is: a certain amount of sample and extract is injected in extraction flask 5, tightens the blind nut 1 of band sealing gasket 2, manual or loading Automatically oscillation extraction on oscillation extraction device, is placed on mixed liquor in centrifuge centrifugal, makes extract separate with sample.Now, density is bigger than water Extract (such as dichloromethane) can be gathered in cone-shaped collection 6 groove bottom extraction flask, use sampling probe extraction extract, be injected into band taper Auto injection (also can directly extract be injected the direct hand sampling of injection port of analytical instrument) in the auto injection bottle 10 of pipe；If extract Density is less than water, and extract can be dispersed in the top of sample, adds a certain amount of blank water, makes liquid level close to extraction bottleneck, uses extract to collect Part, is pressed into extract in transparent glass tube 7, with sampling probe, extract takes out sample introduction analysis.

Claims (1)

1. a dispersion liquid-liquid micro-extraction external member, including extraction flask, extract collecting means and three parts of injector bottle, it is characterised in that

Bottleneck profile bottom described extraction flask is elliptical cylinder-shape or cylinder, offers cone-shaped collection groove (6)；Top offers screw socket, and joins There is the sealing gasket and blind nut mated with screw socket, be used for sealing top；

Described extract collecting means, for realizing the collection of the extractant density extract less than water, including transparent pipe (7) with handle (8) collecting hood (9), the maximum outside diameter of collecting hood (9) matches with extraction flask top bottle internal diameter, when collecting extract from extraction flask top Portion stretches into after in extraction flask can be close to bottle inwall；One end of transparent pipe (7) is fixed on handle (8)；

Described injector bottle includes bottle (10), is within it placed with conical pipe (11), by sampling probe from the extraction of extraction flask bottom collection Liquid or from extract collecting means transparent pipe (7) collect extract collection after be placed in the conical pipe of injector bottle.