CN105498290A - Separation device for polycyclic aromatic hydrocarbon solid-liquid suspension system and separation method - Google Patents
Separation device for polycyclic aromatic hydrocarbon solid-liquid suspension system and separation method Download PDFInfo
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- CN105498290A CN105498290A CN201510973551.0A CN201510973551A CN105498290A CN 105498290 A CN105498290 A CN 105498290A CN 201510973551 A CN201510973551 A CN 201510973551A CN 105498290 A CN105498290 A CN 105498290A
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- aromatic hydrocarbon
- polycyclic aromatic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
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Abstract
The invention discloses a separation device for a polycyclic aromatic hydrocarbon solid-liquid suspension system. The separation device comprises a syringe and a filter head, wherein the filter head is arranged at the front end of an inlet and outlet port of the syringe, and the syringe and the filter head are connected detachably; the filter head comprises a casing made of polypropylene and a filter membrane made of glass fibers; the pore diameter of the filter membrane is 0.45 mu m, and an effective filter area of the filter membrane is 3.5-4.0 cm<2>. The separation method adopting the separation device mainly comprises the following steps: a, suspension extraction; b, assembly of the separation device; c, wetting of the filter head; d, solid-liquid separation. The separation device and the separation method have the advantages of simple operation, high separation efficiency, good separation effect, high precision of follow-up analysis and determination, and the like.
Description
Technical field
The present invention relates to a kind of equipment for separating liquid from solid and method, more specifically to a kind of separator and separation method of polycyclic aromatic hydrocarbon solid-liquid suspension system.
Background technology
Along with deepening continuously of scientific research, solid-liquid separation technique is more and more important, common method, as centrifugal and standing etc.But, in some solid-liquid suspension systems (being hereafter referred to as suspension system), because the particularity of reaction vessels can not process by high speed centrifugation method, or because in system, solid matter mass is lighter, be difficult to be issued to Separation of Solid and Liquid in the centrifugal and standing method of routine, thus make the compartment analysis of liquid phase in this system be difficult to realize.
Most of polycyclic aromatic hydrocarbon solid-liquid system, Separation of Solid and Liquid can be made with leaving standstill with centrifugal, but wherein some polycyclic aromatic hydrocarbon solid-liquid system, because solid matter mass is uneven, such as charcoal, has and floats over liquid phase top layer, there is the portion of floating on a liquid, also have and be deposited in liquid phase lower floor, what system was slight rock will become more muddy, and therefore conventional method is inapplicable to the compartment analysis of polycyclic aromatic hydrocarbon in this type of suspension system.To the liquid phase analysis of this system, previously relevant research is all adopt add-on third party adsorbent, such as Tenaxbeads etc. substantially, polycyclic aromatic hydrocarbon in absorption liquid phase, then take out the solid matter through rinsing top layer, Solvent Extract methods, rotary evaporation concentrates, and last constant volume measures.The separation method operating difficulties of this kind of polycyclic aromatic hydrocarbon solid-liquid suspension system, and step is more, especially concerning the strong polycyclic aromatic hydrocarbon of hydrophobicity, as easy as rolling off a log loss in operation, the concentration in original system cannot be measured accurately, the operation of a large amount of samples is taken time and effort simultaneously.
Summary of the invention
In order to make up the deficiencies in the prior art, the object of the invention is to provide a kind of device and separation method of Separation of Solid and Liquid, is mainly used in suspension system, the compartment analysis of polycyclic aromatic hydrocarbon.
The technical scheme that technical solution problem of the present invention adopts is: a kind of separator of polycyclic aromatic hydrocarbon solid-liquid suspension system, described separator comprises Syringe injector and filtering head, described filtering head is located at the front end of the import and export of described Syringe injector, is detachable connection between described Syringe injector and filtering head; Described filtering head is made up of shell and filter membrane, and the material of described shell is polypropylene, and the material of described filter membrane is glass fibre; The aperture of described filter membrane is 0.45 μm, and the effective filtration area of described filter membrane is 3.5 ~ 4.0cm
2.
Further, described glass fibre filter membrane forms primarily of inorfil mineral wool.For the filtering head of water system, the hydrophily due to its filter membrane causes the polycyclic aromatic hydrocarbon dissolved in the liquid phase to stick on filter membrane thus the polycyclic aromatic hydrocarbon of easy loss part; And the filter membrane of glass fibre material has natural hydrophobicity due to it, therefore its effect is better.
A separation method for polycyclic aromatic hydrocarbon solid-liquid suspension system separator, described separation method mainly comprises the following steps:
A. suspension extracts: use Syringe injector to be suspended by polycyclic aromatic hydrocarbon solid-liquid extracting at the uniform velocity, should avoid the air being extracted into liquid level upper strata in extraction process; Because a large amount of air can make dissolving polycyclic aromatic hydrocarbon in the liquid phase a large amount of stick in syringe, follow-up at the uniform velocity filter process can be affected simultaneously;
B. separator assembling: the import and export of filtering head with Syringe injector front end are connected, composition separator;
C. filtering head soaks: be expelled to slowly in filtering head by the polycyclic aromatic hydrocarbon suspension solid-liquid extracted in Syringe injector, makes the filter membrane in liquid phase and filtering head soak 5 ~ 10 seconds; In whole separation process, wetting very crucial, test result shows that the liquid concentration impact whether soaked filtering is very large;
D. Separation of Solid and Liquid: at the uniform velocity the polycyclic aromatic hydrocarbon suspended sample in Syringe injector is injected through filtering head, completes separation, is further analyzed mensuration by the polycyclic aromatic hydrocarbon liquid phase after being separated.
In described step c, the wetting time of filtering head is preferably 5 seconds, and the polycyclic aromatic hydrocarbon suspended sample volume for wetting filtering head is about 2mL.
The invention has the beneficial effects as follows: compared with prior art, glass fibre filter membrane is used in the compartment analysis of polycyclic aromatic hydrocarbon solid-liquid suspension system by the present invention first; Adopt filtering head and syringe composition filtration system, provide very practical and technical support accurately to the compartment analysis of polycyclic aromatic hydrocarbon in suspension system; This separation method is simple to operate, separative efficiency is high, good separating effect, and for the polycyclic aromatic hydrocarbon that hydrophobicity is strong, the loss that separation process causes is very little, improves the accuracy that subsequent analysis measures.
Accompanying drawing explanation
Fig. 1 be different filter membrane material filtering head on after filtering in filtrate polycyclic aromatic hydrocarbon concentration affect result.
Fig. 2 is the adsorption isotherm of Phenanthrene when different condition filtration system.
Fig. 3 is the adsorption isotherm of polycyclic aromatic hydrocarbon pyrene when different condition filtration system.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, illustrate the present invention further, following detailed description of the invention should be understood and be only not used in for illustration of the present invention and limit the scope of the invention.
Embodiment
A separator for polycyclic aromatic hydrocarbon solid-liquid suspension system, described separator comprises Syringe injector and filtering head, and described filtering head is located at the front end of the import and export of described Syringe injector, is detachable connection between described Syringe injector and filtering head; Described filtering head is made up of shell and filter membrane, and the material of described shell is polypropylene; The filter membrane material of described filtering head is glass fibre, and described glass fibre filter membrane forms primarily of inorfil mineral wool.The filtering head that have studied different filter membrane material in the present embodiment affects situation to the concentration of polycyclic aromatic hydrocarbon in filtrate after filtering, and concrete outcome is shown in Fig. 1.For the filtering head of water system, the hydrophily due to its filter membrane causes the polycyclic aromatic hydrocarbon dissolved in the liquid phase to stick on filter membrane thus the polycyclic aromatic hydrocarbon of easy loss part; And the filter membrane of glass fibre material has natural hydrophobicity due to it, therefore its effect is better.The aperture of described filter membrane is 0.45 μm; The effective filtration area of described filter membrane is 3.5 ~ 4.0cm
2, be preferably 3.8cm
2.
A separation method for polycyclic aromatic hydrocarbon solid-liquid suspension system separator, described separation method mainly comprises the following steps:
A. suspension extracts: use Syringe injector by suspension solid-liquid extracting at the uniform velocity, should avoid the air being extracted into liquid level upper strata in extraction process; Because a large amount of air can make dissolving polycyclic aromatic hydrocarbon in the liquid phase a large amount of stick in syringe, follow-up at the uniform velocity filter process can be affected simultaneously;
B. separator assembling: the import and export of filtering head with Syringe injector front end are connected, composition separator;
C. filtering head soaks: be expelled to slowly in filtering head by the suspension solid-liquid extracted in Syringe injector, 2mL sample was injected through filtering head in 2 seconds, after this treats more than the glass fiber filter wetting 3 seconds again (altogether 5 seconds) in liquid phase and filtering head; In whole separation process, wetting very crucial, test result shows that the liquid concentration impact whether soaked filtering is very large;
D. Separation of Solid and Liquid: after having soaked, more at the uniform velocity the suspended sample in Syringe injector is injected through filtering head, complete separation, the polycyclic aromatic hydrocarbon liquid phase after being separated is measured by high performance liquid chromatograph.
The result of mensuration is converted into the concentration (such as, the adsorption isotherm of luxuriant and rich with fragrance, pyrene, concrete outcome is shown in Fig. 2 and Fig. 3) of liquid phase in original suspension system by the adsorption isotherm that filtration system measures.Known from analytical test result, the number of rings of polycyclic aromatic hydrocarbon is more, and the adsorbance of filtration system can increase, and this becomes certain ratio with the hydrophobicity of polycyclic aromatic hydrocarbon.
Specific nature and the parameter of the separator that the present invention adopts and separation method see the following form 1.
The relevant parameter of polycyclic aromatic hydrocarbon filtration system in table 1. suspension system
| Systematic parameter | Character and numerical value |
| Syringe | 10mL, polyvinyl chloride |
| Filtering head shell | Polypropylene |
| The composition of glass fibre filter membrane | Inorfil mineral wool |
| The area (mm) of filter membrane | 25 |
| Effective filtration area (cm 2） | 3.8 |
| The aperture (μm) of filter membrane | 0.45 |
| Solution temperature (DEG C) | 22 |
| PH value of solution | 7 |
| The volume (ml) of solution | 4 |
| Filter membrane soaks volume (ml) | 2 |
| Wetting time (second) | ≥5 |
Above embodiment is only for illustration of the present invention; and be not limitation of the present invention; the those of ordinary skill of relevant technical field; without departing from the spirit and scope of the present invention; can also make a variety of changes and modification; therefore all equivalent technical schemes also belong to category of the present invention, and scope of patent protection of the present invention should be defined by the claims.
Claims (4)
1. the separator of a polycyclic aromatic hydrocarbon solid-liquid suspension system, it is characterized in that: described separator comprises Syringe injector and filtering head, described filtering head is located at the front end of the import and export of described Syringe injector, is detachable connection between described Syringe injector and filtering head; Described filtering head is made up of shell and filter membrane, and the material of described shell is polypropylene, and the material of described filter membrane is glass fibre; The aperture of described filter membrane is 0.45 μm, and the effective filtration area of described filter membrane is 3.5 ~ 4.0cm
2.
2. the separator of a kind of polycyclic aromatic hydrocarbon solid-liquid suspension system according to claim 1, is characterized in that: described glass fibre filter membrane forms primarily of inorfil mineral wool.
3. a separation method for polycyclic aromatic hydrocarbon solid-liquid suspension system separator according to claim 1 and 2, it is characterized in that, described separation method mainly comprises the following steps:
A. suspension extracts: use Syringe injector to be suspended by polycyclic aromatic hydrocarbon solid-liquid extracting at the uniform velocity, should avoid the air being extracted into liquid level upper strata in extraction process;
B. separator assembling: the import and export of filtering head with Syringe injector front end are connected, composition separator;
C. filtering head soaks: be expelled to slowly in filtering head by the polycyclic aromatic hydrocarbon suspension solid-liquid extracted in Syringe injector, makes the filter membrane in liquid phase and filtering head soak 5 ~ 10 seconds;
D. Separation of Solid and Liquid: at the uniform velocity the polycyclic aromatic hydrocarbon suspended sample in Syringe injector is injected through filtering head, completes separation, is further analyzed mensuration by the polycyclic aromatic hydrocarbon liquid phase after being separated.
4. the separation method of polycyclic aromatic hydrocarbon solid-liquid suspension system separator according to claim 3, it is characterized in that: in described step c, the wetting time of filtering head is preferably 5 seconds, and the polycyclic aromatic hydrocarbon suspended sample volume for wetting filtering head is about 2mL.
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| CN203178126U (en) * | 2012-11-13 | 2013-09-04 | 中国农业科学院农业质量标准与检测技术研究所 | Multifunctional pin type filter |
| CN203324075U (en) * | 2013-06-19 | 2013-12-04 | 中国科学院新疆生态与地理研究所 | Activated carbon filtration purification device |
| CN103464103A (en) * | 2013-09-22 | 2013-12-25 | 南京农业大学 | Thermal cracking carbon for removing polycyclic aromatic hydrocarbon in water as well as preparation method and application thereof |
| CN103789399A (en) * | 2014-01-27 | 2014-05-14 | 南昌大学 | Rapid micro algae fluid trace solid-liquid separation method |
| CN103977766A (en) * | 2014-05-27 | 2014-08-13 | 南京大学 | Sulfydryl-amidogen modified mesoporous silicon material as well as preparation method and application thereof |
| CN104215497A (en) * | 2014-09-19 | 2014-12-17 | 山东省科学院海洋仪器仪表研究所 | Experimental device and method for extracting polycyclic aromatic hydrocarbons in enriched seawater |
| CN204439430U (en) * | 2015-01-19 | 2015-07-01 | 天津出入境检验检疫局动植物与食品检测中心 | A kind of for oil fatty acid esterification pretreating device |
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2015
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| CN203178126U (en) * | 2012-11-13 | 2013-09-04 | 中国农业科学院农业质量标准与检测技术研究所 | Multifunctional pin type filter |
| CN203324075U (en) * | 2013-06-19 | 2013-12-04 | 中国科学院新疆生态与地理研究所 | Activated carbon filtration purification device |
| CN103464103A (en) * | 2013-09-22 | 2013-12-25 | 南京农业大学 | Thermal cracking carbon for removing polycyclic aromatic hydrocarbon in water as well as preparation method and application thereof |
| CN103789399A (en) * | 2014-01-27 | 2014-05-14 | 南昌大学 | Rapid micro algae fluid trace solid-liquid separation method |
| CN103977766A (en) * | 2014-05-27 | 2014-08-13 | 南京大学 | Sulfydryl-amidogen modified mesoporous silicon material as well as preparation method and application thereof |
| CN104215497A (en) * | 2014-09-19 | 2014-12-17 | 山东省科学院海洋仪器仪表研究所 | Experimental device and method for extracting polycyclic aromatic hydrocarbons in enriched seawater |
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