CN204679483U - A kind of device of Fast Measurement semi-volatile organic matter characterization of adsorption - Google Patents
A kind of device of Fast Measurement semi-volatile organic matter characterization of adsorption Download PDFInfo
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- CN204679483U CN204679483U CN201520402417.0U CN201520402417U CN204679483U CN 204679483 U CN204679483 U CN 204679483U CN 201520402417 U CN201520402417 U CN 201520402417U CN 204679483 U CN204679483 U CN 204679483U
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Abstract
The utility model relates to a kind of device and method of Fast Measurement semi-volatile organic matter characterization of adsorption, belongs to semi-volatile organic matter physical property detection field.This device comprise two fixed heads, two pieces distribute source material, two be separated annulus and sorbing material four kinds of parts; Structure is symmetrical up and down, and sorbing material is positioned at central authorities, sorbing material be respectively from inside to outside up and down one be separated annulus, one piece distribute source and a fixed head, each parts are closely connected to form airtight Laboratory Module mutually; Separation annulus will distribute source and sorbing material separates, and builds airtight static absorption environment in annulus inside.The utility model is used to measure semi-volatile organic matter adsorption parameter partition factor K, balance is reached, without the need to measuring the SVOC concentration in air without the need to absorption by the time, meanwhile, the impact that device inwall absorption SVOC brings experimental result can be ignored.Thus, use this device, the characterization of adsorption of semi-volatile organic matter can be measured quickly and accurately.
Description
Technical field
The utility model belongs to semi-volatile organic matter physical property detection field, particularly to the measurement mechanism of semi-volatile organic matter characterization of adsorption, for testing the partition factor between semi-volatile organic matter from different sorbing material.
Background technology
Comfortable, the healthy and work efficiency of indoor air quality appreciable impact people, more and more receives the concern of people.In recent years, a large amount of semi-volatile organic matters (english abbreviation SVOC, such as plastifier, fire retardant, agrochemical) is widely used in all kinds of indoor material, and enters indoor environment by the approach such as distributing.Research shows, the adverse health effects such as SVOC Human body package and endocrine hormone are lacked of proper care, asthma in children, allergic, mankind spermatozoon vigor declines, inborn defect exist relevance.Due to extremely low saturated vapor pressure, SVOC easily by various surface (as furniture, clothes, wall etc.) absorption, and is passed to skin surface when human body and these surface contact, form Human body package.Therefore, develop a kind of fast, Measurement accuracy SVOC at the device of the characterization of adsorption of different surfaces, technological means can be provided for accurate evaluation SVOC Human Exposure via.According to adsorption theory, the characterization of adsorption of SVOC can be characterized by partition factor K.Partition factor K refers to absorption when reaching balance, the ratio of gas phase SVOC concentration in Adsorption Phase SVOC concentration and air; When SVOC concentration one timing in air, in solid, the adsorbance of SVOC can be determined by partition factor K.Therefore, the K of Accurate Determining SVOC and different materials becomes the key measuring SVOC characterization of adsorption.
The device in volatile organic matter feature measurement continued to use mostly by the experimental provision of existing measurement SVOC characterization of adsorption, sorbing material to be measured is normally put into a rectangular parallelepiped or cylindrical cool compartment by the method that this kind of device uses, pass to the air-flow containing constant density SVOC, the environment of a constant SVOC concentration is built in Laboratory Module, in monitoring sorbing material, SVOC adsorbance over time, and by theoretical formula, nonlinear fitting is carried out to it, thus determine partition factor K.Because cool compartment has very large internal surface area, and SVOC is easy to by various adsorption, therefore before sorbing material is put into Laboratory Module, Laboratory Module inside surface and SVOC is needed to reach adsorption equilibrium, otherwise SVOC concentration cannot keep constant in Laboratory Module, and to be generally several days even longer this time, add test period and cost.This kind of device is used only to be suitable for the very weak volatile organic matter of adsorbability.In addition, use existing apparatus to need to measure air mass flow and the gas phase SVOC concentration of turnover cludy, increase the complicacy of experiment; And typically, gas phase SVOC concentration is very low, measuring error is large, reduces the accuracy of test result.In addition, in existing apparatus, due to the gas velocity usually reason such as less, the rate of adsorption of SVOC is general less, and make SVOC in sorbing material reach the chronic of adsorption equilibrium, the time cost of test is very high.
Utility model content
The purpose of this utility model is the weak point in order to overcome existing apparatus, proposes a kind of device of Fast Measurement semi-volatile organic matter characterization of adsorption.The utility model adopts airtight cludy, and without the need to measurement gas flow and gas phase SVOC concentration, structure is simple, easy to operate, stablizes adjustable test condition for the partition factor K measuring SVOC and different materials provides; Experimental period shortens greatly, and has higher accuracy.
The utility model solves the technical scheme that its technical matters adopts:
A device for Fast Measurement semi-volatile organic matter characterization of adsorption, is characterized in that, this device comprise two fixed heads, two pieces distribute source material, two be separated annulus and sorbing material four kinds of parts; Structure is symmetrical up and down, and sorbing material is positioned at central authorities, sorbing material be respectively from inside to outside up and down one be separated annulus, one piece distribute source and a fixed head, each parts are closely connected to form airtight Laboratory Module mutually; Separation annulus will distribute source and sorbing material separates, and builds airtight static absorption environment in annulus inside; Distribute source to distribute area equal with the adsorption area of sorbing material, be separated the thickness of annulus and the ratio <0.025 of internal diameter, to guarantee distributing the adsorption area of area or sorbing material and being separated the surface area ratio >10 of circle ring inner wall of the source of distributing.
After this device has been assembled, be placed in constant-temperature constant-humidity environment, ensure that the humiture of whole test process is consistent.This device can make SVOC when not by surperficial to sorbing material by distributing surface, source free diffusing when the interference of external air flow condition, is then adsorbed onto material surface.After a period of time of setting, device for opening, takes out sorbing material, analyzes the adsorbance of SVOC in sorbing material.By measuring adsorbance corresponding to different adsorption time, and by theoretical formula, nonlinear fitting being carried out to it, partition factor K can be determined.Namely partition factor K has reacted the characterization of adsorption of sorbing material to SVOC, and K value is larger, and the adsorptive power of material is larger; K value is less, and the adsorptive power of material is less.
The beneficial effects of the utility model are, 1) adopt airtight experiment cludy, and without the need to measuring gas phase SVOC concentration, the complicacy of experimental system can be lowered, and the error that measurement phase concentrations is introduced can be avoided; 2) the separation thickness of annulus and the rate of adsorption of SVOC are inversely proportional to, and select less thickness can accelerate the rate of adsorption of SVOC, shorten test period; 3) separation annular radii is large, thickness is little, and the SVOC adsorbance of inwall can be left in the basket; 4) need not adsorption equilibrium be reached, only need carry out matching by absorption data in earlier stage and get final product (but needing the rate of adsorption of SVOC to be obvious sluggish trend), greatly can shorten test period; 5) structure is simply small and exquisite, can repeatedly reuse.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of a kind of Fast Measurement semi-volatile organic matter characterization of adsorption of the present utility model;
Embodiment
Below in conjunction with the drawings and specific embodiments, the technical solution of the utility model is described in detail.
The device example structure schematic diagram of the mensuration semi-volatile organic matter characterization of adsorption that the utility model proposes, as shown in Figure 1.Whole device is flat right cylinder.This device comprises sorbing material 1, is positioned at the central authorities of whole device, and the Homogeneous Circular flat board (diameter 10cm) can made for all kinds of sorbing material, as individual layer clothes, glass, concrete, paper etc.; Be separated annulus 2, totally two, diameter is thickness little (external diameter 10cm, internal diameter 8cm, thickness 2mm) greatly, is made up, is placed in the both sides up and down of sorbing material respectively of the hard material not containing SVOC; Distribute source 3 (being cut into the circle of diameter 10cm), can be all kinds of indoor materials containing different SVOC, as the vinyl floor, wallpaper etc. of plasticizer-containing, totally two pieces, respectively be placed in the opposite side being separated annulus, SVOC is by distributing surface, source by free diffusing to sorbing material surface; Fixed head 4 (diameter 10cm), totally two pieces, the material higher by levelness is made (such as stainless steel, glass fibre etc.), one piece of fixed head is respectively placed in the outside that two panels distributes source material, pressure is applied outside fixed head, the each several part of device is closely connected, and makes the cavity of separation annulus inside form the cavity of relative closure, intercept external air flow to the impact of air in cavity.
Adopt the assay method of the utility model device for adopting passive adsorption mode, after SVOC distributes from the source surface of distributing, free diffusing in the air being separated annulus 2 inside, finally diffuses to sorbing material surface, is adsorbed in sorbing material 1.When the inwall SVOC adsorbance being separated annulus 2 can be ignored, the CONCENTRATION DISTRIBUTION that SVOC is being separated annulus internal cavities can be considered that one-dimensional linear distributes, can Mass Transfer Model be set up accordingly and derive theoretical formula, by this theoretical formula, nonlinear fitting is carried out to test result, namely obtain the value of partition factor K.The size of K value has directly reacted the absorption property of sorbing material to SVOC, and K value is larger, and adsorptive power is stronger; K value is less, then adsorptive power is more weak.
Assay method of the present utility model comprises the following steps:
1) assemble several identical said apparatus (quantity of proving installation has met the quantity required for whole assay method as proving installation simultaneously, be generally 15 ~ 20), be placed in constant-temperature constant-humidity environment at once after device assembles;
2) (1 day is generally through the sample time of setting, also can adjust according to actual conditions) after from constant-temperature constant-humidity environment take out 2 ~ 3 proving installations, sorbing material is taken out again from each proving installation, adopt the adsorbance of SVOC in the methods analyst sorbing material of extraction, (this process is called sampling process to complete the sampling of the adsorbance of SVOC in a sorbing material, getting 2 ~ 3 devices is to provide parallel sample, the stability with validation test method); The concrete operations of extraction are:
2.1) if sorbing material is the Foldable material such as clothes, paper, directly sorbing material is put into apparatus,Soxhlet's; Can comminution of material if sorbing material is concrete etc., put into apparatus,Soxhlet's again with the gauze parcel containing SVOC after can being pulverized; If sorbing material is the hard material such as stainless steel, glass, then need, with gauze its absorption surface of wiping being repeatedly soaked with methylene chloride, the SVOC of sorbing material adsorption to be transferred in gauze, then gauze is put into apparatus,Soxhlet's;
2.2) in apparatus,Soxhlet's, add 60 ~ 100mL methylene chloride, at 70 DEG C, extract 6 ~ 12 hours, the SVOC in sorbing material (or gauze) is separated in dichloromethane solution; Or be extracted liquid by ultrasonic extraction method;
2.3) with Rotary Evaporators concentrated extract to 0.5 ~ 25mL, 100 μ L concentrates are got as sample in chromatography column feed materials bottle; Start gas chromatograph, analyze SVOC concentration in this sample; SVOC concentration in this sample is multiplied by the volume of concentrate, namely (the concentrated final volume of extraction solution is determined on a case-by-case basis to obtain the adsorbance of SVOC in this sorbing material, the concentration of SVOC in concentrate need be within the scope of the graticule of gas chromatograph, often kind of SVOC uses the method possibility of chromatographic different, can consult reference books);
3) step 2 is repeated); By that analogy, altogether step 2 is repeated) complete 4 ~ 5 sub-samplings, (also namely altogether completing 5 ~ 6 sub-sampling processes);
4) to step 2) and 3) adsorbance of SVOC carries out initial analysis in the different time sorbing material that records, takes following three kinds of situations to process further:
4.1) if the adsorbance of SVOC is not substantially with change sample time (showing that the adsorption process of SVOC reached within 1 day (or being tending towards) to balance), then is shortened to 1/20 ~ 1/10 (being generally set to 1 ~ 2 hour) of previous sample time sample time, repeats step 1) ~ step 3);
4.2) if the adsorbance of SVOC increases with sample time and increases, but the rising tendency of SVOC adsorbance has been considerably slower than the rising tendency of sample time, and (such as sample time increases by 2 times, and adsorbance only increases 1 times), then terminate sampling, enter step 5);
4.3) if the adsorbance of SVOC is with being linear increase (showing that the characterization of adsorption of this type of SVOC is very strong) sample time, then sample time is lengthened 5 ~ 10 times (being generally set to 5 ~ 10 days) for the previous sample time, repeats step 1) ~ step 3);
5) by theoretical formula, nonlinear fitting is carried out to test result (sorbing material is in adsorbance corresponding to different adsorption time), obtain partition factor K (nonlinear fitting can complete with Software tools such as Origin, 1stOpt, Matlab); Two kinds are had according to the theoretical formula that different situations nonlinear fitting uses:
5.1) if sorbing material impermeable (such as stainless steel, glass etc., also namely SVOC only can be enriched in sorbing material surface), the theoretical formula of employing is: M=2Ky
0a
solve partition factor K
1; Wherein, M is the adsorbance of SVOC on sorbing material, is obtained by experiment; K
1be partition factor, unit is m; y
0be the concentration of SVOC in sorbing material superficial air layer, SVOC distributed to the y in source
0usually constant can be thought; A is that the adsorption surface area of sorbing material side (notes it not being sorbing material surface area, for device embodiment A=π * 4
2cm
2); L is the diffusion length (being the thickness being separated annulus in this device) of SVOC; D
abe the coefficient of diffusion of SVOCs in air, to all kinds of SVOC, it can be calculated by experimental formula; (in theoretical formula, only parameter K and y
0the unknown, other parameters are known.Therefore, only need experimentally data to carry out matching, unknown parameter K and y can be solved
0)
5.2) if sorbing material is to SVOC permeable (such as clothes, paper, concrete etc.), when not considering sorbing material internal divergence, the theoretical formula of employing is: M=2Ky
0ad
solve partition factor K
2; Wherein, d is the half of sorbing material thickness; K
2being partition factor, is dimensionless group; Meaning and the situation 1 of all the other parameters) the same.
The used device of said method, after being cleaned by the SVOC be separated above annulus, can be used for testing next time, realizes constantly reusing with solvent (as methylene chloride).
Claims (1)
1. a device for Fast Measurement semi-volatile organic matter characterization of adsorption, is characterized in that, this device comprise two fixed heads, two pieces distribute source material, two be separated annulus and sorbing material four kinds of parts; Structure is symmetrical up and down, and sorbing material is positioned at central authorities, sorbing material be respectively from inside to outside up and down one be separated annulus, one piece distribute source and a fixed head, each parts are closely connected to form airtight Laboratory Module mutually; Separation annulus will distribute source and sorbing material separates, and builds airtight static absorption environment in annulus inside; Distribute source to distribute area equal with the adsorption area of sorbing material, be separated the thickness of annulus and the ratio <0.025 of internal diameter, to guarantee distributing the adsorption area of area or sorbing material and being separated the surface area ratio >10 of circle ring inner wall of the source of distributing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104914218A (en) * | 2015-06-11 | 2015-09-16 | 清华大学 | Device and method for rapidly determining adsorption property of semi-volatility organic matters |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104914218A (en) * | 2015-06-11 | 2015-09-16 | 清华大学 | Device and method for rapidly determining adsorption property of semi-volatility organic matters |
| CN104914218B (en) * | 2015-06-11 | 2018-02-02 | 清华大学 | A kind of device and assay method of quick measure semi-volatile organic matter characterization of adsorption |
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