CN103674624A - Sampling membrane and sampler capable of enriching heavy metals in ambient air and application method of sampler - Google Patents
Sampling membrane and sampler capable of enriching heavy metals in ambient air and application method of sampler Download PDFInfo
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Abstract
The invention discloses a sampling membrane and a sampler capable of enriching heavy metals in ambient air and an application method of the sampler. The sampling membrane comprises a nanometer fiber membrane and an air-permeable supporting padding arranged below the nanometer fiber membrane. The sampler comprises the sampling membrane and a sampling clamp; the sampling clamp is composed of an upper cone and a lower cylinder, wherein the upper surface of the cone is horizontal, the cylinder is composed of an upper cylinder and a rotary lower cylinder, the side surfaces of the upper cylinder and the lower cylinder are provided with uniformly distributed vertical ridges, the vertical ridges on the upper cylinder and the lower cylinder are aligned by rotating the lower cylinder, so fixation of the sampling membrane on the horizontal surface of the sampling clamp is realized. After heavy metals in air are acquired by using the sampler, a filter membrane is taken out and put into a centrifuge tube filled with a buffer solution, a solution is used for desorption of the heavy metals on the filter membrane, and after desorption, the solution is determined. According to the invention, detection sensitivity can be substantially improved, pre-treatment of a sample is easy and feasible, and nanometer fiber filter membranes with different functions are used for different detection objects, thereby improving absorption and acquisition efficiency.
Description
Technical field
The present invention relates to atmosphere environment supervision technical field, particularly relate to sampling thief and the application process thereof of heavy metal in a kind of enrichment environment air.
Background technology
Haze weather is serious in recent years, the aerocolloidal fine particle thing of air PM10, PM2.5 are easy to toxic heavy metal in enriched air, acidic oxide, organic contaminant, bacterium and virus etc., this fine grained gasoloid can be attached to respiratory tract, even enter pulmonary deposition, health hazard to human body is very big, therefore, to aerocolloidal sanitary inspection, be the pith of air pollution monitoring.Especially some heavy metal element, as lead, it exists general and harm is larger, but conventionally lower at the content of residential district, be difficult for detecting, in order to improve detection sensitivity, sampling time that need to be very long, time and effort consuming.
The aerocolloidal method of sampling mainly contains electrostatic precipitation method, impinger method and filtrate method.Electrostatic precipitation method sample rate is fast, and sampling efficiency is high, but when the on-the-spot gas that has an explosive, steam or dust, can not use this method of sampling.During impinger sampling, affect the many factors of collecting efficiency, need to carry out the checking of gas production efficiency and impermeability and detect before use, complex steps, should not be used.The advantages such as little, lightweight, easy to store, easy to carry and holding time of volume that filtrate sampling method has filtrate is long, have been widely used in gathering airborne particulate form pollutant.
Conventional filtrate has quantitative filter paper, glass fiber filter paper, organic synthetic fibers filtrate, miillpore filter and dipping reagent filtrate.The ash content of quantitative filter paper is low, and physical strength is high, unsuitable damaged, and heat-resisting (150 ℃) are cheap, but because filter paper fibre is thicker, space is less, so aeration resistance is large, and the aerosol particle gathering can enter into filter paper inside, resolves more difficult.Glass fiber filter paper is insoluble to acid, water and organic solvent, after sampling, available water, organic solvent and rare nitric acid etc. extract test substance, its shortcoming is that metal blank value is higher, machinery is poor by force, when solution extracts, easily become pasty state, need to filter, if glass fibre will be cleared up, need to be with hydrofluorite or pyrophosphoric acid; Quartz glass fibre filter paper has overcome the high shortcoming of blank value, but expensive.Polyvinyl chloride filter membrane is thermo-labile, and maximum operation (service) temperature is 55 ℃, and during the rear sample preparation of sampling, heating can occur curling, and possible enwrapped granule thing, due to easily generation vigorous oxidation burning, causes sample loss, can not clear up sample with perchloric acid.The porous organic film that cellulose acetate is made into, because its ash content is low, physical strength is good, easy to digest and blank value is lower, cost is not high, is now commonly used, in national standard method, adopt this filter membrane sampling, but the bioaccumulation efficiency of itself is limited, makes recall rate not high.
Summary of the invention
The technical matters that the present invention mainly solves is to provide sampling film, sampling thief and the application process thereof of heavy metal in a kind of enrichment environment air, can solve in the existing method of sampling exists gas production resistance large, physical strength is low, blank value high and sampling after determinand be difficult to the difficult problems such as wash-out extraction.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the sampling film that heavy metal in a kind of enrichment environment air is provided, described sampling film is functional nano-fiber filter membrane, comprising: diaphragm and support bedding and padding, and described support bedding and padding lining is below described diaphragm; Described diaphragm is nano fibrous membrane; Described support bedding and padding are gas penetration potential filter material.
For solving the problems of the technologies described above, another technical solution used in the present invention is: the preparation method of the sampling film of heavy metal in a kind of enrichment environment air is provided, comprises the following steps:
(1) high molecular polymer is dissolved in suitable solvent, stirs and to be made into spinning liquid, then to adding in described spinning liquid complexing agent with respect to polymer quality 3～8% as functional modifier, and regulate the pH value of spinning liquid;
(2) utilize electrostatic spinning technique that the spinning liquid of preparation in step (1) is made to nano fibrous membrane material, then described nano fibrous membrane material is cut into diaphragm, lining is usingd filter material as supporting bedding and padding, and combination system makes filter membrane, obtains the sampling film of heavy metal in enrichment environment air.
In a preferred embodiment of the present invention, in described step (1), described high molecular polymer is at least one in polyphenylene sulfide, cellulose acetate, polystyrene, polycaprolactam, acryl resin and polyacrylonitrile.
In a preferred embodiment of the present invention, in described step (1), described solvent is at least one in DMF, tetrahydrofuran, ethanol, acetone, formic acid, water, halogenated hydrocarbons and aromatic hydrocarbon.
In a preferred embodiment of the present invention, in described step (1), described complexing agent is at least one in phenanthroline, zincon, oxine, dithizone, 1-(2-pyridylazo)-beta naphthal, xylenol orange or cupferron.
For solving the problems of the technologies described above, another technical solution used in the present invention is: the sampling thief that heavy metal in a kind of enrichment environment air is provided, comprise sampling film as claimed in claim 1 and sampling folder, it is upper fixing that described sampling film is placed on sampling folder, described sampling folder divides right cylinder to form by top cyclotomy cone and bottom, the upper surface level of described cone, described right cylinder is divided into cylinder and rotatable lower cylinder, the side surface of described upper and lower cylinder is with equally distributed perpendicular stupefied, by rotating lower cylinder, make the perpendicular stupefied alignment of upper and lower cylinder, realize sampling film fixing on the horizontal surface of sampling folder.
For solving the problems of the technologies described above, another technical solution used in the present invention is: the application process that the sampling thief of heavy metal in a kind of enrichment environment air is provided, concrete grammar is: sampled point is chosen in the region in needs monitoring, sampling thief claimed in claim 8 is arranged on sampling instrument, according to required sampling volume setting-up time and sample rate, open sampling instrument and bleed; When air passes filter membrane, aerosol particle thing is directly stopped by filter membrane, and is adsorbed on filter membrane under the effect of inertial settling, diffusion sedimentation, electrostatic attraction and chemical bonding; After sampling finishes, take off filter membrane and put into centrifuge tube, add the vibration of acetic acid-potassium acetate damping fluid or sonic oscillation, discard filter membrane, solution is injected to detecting instrument and carry out analyzing and testing.
In a preferred embodiment of the present invention, the concussion time that described sampling film is placed in damping fluid is 30min.
The invention has the beneficial effects as follows: the enrichment material that in a kind of enrichment environment air of the present invention, the sampling film of heavy metal and sampling thief can be applicable according to the different choice of object to be detected, in conjunction with applicable sample-pretreating method, reach the object of efficiently concentrating, fast resolving object, raising detection sensitivity.
Compared with prior art, concrete advantage of the present invention is as follows:
(1) in enrichment environment air of the present invention, the gas production resistance of the sampling film of heavy metal is little, lightweight, and blank value is low.
(2) in enrichment environment air of the present invention, the preparation method of the sampling film of heavy metal is easy, and applicability is strong, can be according to the object that will trap composition and the formula of feed change accordingly, and preparation facilities is simple.
(3) in enrichment environment air of the present invention, the sampling thief of heavy metal can carry out Concentration Sampling to the gasoloid in surrounding air, be particularly useful for the trapping of heavy metal in air particle, by short time, low discharge, take gas sample, just can reach the enrichment of efficient heavy metal contaminants, improve recall rate.
(4) because nanofiber has absorption fast to object, desorption characteristics, sample pre-treatments step can further be simplified, for example do not need to take traditional digestion method, only by the way of solution mechanical shaking extraction, just can from tunica fibrosa, under fast resolving, detect object, easy to operation, greatly reduce labour intensity and the reagent consumption of sample pre-treatments, sampling and processing time have been shortened, accuracy and the precision of detection method have been improved, it is a kind of technical method of reliable and relative high-efficiency environment friendly, monitoring to outdoor IAQ (indoor air quality) is all suitable for.
Accompanying drawing explanation
Fig. 1 is the structural representation of the sampling thief of heavy metal in a kind of enrichment environment air of the present invention;
After Fig. 2 is the lead being depicted as in national standard (GB) method and functional nano-fiber filter membrane enriched air particle, different disposal method records plumbous quality contrast schematic diagram;
In accompanying drawing, the mark of each parts is as follows: 1. functional nano fibrous membrane, 2. sampling folder.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.
Refer to Fig. 1 and Fig. 2, the embodiment of the present invention comprises:
A sampling film for heavy metal in enrichment environment air, described sampling film is functional nano-fiber filter membrane, comprising: diaphragm and support bedding and padding, described support bedding and padding lining is below described diaphragm; Described diaphragm is nano fibrous membrane; Described support bedding and padding are gas penetration potential filter material.
A preparation method for the sampling film of heavy metal in enrichment environment air, comprises the following steps:
(1) by high molecular polymer (polyphenylene sulfide, cellulose acetate, polystyrene, polycaprolactam, in acryl resin and polyacrylonitrile at least one) be dissolved in suitable solvent (N, dinethylformamide, tetrahydrofuran, ethanol, acetone, formic acid, water, at least one in halogenated hydrocarbons and aromatic hydrocarbon) in, stirring is made into spinning liquid, then in described spinning liquid, add the complexing agent (phenanthroline with respect to polymer quality 3～8%, zincon, oxine, dithizone, 1-(2-pyridylazo)-beta naphthal, at least one in xylenol orange or cupferron) as functional modifier, and regulate the pH value of spinning liquid,
(2) utilize electrostatic spinning technique that the spinning liquid of preparation in step (1) is made to nano fibrous membrane material, then described nano fibrous membrane material is cut into diaphragm, lining is usingd filter material as supporting bedding and padding, and combination system makes filter membrane, obtains the sampling film of heavy metal in enrichment environment air.
The sampling thief of heavy metal in a kind of enrichment environment air, see Fig. 1, comprise above-mentioned sampling film 1 and sampling folder 2, described sampling film 1 is placed on sampling folder 2 fixing, described sampling folder 2 divides right cylinder to form by top cyclotomy cone and bottom, the upper surface level of described cone, described right cylinder is divided into cylinder and rotatable lower cylinder, the side surface of described upper and lower cylinder is with equally distributed perpendicular stupefied, by rotating lower cylinder, make the perpendicular stupefied alignment of upper and lower cylinder, realize sampling film fixing on the horizontal surface of sampling folder.
The application process of the sampling thief of heavy metal in a kind of enrichment environment air, concrete grammar is: sampled point is chosen in the region in needs monitoring, above-mentioned sampling thief is arranged on sampling instrument, according to required sampling volume setting-up time and sample rate, opens sampling instrument and bleed; When air passes filter membrane, aerosol particle thing is directly stopped by filter membrane, and is adsorbed on filter membrane under the effect of inertial settling, diffusion sedimentation, electrostatic attraction and chemical bonding; After sampling finishes, take off filter membrane and put into centrifuge tube, add the vibration of acetic acid-potassium acetate damping fluid or sonic oscillation 30min, discard filter membrane, solution is injected to detecting instrument and carry out analyzing and testing.
Embodiment 1
Prepare dithizone functional polystyrene nanofiber (DZ-PS) filter membrane: get 10%(w/v) PS(polystyrene) be dissolved in DMF(N, dinethylformamide) and THF(tetrahydrofuran) in mixed solution (4:6), after PS dissolves completely, add 5%(w/w, quality with respect to PS) dithizone, continues by magnetic stirrer more than 10 hours.Pack glass syringe (spend the night with 1+9 nitric acid dousing, washed with de-ionized water is dried) into, syringe needle is installed, dash receiver is installed the aluminium foil being of moderate size, and covers gauze (spend the night with 1+9 nitric acid dousing, use deionized water cleaning, drying) on aluminium foil.It is 17KV that voltage is set, and flow velocity is 1.0ml/h, regulates the distance between dash receiver and syringe needle to be approximately 25cm, according to about 1ml/40cm
2(spinning liquid consumption/receiving area) carries out electrostatic spinning.The nanofiber being spun into is cut into suitable big or small thin rounded flakes, and lining is usingd the good filter material of permeability that diameter is 50mm as supporting bedding and padding, and combination system makes filter membrane, for sampling.
Filter membrane is arranged on sampling folder and makes sampling thief of the present invention, in the region of needs monitoring, choose sampled point, sampling thief is arranged on sampling instrument, open sampling instrument with the flow collection air 15min of 5L/min.In order to show validity of the present invention, with the filter membrane that PS nanofiber filter membrane and national standard method require, do control experiment simultaneously.
The filter membrane of sample will be adopted, the acetate fiber filter membrane (GB) using in polystyrene (PSDZ) the nanofiber filter membrane that dithizone is modified, PS nanofiber filter membrane, national standard method is put into centrifuge tube, adding 5mL PH is acetic acid-potassium acetate damping fluid of 4.5, vibration or ultrasonic processing 30min under room temperature.Use the same method and process blank filter membrane, prepare blank solution.Solution after resolving is injected to detecting instrument and carry out analyzing and testing, test result as shown in Figure 2.
Press the wet digestion method that national standard method is used, after the filter membrane (the acetate fiber filter membrane using in PS nanofiber filter membrane, PSDZ nanofiber filter membrane, national standard method) of adopting sample is put into polytetrafluoroethylene beaker and is cleared up with nitric acid-hydrogen peroxide, and add the nitric acid lixiviate of 5mL 1+9, leaching liquor is transferred in 50mL volumetric flask, with ultrapure water constant volume, shake up, after placement 30min, measure.Use the same method and process blank filter membrane, prepare blank solution.Test result is as Fig. 2.
Result shows: polystyrene (PS) nanofiber filter membrane, polystyrene doping dithizone (PSDZ) functional nano-fiber filter membrane are different to the bioaccumulation efficiency of heavy metal lead in air particle with the acetate fiber filter membrane using in national standard (GB) method, and also difference of the amount that adopts different sample-pretreating method stripping objects.In national standard method, using aperture is the acetate fiber filter membrane of 0.45 μ m, and because the diameter of its fiber is thicker, collecting efficiency is lower, even if take lead amount that the method for Wet records also lower than nanofiber filter membrane.The efficiently concentrating of functional nano-fiber filter membrane makes also can detect in the low area of lead content, and the method for only taking simply to add solution mechanical shaking extraction just can be easily from filter membrane stripping plumbous, greatly improved its recall rate.Air quality monitoring technical merit is significantly improved.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes instructions of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (8)
1. a sampling film for heavy metal in enrichment environment air, is characterized in that, described sampling film is functional nano-fiber filter membrane, comprising: diaphragm and support bedding and padding, and described support bedding and padding lining is below described diaphragm; Described diaphragm is nano fibrous membrane; Described support bedding and padding are gas penetration potential filter material.
2. a preparation method for the sampling film of heavy metal in enrichment environment air as claimed in claim 1, is characterized in that, comprises the following steps:
(1) high molecular polymer is dissolved in suitable solvent, stirs and to be made into spinning liquid, then to adding in described spinning liquid complexing agent with respect to polymer quality 3～8% as functional modifier, and regulate the pH value of spinning liquid;
(2) utilize electrostatic spinning technique that the spinning liquid of preparation in step (1) is made to nano fibrous membrane material, then described nano fibrous membrane material is cut into diaphragm, lining is usingd filter material as supporting bedding and padding, and combination system makes filter membrane, obtains the sampling film of heavy metal in enrichment environment air.
3. the preparation method of the sampling film of heavy metal in enrichment environment air according to claim 2, it is characterized in that, in described step (1), described high molecular polymer is at least one in polyphenylene sulfide, cellulose acetate, polystyrene, polycaprolactam, acryl resin and polyacrylonitrile.
4. the preparation method of the sampling film of heavy metal in enrichment environment air according to claim 2, it is characterized in that, in described step (1), described solvent is at least one in DMF, tetrahydrofuran, ethanol, acetone, formic acid, water, halogenated hydrocarbons and aromatic hydrocarbon.
5. the preparation method of the sampling film of heavy metal in enrichment environment air according to claim 2, it is characterized in that, in described step (1), described complexing agent is at least one in phenanthroline, zincon, oxine, dithizone, 1-(2-pyridylazo)-beta naphthal, xylenol orange or cupferron.
6. the sampling thief of heavy metal in an enrichment environment air, it is characterized in that, comprise sampling film as claimed in claim 1 and sampling folder, it is upper fixing that described sampling film is placed on sampling folder, described sampling folder divides right cylinder to form by top cyclotomy cone and bottom, the upper surface level of described cone, described right cylinder is divided into cylinder and rotatable lower cylinder, the side surface of described upper and lower cylinder is with equally distributed perpendicular stupefied, by rotating lower cylinder, make the perpendicular stupefied alignment of upper and lower cylinder, realize sampling film fixing on the horizontal surface of sampling folder.
7. the application process of the sampling thief of heavy metal in an enrichment environment air as claimed in claim 6, it is characterized in that, concrete grammar is: sampled point is chosen in the region in needs monitoring, sampling thief claimed in claim 8 is arranged on sampling instrument, according to required sampling volume setting-up time and sample rate, open sampling instrument and bleed; When air passes filter membrane, aerosol particle thing is directly stopped by filter membrane, and is adsorbed on filter membrane under the effect of inertial settling, diffusion sedimentation, electrostatic attraction and chemical bonding; After sampling finishes, take off filter membrane and put into centrifuge tube, add the vibration of acetic acid-potassium acetate damping fluid or sonic oscillation, discard filter membrane, solution is injected to detecting instrument and carry out analyzing and testing.
8. the application process of the sampling thief of heavy metal in enrichment environment air according to claim 7, is characterized in that, the concussion time that described sampling film is placed in damping fluid is 30min.
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| CN107192587A (en) * | 2017-05-04 | 2017-09-22 | 北京大学 | A kind of bioaerosol liquid phase acquisition method of portable big flow height enrichment |
| CN107907388A (en) * | 2017-12-12 | 2018-04-13 | 华南理工大学 | The device of micro dust and the method for detection grain diameter and content in a kind of collection gas |
| CN108027303A (en) * | 2015-09-22 | 2018-05-11 | 纳米制药有限公司 | Instrument and method for the fine particle dose for determining powder suction preparation |
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| CN107907388A (en) * | 2017-12-12 | 2018-04-13 | 华南理工大学 | The device of micro dust and the method for detection grain diameter and content in a kind of collection gas |
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