CN105806674A - Preparation method of acid nanoparticles for calibration - Google Patents
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- CN105806674A CN105806674A CN201610128833.5A CN201610128833A CN105806674A CN 105806674 A CN105806674 A CN 105806674A CN 201610128833 A CN201610128833 A CN 201610128833A CN 105806674 A CN105806674 A CN 105806674A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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Abstract
The invention discloses a preparation method of acid nanoparticles for calibration, relating to the field of atmospheric sampling. The preparation method comprises the steps of according to weight parts, adding 1 part of alcohol into 3-7 parts of saturated glucose solution, mixing uniformly, and atomizing to obtain atomized particles with the particle diameters of 1.2-1.5mm; introducing the atomized particles into a quartz-tube burning furnace with the temperature of 370-400 DEG C and burning for 5-15 minutes, thus obtaining carbon nanoparticles with the particle diameters of 10-200nm; diluting and drying the carbon nanoparticles to obtain carbon nanoaerosol; evaporating concentrated sulfuric acid with the concentration of 95%-99% at the temperature of 300-350 DEG C to obtain acid mist, carrying out contact on 1 part of carbon nanoaerosol and 3-7 parts of acid mist for 3-5 seconds according to the volume ratio, cooling to 15-20 DEG C, carrying out condensation, thus obtaining the acid carbon nanoparticles with the particle diameter of 20-250nm. The preparation method disclosed by the invention has the advantages that carbon nanocores with more uniform size and lower cost can be obtained, and the quantity concentration and particle-diameter distribution of the acid superfine particles in atmosphere can be accurately calibrated.
Description
Technical field
The present invention relates to atmospheric sampling field, the preparation method being specifically related to a kind of acid nanometer property granule for demarcating.
Background technology
In in air, the diameter pellet less than 0.1 micron is referred to as UFPs (ultrafine particle), UFPs accounts for the atmosphere pollution fine particle (diameter particulate matter less than 2.5 microns, PM2.5) the 90% of total mass fraction, is the primary pollutant in the surrounding air of domestic and international many big and medium-sized cities.Owing to the diameter of particulate matter is more little, its position entering respiratory tract is more deep, thus UFPs can enter human body alveolar even blood system, can cause the diseases such as cardiovascular diseases.
At present, the UFPs in air mainly through following two approach formed: a, by under high temperature discharge supersaturation gaseous state material condensation, then through collision, cohesion, absorption and formed, such as the discharge of vehicle exhaust；B, surrounding air sulphur oxide, nitrogen oxides, VOC and other compound convert through complicated heterogeneous chemical reaction and formed, such as photochemical fog, owing to vehicle exhaust and photochemical fog containing a large amount of acid chemical composition such as sulfate ions or nitrate ion, cause that the acidity of UFPs is higher.
In the past decade, epidemiological specialist begins one's study the toxicology containing acid aerosol, such as, early stage MortonLippmann in 1989 once reported on academic journal " EnvironmentalHealthPerspectives " acid aerosol and bronchitis and pulmonary function decay prevalence between be likely to there are close ties.Due to the feature that UFPs particle diameter smallest number is many, its deposition on alveolar is significantly high, can damage alveolar and mucosa, cause the chronic fibrosis of lung tissue, cause pulmonary heart disease, increase the weight of asthma, causing a series of disease such as chronic nasopharyngitis, chronic bronchitis, serious can threat to life.
Therefore, in further investigation air, the harm of health is likely to there is prior meaning than the PM10 (diameter granule less than 10 μm) and PM2.5 of research at present by UFPs especially UFPs containing acid ingredient.
But, owing to acid ultramicron mass concentration ratio in fine particle is less, detection difficulty is relatively big, at present, tests concentration and the Size of UFPs mainly through measurement and off-line analysis in real time.
But, current Real-time Measuring Technique is only used for measuring number concentration and the Size of total UFPs, it is impossible to individually for acid UFPs measurement.
Off-line analysis first by particulate collection on carrier, geomery and the chemical constituent of single particle analyzed by recycling optical instrument, however it is necessary that and collect UFPs in advance, current business-like collection device is sampled mainly by high-pressure electrostatic, and general acquisition time is shorter, can only carry out collection and the measurement of short-term UFPs concentration level, it is not suitable for the toxicologic study that research long-term chronic exposes, and the price of collection device is higher, energy consumption is relatively big, and operation easier is bigger.
At present, the supporting body that existing document is proposed by collecting particulate matter is modified the acid particles thing for distinguishing on carrier.Such as Horstman and Wagman in 1967 proposes with ferrous metal coated carrier on " AmericanIndustrialHygieneAssociationjournal " academic journal and is exposed in acid particle, by the electron microscope observation acid particle form on carrier top layer.But these are all only at the primary stage of test about the research of acid particles thing measuring method at present, and all fail to reach nanoscale, it is difficult to acid ultramicron number concentration and particle size distribution in Accurate Determining air.
Simultaneously, owing to the particle diameter of acid ultrafine particle is less, it is difficult to by conventional mode, acid ultrafine particle be demarcated, at present, existing research is by demarcating synthetic acidity ultrafine particle, compare with the testing result in air, determine concentration and the content of acid ultrafine particle in air.
At present the acid ultrafine particle of artificial preparation is mainly through first preparing solid core, then solid core is carried out outside wraps up in acid, to obtain acid ultrafine particle.Existing solid core obtains mainly through combustibility Organic substance such as acetylene, diesel oil carry out burning, or directly buy carbon granule standard bead as solid core, owing to combustion of organic matter can cause air pollution, and the solid core size heterogeneity produced, on kernel, contamination has more impurity, containing certain toxic gas, not only contaminated environment, and ratio is relatively hazardous；The price of carbon granule standard bead is higher, and experimentation cost is higher.
Summary of the invention
For the defect existed in prior art, the preparation method that it is an object of the invention to provide a kind of acid nanometer property granule for demarcating, it is possible to obtain that size is more uniform and lower-cost carbon nano inner core.
For reaching object above, the present invention adopts the technical scheme that:
The preparation method of a kind of acid nanometer property granule for demarcating, comprises the following steps:
S1, by mass parts, 1 part of ethanol is joined in 3～7 parts of saturated glucose solutions, after mix homogeneously atomization obtain the atomizing particle that particle diameter is 1.2～1.5mm；
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 370～400 DEG C and burn after 5～15min, obtain the nano carbon particle that particle diameter is 10～200nm；
S3, it is diluted drying by carbon nano-particle, obtains carbon nanometer aerosol；
S4, it is that at 300～350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 95～99% in temperature, by volume, condensing being cooled to 15～20 DEG C after 1 part of carbon nanometer aerosol and 3～7 parts of acid mist contact 3～5s, obtaining particle diameter is 20～250nm acidic carbon nano-particle.
On the basis of technique scheme, in described step S1, the speed of atomization is 2ml/min, and the time of atomization is 20～40min.
On the basis of technique scheme, in described step S2, the ignition temperature in quartz ampoule combustion furnace is 390 DEG C, and burning time is 10min.
On the basis of technique scheme, diluting the water content of dried carbon nano-particle lower than 5% in described step S3, density is 90～120g/cm3。
On the basis of technique scheme, the water content diluting dried carbon nano-particle in described step S3 is 1%, and density is 103g/cm3。
On the basis of technique scheme, in described step S4, the concentration of sulphuric acid is 98%.
On the basis of technique scheme, in described step S4, the evaporating temperature of sulphuric acid is 340 DEG C.
Compared with prior art, it is an advantage of the current invention that:
(1) preparation method being used for the acid nanometer property granule demarcated in the present invention, by being atomized by glucose solution, obtains grain diameter ratio more uniform, and the atomizing particle concentration after dry dilution is 90～120g/cm3, the atomizing particle under this condition is carried out high temperature cabonization, it is possible to obtain the nano silicon carbide granule of uniform particle diameter；Owing to glucose solution being atomized and that high temperature cabonization obtains is less costly, compared with directly buying carbon granule standard bead, it is possible to reduce experimentation cost.
(2) preparation method being used for the acid nanometer property granule demarcated in the present invention, owing to the carbonized particles exterior surface area that particle diameter is identical and concentration is relatively low is identical, and surface pore is in the same size, contact with excessive acid mist 3～5s rapidly after condensation at carbonized particles, carbonized particles can one layer of acid mist of active adsorption, form acid particle, the application is by instrument absorption detection, obtain under same particle diameter, the adsorbance of acidity nanometer granule is directly proportional to particle diameter, simultaneously, after this result is compared with existing gas chromatograph testing result, concordance is higher, illustrate that acidity nanometer granule prepared by the present invention can be used in acid ultrafine particle number concentration and particle size distribution in accurate calibration air.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
The preparation method that the embodiment of the present invention provides a kind of acid nanometer property granule for demarcating, comprises the following steps:
S1, by mass parts, 1 part of ethanol is joined in 3～7 parts of saturated glucose solutions, after mix homogeneously when speed is 2ml/min be atomized 20～40min, obtain the atomizing particle that particle diameter is 1.2～1.5mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 370～400 DEG C and burn after 5～15min, obtain the nano carbon particle that particle diameter is 10～200nm.
S3, it is diluted drying by carbon nano-particle so that carbon nano-particle forms water content lower than 5%, and density is 90～120g/cm3(optimum is 103/cm3) carbon nanometer aerosol.
S4, it is that at 300～350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 95～99% in temperature, by volume, condensing being cooled to rapidly 15～20 DEG C after 1 part of carbon nanometer aerosol and 3～7 parts of acid mist contact 3～5s, obtaining particle diameter is 20～250nm acidic carbon nano-particle.
When actually used, the addition of ethanol is added according to actual needs, and the volatility of ethanol is relatively big, and therefore, the ethanol of addition is more many, and atomization quantity is more big, and the atomizing particle size obtained is more little；Meanwhile, the temperature in combustion furnace is more high, and the particle diameter of the carbon nano-particle of generation is also more little.
Due to more uniform by the atomizing particle particle diameter ratio that obtains of mode that is atomized in the present invention, and the atomizing particle concentration after dry dilution is 90～120g/cm3, the atomizing particle under this condition is carried out high temperature cabonization, it is possible to obtain the nano silicon carbide granule of uniform particle diameter.
The carbonized particles exterior surface area that particle diameter is identical and concentration is relatively low is identical, and pore size is consistent, contacts with excessive acid mist 3～5s after condensing rapidly at carbonized particles, carbonized particles can one layer of acid mist of active adsorption, formation acid particle.
Below, by 5 embodiments, the present invention is described in detail.
Embodiment 1
By mass parts, 1 part of ethanol is joined in 3 parts of saturated glucose solutions, be atomized 40min after mix homogeneously when speed is 2ml/min, obtain the atomizing particle that particle diameter is 1.2mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 400 DEG C and burn after 15min, obtain the nano carbon particle that particle diameter is 10nm.
S3, it is diluted drying by carbon nano-particle so that it is 1% that carbon nano-particle forms water content, and density is 103g/cm3Carbon nanometer aerosol.
S4, being that at 330 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 98% in temperature, by volume, be cooled to rapidly 15 DEG C and condense after 1 part of carbon nanometer aerosol is contacted 4s with 5 parts of acid mists, obtaining particle diameter is 20nm acidic carbon nano-particle.
Embodiment 2
S1, by mass parts, 1 part of ethanol is joined in 3 parts of saturated glucose solutions, after mix homogeneously when speed is 2ml/min be atomized 20min, obtain the atomizing particle that particle diameter is 1.5mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 395 DEG C and burn after 5min, obtain the nano carbon particle that particle diameter is 50nm.
S3, it is diluted drying by carbon nano-particle so that it is 5% that carbon nano-particle forms water content, and density is 90g/cm3Carbon nanometer aerosol.
S4, being that at 350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 95% in temperature, by volume, be cooled to rapidly 20 DEG C and condense after 1 part of carbon nanometer aerosol is contacted 3s with 3 parts of acid mists, obtaining particle diameter is 70nm acidic carbon nano-particle.
Embodiment 3
S1, by mass parts, 1 part of ethanol is joined in 4 parts of saturated glucose solutions, after mix homogeneously when speed is 2ml/min be atomized 40min, obtain the atomizing particle that particle diameter is 1.2mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 385 DEG C and burn after 5min, obtain the nano carbon particle that particle diameter is 70nm.
S3, it is diluted drying by carbon nano-particle so that it is 2% that carbon nano-particle forms water content, and density is 120g/cm3Carbon nanometer aerosol.
S4, being that at 350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 99% in temperature, by volume, be cooled to rapidly 20 DEG C and condense after 1 part of carbon nanometer aerosol is contacted 5s with 7 parts of acid mists, obtaining particle diameter is 90nm acidic carbon nano-particle.
Embodiment 4
S1, by mass parts, 1 part of ethanol is joined in 5 parts of saturated glucose solutions, after mix homogeneously when speed is 2ml/min be atomized 30min, obtain the atomizing particle that particle diameter is 1.2mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 370 DEG C and burn after 5min, obtain the nano carbon particle that particle diameter is 100nm.
S3, it is diluted drying by carbon nano-particle so that it is 5% that carbon nano-particle forms water content, and density is 103g/cm3Carbon nanometer aerosol.
S4, being that at 350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 99% in temperature, by volume, be cooled to rapidly 20 DEG C and condense after 1 part of carbon nanometer aerosol is contacted 3s with 3 parts of acid mists, obtaining particle diameter is 120nm acidic carbon nano-particle.
Embodiment 5
S1, by mass parts, 1 part of ethanol is joined in 7 parts of saturated glucose solutions, after mix homogeneously when speed is 2ml/min be atomized 20min, obtain the atomizing particle that particle diameter is 1.0mm.
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 370 DEG C and burn after 3min, obtain the nano carbon particle that particle diameter is 200nm.
S3, it is diluted drying by carbon nano-particle so that it is 0.5% that carbon nano-particle forms water content, and density is 90g/cm3Carbon nanometer aerosol.
S4, being that at 300 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 95% in temperature, by volume, be cooled to rapidly 17 DEG C and condense after 1 part of carbon nanometer aerosol is contacted 5s with 7 parts of acid mists, obtaining particle diameter is 250nm acidic carbon nano-particle.
By tests below, the present invention proves that the particle diameter of acid particle has good concordance, and acid more uniform.
This device includes sampler and QCM, the sensitivity of QCM is 0.02ng, sampler is for gathering the gas with acidity nanometer granule, QCM includes the probe with crystal-vibration-chip, crystal-vibration-chip is coated with ferrum nanometer film, the thickness of ferrum nanometer film is 15～20nm, and crystal-vibration-chip is positioned at sampler.
In use, after the gas with acid particle enters sampler, ultrafine particle is deposited in the ferrum nanometer film of crystal-vibration-chip, and QCM can weigh the weight G1 of the ultrafine particle of absorption；Simultaneously; owing to acidity nanometer granule can be adhering closely in ferrum nanometer film; other ultrafine particles are only attached in ferrum nanometer film; when using inert blowing gas deferrization nanometer film, acidity nanometer granule is retained in ferrum nanometer film, and other micropartical meeting desorption; meanwhile; it is the micropartical that G2, G1-G2 are desorption that QCM weighs the weight obtained, and G2 is the weight of acidity nanometer granule.
Practical operation step is as follows:
A, it is 0.03Lmin-by speed1, passing into the gas with acidity nanometer granule to the inlet end of sampler, duration of ventilation is 4h, now, the ferrum nanometer film of described crystal-vibration-chip deposits the micropartical with acidity nanometer granule and forms fine particle film.
B, QCM weigh the weight of the acidity nanometer granule weighing in real time ferrum nanometer film surface deposition, and to record the absorption weight after having ventilated be G1.
C, ferrum nanometer film with acidity nanometer granule is placed after at least 12h combines closely to acidity nanometer granule and ferrum nanometer film, under dustless condition, use noble gas purging with the ferrum nanometer film of acidity nanometer granule, the flow velocity of noble gas is that 5～40m/s is (in the present embodiment, duration of ventilation is 15m/s, in concrete test, test site ambient As flow velocity according to different), flushing times is 5s, nonacid nano-particle comes off, obtain only with the ferrum nanometer film of acidity nanometer granule and weigh, record weight is G2, G2 is in the air passed into the quality of acidity nanometer granule.
The principle of detection and feasibility analysis:
Carry out hypothesis below: a in the present invention, acidity nanometer granule is the bead that radius is identical；The collectable the largest particles number in b, crystal-vibration-chip sensitive face and ferrum nanometer film surface is the granule number of bead close-packed arrays one layer；C, ignore the mass change that particulate matter and ferrum nanometer film generation chemical reaction cause.
Concurrently setting: particulate matter mean radius dp is 100nm, average density ρ is 2.5g/cm3, acid particles thing concentration c be 5000/cm3。
When sampling rate v is 500cm3；Sampling time t is 200min, and crystal-vibration-chip sensitive face is diametrically the circle of 0.5cm, and area s is 0.2cm2, sensitive face collecting coefficient σ is 0.1；The mass sensitivity of QCM is 0.02ng.
Then in time t, the particulate count of sensitive face trapping is Nt=σ × υ × c × t formula 1
The particulate matter quality sensing rice trapping in time t is: Mt=Nt× m=σ × υ × c × t × (4 × π × dp3 × ρ)/3 formula 2
Calculating, according to formula 2, the particulate matter quality obtaining trapping in 200 minutes is 500ng, and considerably beyond the sensitivity of QCM, the degree of accuracy that namely the method measurement obtains is higher.
And the present invention uses the mean diameter that concentrated sulphuric acid and carbon reaction generate to be in the detecting device that 20～250nm acidity nanometer granule passes into the present invention, passing into speed is 0.03Lmin-1, the time of passing into is 5min, when having passed into, QCM measures the quality m1 of the acidity nanometer granule being deposited on ferrum nanometer film surface in real time, ferrum nanometer film with acidity nanometer granule is stood under dustless condition, and use noble gas stripping postscript record current Quality mx every 2min, obtain through test, when being 15～20min between when left, weight remains stable for, namely now acidity nanometer granule compares tight with ferrum nanometer film surface combination, will not by noble gas stripping, if the time is longer, acidity nanometer granule can corrode ferrum nanometer film, cause mass loss.
Simultaneously, the present invention is by controlling concentrated sulphuric acid, ethanol, the consumption of glucose and response time, obtain variable concentrations, the acidity nanometer granule of particle diameter, the acidity nanometer granule of variable concentrations is passed in the detecting device of the present invention (concentration of deacidification property nano-particle differs, other conditions are all identical), measure the quality of the acidity nanometer granule of ferrum nanometer film surface adsorption, and learn accordingly, the quality of the acidity nanometer granule of ferrum nanometer film surface adsorption is directly proportional to the concentration of acidity nanometer granule, and follow: m=Ax+B, m is the quality of the acidity nanometer granule of ferrum nanometer film surface adsorption, x is the concentration of acidity nanometer granule, A is mass concentration factor, in the present embodiment, when the particle diameter of acidity nanometer granule is for 101.4nm, A is 6.99, B is mass concentration slope, B is zero.
And for the acidity nanometer granule that particle diameter is 20.7,32.5,51.5,75.4,101.4 and 153.9 (unit is nm), A respectively 1.55,2.25,3.60,5.20,6.99 and 10.5, B is mass concentration slope, and B is zero.
Namely under same particle diameter, the adsorbance of acidity nanometer granule is directly proportional to particle diameter, simultaneously, after this result is compared with existing gas chromatograph testing result, concordance is higher, illustrates that acidity nanometer granule prepared by the present invention can be used in acid ultrafine particle number concentration and particle size distribution in accurate calibration air.
The present invention is not limited to above-mentioned embodiment, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, and these improvements and modifications are also considered as within protection scope of the present invention.The content not being described in detail in this specification belongs to the known prior art of professional and technical personnel in the field.
Claims (7)
1. the preparation method of the acid nanometer property granule for demarcating, it is characterised in that: comprise the following steps:
S1, by mass parts, 1 part of ethanol is joined in 3～7 parts of saturated glucose solutions, after mix homogeneously atomization obtain the atomizing particle that particle diameter is 1.2～1.5mm；
S2, atomizing particle is imported in the quartz ampoule combustion furnace that temperature is 370～400 DEG C and burn after 5～15min, obtain the nano carbon particle that particle diameter is 10～200nm；
S3, it is diluted drying by carbon nano-particle, obtains carbon nanometer aerosol；
S4, it is that at 300～350 DEG C, evaporation obtains acid mist by concentrated sulphuric acid that concentration is 95～99% in temperature, by volume, condensing being cooled to 15～20 DEG C after 1 part of carbon nanometer aerosol and 3～7 parts of acid mist contact 3～5s, obtaining particle diameter is 20～250nm acidic carbon nano-particle.
2. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 1, it is characterised in that: in described step S1, the speed of atomization is 2ml/min, and the time of atomization is 20～40min.
3. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 1, it is characterised in that: in described step S2, the ignition temperature in quartz ampoule combustion furnace is 390 DEG C, and burning time is 10min.
4. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 1, it is characterised in that: diluting the water content of dried carbon nano-particle in described step S3 lower than 5%, density is 90～120g/cm3。
5. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 4, it is characterised in that: the water content diluting dried carbon nano-particle in described step S3 is 1%, and density is 103g/cm3。
6. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 1, it is characterised in that: in described step S4, the concentration of sulphuric acid is 98%.
7. the preparation method of a kind of acid nanometer property granule for demarcating as claimed in claim 1, it is characterised in that: in described step S4, the evaporating temperature of sulphuric acid is 340 DEG C.
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