CN105928840A - Method using single point adsorption method to measure specific surface area of atmospheric particulates - Google Patents
Method using single point adsorption method to measure specific surface area of atmospheric particulates Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 81
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 62
- 238000002835 absorbance Methods 0.000 claims abstract description 25
- 239000012086 standard solution Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims description 56
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 239000003463 adsorbent Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- 238000007865 diluting Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 11
- 239000003085 diluting agent Substances 0.000 claims description 9
- 239000013618 particulate matter Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 230000009514 concussion Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 230000000873 masking effect Effects 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical group [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000003556 assay Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000002156 adsorbate Substances 0.000 description 6
- 238000003795 desorption Methods 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000011481 absorbance measurement Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000005427 atmospheric aerosol Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000613 environmental toxicology Toxicity 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method using a single point adsorption method to measure the specific surface area of atmospheric particulates. The single point adsorption method utilizes a methylene blue water solution and comprises the following steps: (1) collecting atmospheric particulates, cutting, and weighing; (2) preparing a diluted original solution of methylene blue and a standard solution, determining the absorbance of standard solution, and drawing a work curve; (3) determining the absorbance of methylene blue solution, and calculating the adsorption amount of methylene blue according to the work curve; (4) calculating the specific surface area of atmospheric particulates. The method is simple, feasible, fast, and convenient, is suitable for measuring the surface area of atmospheric particulates, and has the characteristics of simple technology, low cost, strong operability, and low instrument requirements.
Description
Technical field
The invention belongs to atmospheric environment field, utilize single-point determination of adsorption method Atmospheric particulates ratio particularly to one
The method of surface area.
Background technology
Specific surface area be research Atmospheric particulates as environmental contaminants important parameter in environmental toxicology,
Therefore, it is possible to the specific surface area of accurate characterization Atmospheric particulates is extremely important.The method of measurement the specific area is a lot,
Conventional has BET low-temperature adsorption, electron microscope method and gas chromatography etc., but these methods all need
Want complicated device, or longer time.Detection sample is wanted by the specific surface area analysis instrument that experiment detection is commonly used
Asking higher, the Atmospheric particulates being attached on filter membrane do not meet testing conditions, thus cause Atmospheric particulates to compare table
The mensuration of area is limited, is unfavorable for the sign of Atmospheric particulates physico-chemical properties, seriously hinders air
The correlational study that grain thing is pathogenic.And solution adsorption method measures solid matter specific surface area, instrument is simple, operation
Convenient, the most often it is employed to measure material specific surface area.
The basic assumption of youth's Ge Miaoer adsorption theory is: the surface of solids is uniform, and absorption is monolayer adsorption,
Adsorbent is once adsorbed matter and covers and cannot be adsorbed again；When adsorption equilibrium, adsorb and be desorbed foundation and move
State balances；Before adsorption equilibrium, the rate of adsorption is directly proportional to blank surface, and desorption rate is directly proportional to coverage.
If the adsorption potential sum of the surface of solids is N, coverage is θ, and in solution, the concentration of adsorbate is c, according to
Above-mentioned it is assumed that have
The rate of adsorption: rInhale=k1N(1-q)c(k1For adsorbing filament technique) (1)
Desorption rate: rDe-=k-1Nq(k-1For desorption rate constant) (2)
When reaching adsorption equilibrium: rInhale=rDe-I.e. k1N (1-q) c=k-1Nq
Thus can obtain:
K in formulaInhale=k1/k-1Being referred to as adsorption equilibrium costant, its value is decided by adsorbent and the character of adsorbate and temperature
Degree, K suction value is the biggest, and solid is the strongest to adsorbate absorbability.If with equilibrium adsorption capacity during Γ indicated concentration c,
With Γ∞Represent monolayer adsorption amount, i.e. saturated extent of adsorption when whole adsorption potential is occupied, then: θ=Γ/Γ∞
Substitution formula (3)
Arrangement formula (4) obtains following form
Make c/ Γ～c figure, Γ can be tried to achieve from straight slope∞, K is just can get in conjunction with interceptInhale。Γ∞Refer to every gram of absorption
The agent saturated extent of adsorption (representing by the amount of material) to adsorbate, if each adsorption molecule is shared on the sorbent
According to area be SA, then the specific surface area of adsorbent can calculate according to the following formula
S=Γ∞LSA (6)
In formula, S is adsorbent specific surface area, and L is avogadros constant, SAAbsorption for methylene blue projects
Area.
Calculate specific surface area according to computing formula (6), need at least 3 variable concentrations ladders of material of the same race in theory
Degree, this is to limit, because this needs each atmospheric aerosol samples the heaviest greatly for Atmospheric particulates
Multiple three variable concentrations just can obtain specific surface area, greatly reduces experiment progress.
But according to Lang Gemiaoer mono molecule layer adsorption, when adsorbent and adsorbate reach to adsorb saturated after,
Absorption and desorption are in dynamic equilibrium, and at this moment adsorbate is paved with whole particle surface and does not leave room.Now inhale
The specific surface of attached dose of Atmospheric particulates can be calculated by formula (7):
In formula, S is specific surface area (m2/g)；C0For the mass fraction (%) of methylene blue in blank filter membrane solution；C is
The mass fraction (%) of methylene blue in filter membrane solution；V is the gross mass (g) of adsorbent solution；M is for adding solution
Adsorbent mass (g)；2450 can cover the area (m of particulate matter for 1g methylene blue2/g)。
The absorption of water-soluble dye is widely used to the mensuration of solid matter specific surface.In all dyestuffs, secondary
Methyl blue has the absorption tendency of maximum, and its chemical constitution is as follows:
Cation size is 1.70 × 10-10m×76×10-10m×325×10-10m.Research shows, in most solid,
Methylene blue absorption is all monolayer, i.e. meets the absorption of Lang Gemiaoer type.But when original solution concentration is higher,
There will be multilayer adsorption, and if after adsorption equilibrium the concentration of solution too low, then adsorb and can not reach full
With, therefore, the solution concentration after the concentration of original solution and adsorption equilibrium all should be selected in suitable scope.
Methylene blue be adsorbed with three kinds of trends: Planar adsorbent, projected area is 1.35 × 10-18m2；Side is inhaled
Attached, projected area is 7.5 × 10-19m2；End group adsorbs, and projected area is 39.5 × 10-19m2.For air
Grain thing, owing to structure is complicated, the suction type of methylene blue is current and uncertain.But, according to correlational study
Result calculates, in the case of monolayer adsorption, the area that 1mg methylene blue covers can be by 2.45m2Calculate,
Therefore the present invention also continues to use these data.
The measurement of solution concentration is by mean of what spectrophotometer completed.According to law of light absorption, work as incident illumination
During for the monochromatic light of certain wavelength, the optical density of certain solution and the concentration of coloring matter in solution and the thickness of solution
It is directly proportional, i.e.
A=-lg (I/I0)=ε bc (8)
Wherein: A is absorbance；I is transmitted intensity；I0For incident intensity；ε is absorptance；C is
Solution concentration；B is optical path length or the liquid layer thickness of solution.
It is, in general, that the absorption law of light can be suitably used for the monochromatic light of any wavelength, but for one specify molten
Liquid, the absorbance recorded under different wavelength is different.If absorbance A is mapped by wavelength X, available
The absorption curve of solution, as shown in Figure 1.Showing in figure, change with wavelength X, absorbance A is also constantly becoming
Change, and there is a maximum absorption wavelength.
In order to improve the sensitivity of measurement, operation wavelength should select the ripple corresponding when absorbance A value maximum
Long.Methylene blue solution has 2 absworption peak: 445nm and 665nm in visual field.But it is dry at 445nm
Disturb relatively big, therefore the general operation wavelength selected is 665nm, and measure with spectrophotometer.
Summary of the invention
It is an object of the invention to for above-mentioned existing problems and technical bottleneck, it is provided that one utilizes single-point absorption method to survey
The method determining Atmospheric particulates specific surface area, the method is simple and feasible, convenient, quick, is suitable for measuring air
The surface area of particulate matter.Additionally, this assay method also has technique simply, low cost, strong operability, to instrument
Device requires the features such as low.
Technical scheme:
A kind of method utilizing single-point determination of adsorption method Atmospheric particulates specific surface area, utilizes methylene blue aqueous solution
Single-point absorption method measuring point, comprises the following steps:
1) gather Atmospheric particulates collection shredding to weigh
Utilize atmosphere particulate matter sampler continuous acquisition 24 hours, sampler flow 28.3L/min, sampling membrane
For glass fiber filter, before sample collecting, it is placed in 450 DEG C of calcination 4h of Muffle furnace, sample with masking foil parcel filter membrane
Filter membrane is placed in after product collection in 4 DEG C of refrigerators preservation, and before and after sampling, filter membrane is all placed on temperature 25 DEG C, relative humidity
Thermostatic constant wet chamber's inner equilibrium 24h of 50%, finally weighs with 100,000/analytical balance, by the matter after sampling
Amount deducts the quality before sampling, obtains the quality of Atmospheric particulates, by the filter membrane containing small particle Atmospheric particulates
Being divided into quarter, shred with the rustless steel shears crossed through 400 DEG C of high-temperature process, same material is through phase
Shred as blank filter membrane with the filter membrane of processing procedure；
2) configure methylene blue original solution diluent and standard solution, determine the absorbance of standard solution and paint
Working curve processed
In order to accurately measure the concentration of 0.2m% methylene blue original solution, measure 2.5mL methylene blue solution
Put in 500mL volumetric flask, and with distilled water diluting to scale, stand-by, this is original solution diluent；
Measure 5.0mL 0.2m% methylene blue original solution to put in 100mL volumetric flask, and with distilled water diluting extremely
Scale is stand-by, and this is 0.01m% methylene blue standard solution；Take 2,4,6,8,10mL 0.01m%
Methylene blue standard solution is placed in 1000mL volumetric flask, by distilled water diluting to 1000mL, number consecutively
For A1, A2, A3, A4, A5, i.e. obtain concentration for (0.002,0.004,0.006,0.008,0.010) × 0.01%
The methylene blue standard solution of 5 kinds of concentration；
3) determine the absorbance of methylene blue solution, calculate the adsorbance of methylene blue according to working curve
It is placed in shredding the filter membrane after weighing in dry band plug Erlenmeyer flask, adds 2.5mL methylene blue water-soluble
Liquid diluent, by distilled water diluting to 50mL, numbering；Then band plug Erlenmeyer flask being placed on temperature is at 25 DEG C,
Ultrasonic 2.5-3h, ultrasonic after put on the oscillator 25 DEG C, rotating speed be under 120-150r/min concussion 1.5-2h,
The Atmospheric particulates being attached on filter membrane are made fully to be dissolved in aqueous solution, finally by solution by ultrasonic and concussion
Cross filter membrane that aperture is 0.22 μm fully to remove the big particle diameter filter membrane residue in solution；
4) calculating of the specific surface area of Atmospheric particulates
According to specific surface area computing formula
By 3) in obtain blank filter membrane solution and collect the filter membrane solution of Atmospheric particulates in the quality of methylene blue divide
The difference of number, and the quality of gross mass 50g of adsorbent solution and Atmospheric particulates brings in above formula, calculates big
The specific surface area of aerated particle thing.Wherein: S is specific surface area (m2/g)；C0For methine in blank filter membrane solution
Blue mass fraction (%)；C is the mass fraction (%) of methylene blue in filter membrane solution；V is the total of adsorbent solution
Quality (g)；M is the adsorbent mass (g) adding solution；2450 can cover the face of particulate matter for 1g methylene blue
Long-pending (m2/g)。
The working mechanism of the present invention:
This assay method is to utilize solution adsorption method to measure on the basis of solid specific surface original, combines greatly
The method that aerated particle thing attribute and mensuration reality are improved again.Original assay method is according to original solution and mark
The absorbance difference of quasi-solution determines specific surface area, but owing to Atmospheric particulates collection is on filter membrane, there is sky
The white filter membrane impact on final specific surface area, this impact is more prominent after filter membrane shreds.Therefore, the present invention
Give up original mensuration thinking, directly measure the difference of blank filter membrane and the filter membrane absorbance collecting Atmospheric particulates
Value, and original solution and extension rate need not be considered.
The invention have the advantage that this assay method is simple and feasible, convenient, quick, be suitable for measuring airborne particulate
The surface area of thing.Additionally, this assay method also has technique simply, low cost, strong operability, instrument is wanted
Seek the feature such as low.
Accompanying drawing explanation
Fig. 1 is solution absorption curve.
Fig. 2 is standard solution working curve.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1:
A kind of method utilizing single-point determination of adsorption method Atmospheric particulates specific surface area, utilizes methylene blue aqueous solution
Use single-point absorption method, the specific surface area of the small particle Atmospheric particulates collected is measured, including following
Step:
1) gather Atmospheric particulates collection shredding to weigh
Utilize atmosphere particulate matter sampler (JMT-3 type aerosol granularity profile samples device) continuous acquisition 24 little
Time, sampler flow 28.3L/min, sampling membrane is glass fiber filter, uses masking foil before sample collecting
Parcel filter membrane is placed in 450 DEG C of calcination 4h of Muffle furnace, filter membrane is placed in after sample collecting in 4 DEG C of refrigerators preservation, adopts
Before and after sample, filter membrane is all placed on thermostatic constant wet chamber's inner equilibrium 24h of temperature 25 DEG C, relative humidity 50%, finally uses
100000/analytical balance is weighed, and deducts the quality before sampling by the quality after sampling, obtains Atmospheric particulates
Quality, quarter will be divided into containing the filter membrane of small particle Atmospheric particulates, with at 400 DEG C of high temperature
The rustless steel shears managed shreds, and same material shreds as blank filter membrane through the filter membrane of same process.
2) configure methylene blue original solution diluent and standard solution, determine the absorbance of standard solution and paint
Working curve processed
In order to accurately measure the concentration of 0.2m% methylene blue original solution, measure 2.5mL methylene blue solution
Put in 500mL volumetric flask, and with distilled water diluting to scale, stand-by, this is original solution diluent；
Measure 5.0mL 0.2m% methylene blue original solution to put in 100mL volumetric flask, and with distilled water diluting extremely
Scale is stand-by, and this is 0.01m% methylene blue standard solution；Take 2,4,6,8,10mL 0.01m%
Methylene blue standard solution is placed in 1000mL volumetric flask, by distilled water diluting to 1000mL, number consecutively
For A1, A2, A3, A4, A5, i.e. obtain concentration for (0.002,0.004,0.006,0.008,0.010) × 0.01%
The methylene blue standard solution of 5 kinds of concentration.
For methylene blue solution, operation wavelength is 665nm.Owing to each spectrophotometer wave length calibration slightly misses
Difference, takes the standard solution (i.e. A3) that concentration is 0.04 × 0.01%, utilizes light splitting light in the range of 600-700nm
Degree meter carries out absorbance scanning, and with the maximum wavelength of absorbance as operation wavelength, the present embodiment is 600～700nm
In the range of entirely sweep, entirely sweep rear absorption curve as it is shown in figure 1, according to data in figure are analyzed observe, obtain
The wavelength of absorbance maximum is 663nm, and therefore using 663nm is operation wavelength.Because methine has suction
Attached property, according to the sequential determination absorbance from dilute to dense.According to the absorbance obtained, draw about A C's
Working curve.Absorbance measurement the results are shown in Table 1, and working curve is shown in Fig. 2.
| Sample | Mass fraction % | Absorbance A |
| A1 | 0.00002 | 0.0076 |
| A2 | 0.00004 | 0.0187 |
| A3 | 0.00006 | 0.0291 |
| A4 | 0.00008 | 0.0417 |
| A5 | 0.0001 | 0.0537 |
Table 1
3) determine the absorbance of methylene blue solution, calculate the adsorbance of methylene blue according to working curve
It is placed in shredding the filter membrane after weighing in dry band plug Erlenmeyer flask, adds 2.5mL methylene blue water-soluble
Liquid diluent, by distilled water diluting to 50mL, numbering；Then band plug Erlenmeyer flask being placed on temperature is at 25 DEG C,
Ultrasonic 3h, ultrasonic after put on the oscillator 25 DEG C, shake 2h under rotating speed 150r/min, by ultrasonic and
Concussion makes the Atmospheric particulates being attached on filter membrane fully be dissolved in aqueous solution, and solution is finally crossed aperture is
The filter membrane of 0.22 μm is fully to remove the big particle diameter filter membrane residue in solution.
The absorbance of the solution obtained is brought into the concentration value checking in correspondence on A C working curve, spectrophotometric
Meter Automatic continuous measures three times, and the concentration value therefore finally given is meansigma methods.According in blank filter membrane solution
The mass fraction of methylene blue and collect Atmospheric particulates filter membrane solution in the mass fraction of methylene blue
Difference, in conjunction with gross mass and the quality of Atmospheric particulates of adsorbent solution, can obtain the adsorbance of methylene blue.
4) calculating of the specific surface area of Atmospheric particulates
According to specific surface area computing formula
By 3) in obtain blank filter membrane solution and collect the filter membrane solution of Atmospheric particulates in the quality of methylene blue divide
The difference of number, and the quality of gross mass 50g of adsorbent solution and Atmospheric particulates brings in above formula, calculates big
The specific surface area of aerated particle thing, wherein: S is specific surface area (m2/g)；C0For methine in blank filter membrane solution
Blue mass fraction (%)；C is the mass fraction (%) of methylene blue in filter membrane solution；V is the total of adsorbent solution
Quality (g)；M is the adsorbent mass (g) adding solution；2450 can cover the face of particulate matter for 1g methylene blue
Long-pending (m2/g)。
Result sees table 2:
| Sample | Atmospheric particulates quality g | Absorbance A | Mass fraction difference % | Specific surface area m2/g |
| Blank | 0.0633 | |||
| 1 | 0.00007 | 0.0358 | 4.77431E-05 | 83.55035 |
| 2 | 0.00008 | 0.0344 | 5.01736E-05 | 76.82834 |
| 3 | 0.00004 | 0.0329 | 5.27778E-05 | 161.6319 |
| 4 | 0.00005 | 0.0458 | 3.03819E-05 | 74.43576 |
| 5 | 0.00007 | 0.0293 | 5.90278E-05 | 103.298611 |
Table 2
Assay method described in the embodiment of the present invention 1 is applicable to the mensuration of small particle Atmospheric particulates specific surface area.
Embodiment 2:
A kind of method utilizing single-point determination of adsorption method Atmospheric particulates specific surface area, utilizes methylene blue aqueous solution
Use single-point absorption method, the specific surface area of the big particle diameter Atmospheric particulates collected is measured, implement step
Substantially the same manner as Example 1, difference is:
In step 3) in, ultrasonic time is 2.5h, and the concussion time is 1.5h, and concussion rotating speed is 120r/min；
Solution crosses the filter membrane of aperture 0.45 μm to remove the residue in solution.
For large-size particles thing, its specific area measuring the results are shown in Table 3.
| Sample | Atmospheric particulates quality g | Absorbance A | Mass fraction difference % | Specific surface area m2/g |
| Blank | 0.0633 | |||
| 1 | 0.00009 | 0.056 | 1.26736E-05 | 17.25019 |
| 2 | 0.0001 | 0.0569 | 1.11111E-05 | 13.61111 |
| 3 | 0.00015 | 0.0365 | 4.65278E-05 | 37.99769 |
| 4 | 0.00006 | 0.0486 | 2.55208E-05 | 52.10503 |
| 5 | 0.00005 | 0.0489 | 0.000025 | 61.25 |
Table 3
Assay method described in the embodiment of the present invention 2 is applicable to the mensuration of big particle diameter Atmospheric particulates specific surface area.
The spectrophotometric sensitivity used according to those skilled in the art and degree of stability, can suitably adjust
The extension rate of methylene blue solution, the absorbance detected in theory is at least greater than 0.1, optimal line
Property scope is between 0.3～0.7, and the result repeatedly tested should change between average 1.0%.But, implement
Example instrument can meet condition determination completely, does not therefore perform in strict accordance with above-mentioned condition.It addition,
The control of methylene blue original solution mass fraction, for ensureing adsorption effect, is typically by other reference examples
0.2%, balance solution mass fraction is not less than 0.1%.But the present invention is few in view of the amount of Atmospheric particulates, and
The methylene blue severe contamination cuvette of high concentration and spectrophotometer, therefore, done corresponding on extension rate
Adjust.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and
And without departing from the spirit or essential characteristics of the present invention, it is possible to realize this in other specific forms
Bright, and appropriateness of the present invention is extended in other embodiments.Therefore, no matter from the point of view of which point, all should
Regarding embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by claims
It not that described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, but the most each embodiment party
Formula only comprises an independent technical scheme, and this narrating mode of description is only for clarity sake, ability
Field technique personnel should be using description as an entirety, and the technical scheme in each embodiment can also be through suitable group
Close, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (1)
1. the method utilizing single-point determination of adsorption method Atmospheric particulates specific surface area, it is characterised in that utilize secondary
Methyl blue aqueous solution single-point absorption method measuring point, comprises the following steps:
1) gather Atmospheric particulates collection shredding to weigh
Utilize atmosphere particulate matter sampler continuous acquisition 24 hours, sampler flow 28.3L/min, sampling membrane
For glass fiber filter, before sample collecting, it is placed in 450 DEG C of calcination 4h of Muffle furnace, sample with masking foil parcel filter membrane
Filter membrane is placed in after product collection in 4 DEG C of refrigerators preservation, and before and after sampling, filter membrane is all placed on temperature 25 DEG C, relative humidity
Thermostatic constant wet chamber's inner equilibrium 24h of 50%, finally weighs with 100,000/analytical balance, by the matter after sampling
Amount deducts the quality before sampling, obtains the quality of Atmospheric particulates, by the filter membrane containing small particle Atmospheric particulates
Being divided into quarter, shred with the rustless steel shears crossed through 400 DEG C of high-temperature process, same material is through phase
Shred as blank filter membrane with the filter membrane of processing procedure；
2) configure methylene blue original solution diluent and standard solution, determine the absorbance of standard solution and paint
Working curve processed
In order to accurately measure the concentration of 0.2m% methylene blue original solution, measure 2.5mL methylene blue solution
Put in 500mL volumetric flask, and with distilled water diluting to scale, stand-by, this is original solution diluent；
Measure 5.0mL 0.2m% methylene blue original solution to put in 100mL volumetric flask, and with distilled water diluting extremely
Scale is stand-by, and this is 0.01m% methylene blue standard solution；Take 2,4,6,8,10mL 0.01m%
Methylene blue standard solution is placed in 1000mL volumetric flask, by distilled water diluting to 1000mL, number consecutively
For A1, A2, A3, A4, A5, i.e. obtain concentration for (0.002,0.004,0.006,0.008,0.010) × 0.01%
The methylene blue standard solution of 5 kinds of concentration；
3) determine the absorbance of methylene blue solution, calculate the adsorbance of methylene blue according to working curve
It is placed in shredding the filter membrane after weighing in dry band plug Erlenmeyer flask, adds 2.5mL methylene blue water-soluble
Liquid diluent, by distilled water diluting to 50mL, numbering；Then band plug Erlenmeyer flask being placed on temperature is at 25 DEG C,
Ultrasonic 2.5-3h, ultrasonic after put on the oscillator 25 DEG C, rotating speed be under 120-150r/min concussion 1.5-2h,
The Atmospheric particulates being attached on filter membrane are made fully to be dissolved in aqueous solution, finally by solution by ultrasonic and concussion
Cross filter membrane that aperture is 0.22 μm fully to remove the big particle diameter filter membrane residue in solution；
4) calculating of the specific surface area of Atmospheric particulates
According to specific surface area computing formula
By 3) in obtain blank filter membrane solution and collect the filter membrane solution of Atmospheric particulates in the quality of methylene blue divide
The difference of number, and the quality of gross mass 50g of adsorbent solution and Atmospheric particulates brings in above formula, calculates big
The specific surface area of aerated particle thing.Wherein: S is specific surface area (m2/g)；C0For methine in blank filter membrane solution
Blue mass fraction (%)；C is the mass fraction (%) of methylene blue in filter membrane solution；V is the total of adsorbent solution
Quality (g)；M is the adsorbent mass (g) adding solution；2450 can cover the face of particulate matter for 1g methylene blue
Long-pending (m2/g)。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107421865A (en) * | 2017-05-10 | 2017-12-01 | 大连理工大学 | A kind of detection method of textile retention Atmospheric particulates ability |
| CN107543786A (en) * | 2017-08-29 | 2018-01-05 | 中国科学院宁波材料技术与工程研究所 | A kind of method for determining grapheme material specific surface area |
| CN110177476A (en) * | 2016-11-18 | 2019-08-27 | 莱战略控股公司 | Humidity Sensing for Aerosol Delivery Devices |
| CN110346474A (en) * | 2019-07-26 | 2019-10-18 | 南京信息工程大学 | TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample |
| CN111474084A (en) * | 2020-04-07 | 2020-07-31 | 河北科技大学 | Characterization method for density of silicon dioxide particles in silica sol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734656A (en) * | 2008-11-20 | 2010-06-16 | 西安科技大学 | Method for preparing active carbon with high specific surface area from coal and waste and old plastics by microwave |
| CN102854167A (en) * | 2012-08-14 | 2013-01-02 | 浙江中一检测研究院股份有限公司 | Method for determination of concentration of mineral oil mist in workshop air |
| CN104089849A (en) * | 2014-06-18 | 2014-10-08 | 攀枝花市钛都化工有限公司 | Measuring method for specific surface area of denitration titanium dioxide |
-
2016
- 2016-04-13 CN CN201610230807.3A patent/CN105928840A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734656A (en) * | 2008-11-20 | 2010-06-16 | 西安科技大学 | Method for preparing active carbon with high specific surface area from coal and waste and old plastics by microwave |
| CN102854167A (en) * | 2012-08-14 | 2013-01-02 | 浙江中一检测研究院股份有限公司 | Method for determination of concentration of mineral oil mist in workshop air |
| CN104089849A (en) * | 2014-06-18 | 2014-10-08 | 攀枝花市钛都化工有限公司 | Measuring method for specific surface area of denitration titanium dioxide |
Non-Patent Citations (2)
| Title |
|---|
| 吾拉尔·哈那哈提，薛静，迪丽努尔·塔力甫: "乌鲁木齐市大气可吸入颗粒物中多环芳烃与颗粒物比表面积、气象因素相关性的探讨", 《广东化工》 * |
| 张国艳等: "关于次甲基蓝水溶液吸附法测定颗粒活性炭比表面积实验的探讨", 《大学化学》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110177476A (en) * | 2016-11-18 | 2019-08-27 | 莱战略控股公司 | Humidity Sensing for Aerosol Delivery Devices |
| CN110177476B (en) * | 2016-11-18 | 2022-10-21 | 莱战略控股公司 | Humidity sensing for aerosol delivery devices |
| CN107421865A (en) * | 2017-05-10 | 2017-12-01 | 大连理工大学 | A kind of detection method of textile retention Atmospheric particulates ability |
| CN107543786A (en) * | 2017-08-29 | 2018-01-05 | 中国科学院宁波材料技术与工程研究所 | A kind of method for determining grapheme material specific surface area |
| CN110346474A (en) * | 2019-07-26 | 2019-10-18 | 南京信息工程大学 | TD-GCMS measures the sample injection method of nonpolar organic matter on gradation diameter aerosol sample |
| CN111474084A (en) * | 2020-04-07 | 2020-07-31 | 河北科技大学 | Characterization method for density of silicon dioxide particles in silica sol |
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