CN109917052A - A method of sulfuric acid mist in the organized discharge exhaust gas of measurement - Google Patents
A method of sulfuric acid mist in the organized discharge exhaust gas of measurement Download PDFInfo
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- CN109917052A CN109917052A CN201910334314.8A CN201910334314A CN109917052A CN 109917052 A CN109917052 A CN 109917052A CN 201910334314 A CN201910334314 A CN 201910334314A CN 109917052 A CN109917052 A CN 109917052A
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Abstract
The invention discloses the methods of sulfuric acid mist in a kind of organized discharge exhaust gas of measurement, comprising: is extracted using sodium carbonate and sodium bicarbonate mixed solution as leacheate using sodium bicarbonate solution as absorbing liquid using ultrasonic extraction, uses Dionex IonPacTMAS22 analytical column and electric conductivity detector carry out ion-chromatographic determination to sulfuric acid mist content.
Description
Technical field
The invention belongs to wasted nickel catalyst technical fields, and in particular to a kind of organized side for discharging sulfuric acid mist in exhaust gas of measurement
Method.
Background technique
Sulfuric acid mist refers to the smog that the sulfuric acid particles largely floated are formed, and is smelted by fossil-fuel-fired or mineral, sulfuric acid
The sulfur-containing oxide exhaust gas discharged during production etc. causes, and is a kind of atmosphere pollution phenomenon.There is the standard regulation sulfuric acid mist to include
Soluble sulphate in sulfuric acid droplet, sulfur trioxide and particulate matter.The generation of sulfuric acid mist, which had both betided, directly to be produced or makes
With the factory of sulfuric acid, also from discharging fume by the factory of raw material and fuel of coal, petroleum or heavy oil.Sulfur dioxide gas in smoke evacuation
After being oxidized to sulfur trioxide, sulfuric acid mist is generated in conjunction with the moisture in air.Sulfur Dioxide In The Atmosphere can be oxidized to sulfuric acid
Mist is directly entered alveolar with floating dust.The Acid Rain Pollution range as caused by sulfur dioxide (SO2) emissions constantly expands, to human health and
Ecological environment does great damage.
Measurement about sulfuric acid mist in exhaust gas at present be concentrated mainly on the chromatography of ions and Barium Chromate Spectrophotometry this two
Kind of method, but Barium Chromate Spectrophotometry suitable for it is low, content sulfuric acid mist measurement, and analysis time is long, ion chromatography
Method is simple, efficient.
For sulfuric acid mist other than soluble sulphate in finger particulate matter and fine drop, sulfur trioxide gas also belongs to sulfuric acid
The scope of mist, the previous filter cylinder that samples is as utensil Shortcomings place is absorbed, it can only acquire soluble sulphate and part is thin
Droplet, fine drop sampling is incomplete in sampling process if the adsorption capacity that droplet content has been larger than filter cylinder, and filters
Cylinder can not absorb sulfur trioxide gas, therefore the absorbing liquid in sampling process is particularly significant, but the selection of absorbing liquid is in addition to needing
It adapts to also want effectively adsorb fine drop and sulfur trioxide gas other than the requirement of ion chromatograph itself.
Summary of the invention
The purpose of the invention is to overcome the problems, such as that the sampling in the presence of the prior art is incomplete, and provide one kind
The method of sulfuric acid mist in the organized discharge exhaust gas of measurement, precision is high, and accuracy is high.
To achieve the goals above, the organized method for discharging sulfuric acid mist in exhaust gas is measured the present invention provides a kind of,
In, this method is using sodium carbonate and sodium bicarbonate mixed solution as leacheate, using sodium bicarbonate solution as absorbing liquid, using super
Sound wave extraction extracts, and is measured by the chromatography of ions to sulfuric acid mist content.
The method of sulfuric acid mist in the organized discharge exhaust gas of a kind of measurement provided by the present invention, comprising the following steps: sample
Acquisition, the preparation of standard curve, the preparation of sample, the measurement of sample, result calculate.
The sample acquisition includes: organized discharge waste gas collecting: sampling step refers to HJ 544-2016, by glass fibers
It ties up filter cylinder to be packed into the filter cylinder folder on sampler head, the impact type for filling 50mL absorbing liquid in series connection two after smoke dust sampling instrument is inhaled
Bottle, acquisition sulfur trioxide gas and the fine drop for penetrating filter cylinder are received, is then connect again with empty bottle and drier.Connecting tube to the greatest extent may be used
It can air-tightness and reliability short and that check system.The sampled point constant speed that sampler equipped with filter cylinder protrudes into exhaust tube is adopted
Sample, in sampling process, opium pipe heating temperature is not less than flue-gas temperature.The sampling time appropriate is selected according to sulfuric acid mist concentration, even
Sampling in continuous 1 hour acquires 3~4 samples, while measuring temperature, pressure and other parameters in 1 hour with constant duration.It adopts
After sample, the careful filter cylinder that takes out is put into cap-rotating type wide mouth polyethylene seal pipe, samples mouth and curved with a small amount of ultrapure water
Inside pipe wall, cleaning solution are incorporated in seal pipe, cover bottle stopper, first, second impact type absorption bottle with polyethylene pipe be sealed to
It surveys.Organized discharge full procedure blank acquisition: every time acquisition sample should at least two sets of full procedure blank samples of band, will be filtered with batch
Cylinder and the absorption bottle for installing absorbing liquid are brought to sampling location, do not connect with sampler, it is to be measured that laboratory is taken back after sampling.
The preparation of the standard curve includes: using pure water as the preparation of the sulfate radical standard solution of solvent: being pipetted respectively dense
Degree be 1000 μ g/mL sulfate radical standard solution 0.075mL, 0.030mL, 0.060mL, 0.15mL, 0.30mL in 50mL,
In 10mL, 10mL, 10mL, 10mL volumetric flask, be settled to scale with ultrapure water, mix, be configured to concentration be 1.5mg/L,
The sulfate radical standard solution of 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L；Using 15mmol/L sodium hydrate aqueous solution as solvent
Sulfate radical standard solution preparation: pipette respectively concentration be 1000 μ g/mL sulfate radical standard solution 0.075mL,
0.030mL, 0.060mL, 0.15mL, 0.30mL are in 50mL, 10mL, 10mL, 10mL, 10mL volumetric flask, with 15mmol/L hydrogen
Aqueous solution of sodium oxide is settled to scale, mixes, and being configured to concentration is 1.5mg/L, 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L
Sulfate radical standard solution；Using 15mmol/L sodium bicarbonate aqueous solution as the preparation of the sulfate radical standard solution of solvent: moving respectively
Take concentration be 1000 μ g/mL sulfate radical standard solution 0.075mL, 0.030mL, 0.060mL, 0.15mL, 0.30mL in 50mL,
In 10mL, 10mL, 10mL, 10mL volumetric flask, it is settled to scale with 15mmol/L sodium bicarbonate aqueous solution, mixes, is configured to dense
Degree is the sulfate radical standard solution of 1.5mg/L, 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L.
The preparation of the sample includes: that will acquire resulting absorbing liquid and filter cylinder is fully transferred to 100mL color-comparison tube
In, polymeric seal pipe and absorption bottle inner wall are washed with appropriate experimental water, washing lotion is incorporated in color-comparison tube, is settled to scale
Color-comparison tube is put into ultrasound 45min in ultrasonic cleaner, cooling to mix, leachate by (need to submerge glass fiber filter cylinder)
It is to be measured into clean container through 0.45 μm of washing filtering with microporous membrane.Sample in second absorption bottle moves into another 100mL
In color-comparison tube, with appropriate milli-Q water absorption bottle inner wall, it is to be measured that imbibition is incorporated to constant volume in color-comparison tube.Whole Process is empty
Sample together pre-treatment preparation of the white sample with acquisition.
The measurement of the sample includes: ready sample to be pipetted 1mL with syringe sample introduction is analyzed, fixed with retention time
Property, peak area quantification.
The result calculates
In formula: the concentration of sulfuric acid mist, mg/m in ρ-exhaust gas3；
ρ1The concentration of sulfate radical, μ g/mL in the filter cylinder and first absorption bottle sample of-measurement；
ρ2The concentration of sulfate radical, μ g/mL in the filter cylinder and second absorption bottle sample of-measurement；
ρ0The concentration of sulfate radical, μ g/mL in the blank sample of-measurement experiment room；
V-sample to be tested volume, mL；
VndThe sampling volume of dry flue gas, L under-standard state (101.325kPa, 273K)；
DF-sample extension rate；
The molal weight of 98.08-sulfuric acid, g/mol；
The molal weight of 96.06-sulfate radicals, g/mol.
Detailed description of the invention
Fig. 1 is the map that sodium bicarbonate aqueous solution is absorbing liquid
Fig. 2 is the map that sodium hydrate aqueous solution is absorbing liquid
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, however it is not limited to the present invention.
Embodiment 1: using 30mmol/L sodium hydrate aqueous solution as absorbing liquid
Step 1: sample acquisition
Organized discharge waste gas collecting: glass fiber filter cylinder is packed into the filter cylinder folder on sampler head, in smoke dust sampling
The impact type absorption bottle for two built-in 50mL 30mmol/L sodium hydrate aqueous solution absorbing liquids of connecting after device, acquires sulfur trioxide
Gas and the fine drop for penetrating filter cylinder, then connect with empty bottle and drier again.Connecting tube is as short as possible and checks system
Air-tightness and reliability.Sampler equipped with filter cylinder is protruded into the sampled point isokinetic sampling in exhaust tube, in sampling process, opium pipe
Heating temperature is not less than flue-gas temperature.Sampling time appropriate, sampling or small 1 in continuous 1 hour are selected according to sulfuric acid mist concentration
When interior 3~4 samples, while measuring temperature, pressure and other parameters are acquired with constant duration.It is careful to take out after sampling
Filter cylinder is put into cap-rotating type wide mouth polyethylene seal pipe, samples mouth with a small amount of ultrapure water and elbow internal wall, cleaning solution are incorporated to
In seal pipe, bottle stopper is covered, first, second impact type absorption bottle is sealed to be measured with polyethylene pipe.
Organized discharge full procedure blank acquisition: every time acquisition sample should at least two sets of full procedure blank samples of band, will be same
Batch filter cylinder and the absorption bottle for installing absorbing liquid are brought to sampling location, are not connect with sampler, and experiment is taken back after sampling
Room is to be measured.
Step 2: the preparation of standard curve
Using pure water as the preparation of the sulfate radical standard solution of solvent:
Pipette respectively concentration be sulfate radical standard solution 0.075mL, 0.030mL of 1000 μ g/mL, 0.060mL,
0.15mL, 0.30mL are settled to scale in 50mL, 10mL, 10mL, 10mL, 10mL volumetric flask, with ultrapure water, mix, and prepare
It is the sulfate radical standard solution of 1.5mg/L, 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L at concentration.
Using 15mmol/L sodium hydrate aqueous solution as the preparation of the sulfate radical standard solution of solvent:
Pipette respectively concentration be sulfate radical standard solution 0.075mL, 0.030mL of 1000 μ g/mL, 0.060mL,
0.15mL, 0.30mL are in 50mL, 10mL, 10mL, 10mL, 10mL volumetric flask, with 15mmol/L sodium hydrate aqueous solution constant volume
It to scale, mixes, it is molten to be configured to the sulfate radical standard that concentration is 1.5mg/L, 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L
Liquid.
Using 15mmol/L sodium bicarbonate aqueous solution as the preparation of the sulfate radical standard solution of solvent:
Pipette respectively concentration be sulfate radical standard solution 0.075mL, 0.030mL of 1000 μ g/mL, 0.060mL,
0.15mL, 0.30mL are in 50mL, 10mL, 10mL, 10mL, 10mL volumetric flask, with 15mmol/L sodium bicarbonate aqueous solution constant volume
It to scale, mixes, it is molten to be configured to the sulfate radical standard that concentration is 1.5mg/L, 3.0mg/L, 6.0mg/L, 15mg/L, 30mg/L
Liquid.
Step 3: the preparation of sample
Resulting absorbing liquid will be acquired and filter cylinder is fully transferred in 100mL color-comparison tube, washed with appropriate experimental water
Polymeric seal pipe and absorption bottle inner wall are washed, washing lotion is incorporated in color-comparison tube, and being settled to scale (need to submerge glass fibre filter
Cylinder), color-comparison tube is put into ultrasound 45min in ultrasonic cleaner, cooling to mix, leachate is filtered through 0.45 μm of washing micropore
Film filters into clean container to be measured.Sample in second absorption bottle moves into another 100mL color-comparison tube, with appropriate
Milli-Q water absorption bottle inner wall, it is to be measured that imbibition is incorporated to constant volume in color-comparison tube.Sample of the full procedure blank sample with acquisition
Together prepared by pre-treatment.
Step 4: the measurement of sample
Ready sample with syringe is pipetted 1mL, and sample introduction is analyzed, peak area quantification qualitative with retention time.
(1) selection of leacheate
Instrument carries the analytical column of AS22, belongs to the chromatographic column of carbonate system, therefore selects sodium carbonate and sodium bicarbonate mixed
For standardization solution as leacheate, proportion is 4.5mM NaCO3/1.4mM NaHCO3。
Fig. 1 is the map that sodium bicarbonate aqueous solution is absorbing liquid, it will be seen from figure 1 that in 4.5mM NaCO3/1.4mM
NaHCO3Under this leacheate system, when in solution using sodium bicarbonate aqueous solution as matrix, baseline is more steady after instrument analysis；
When a certain amount of sulfate radical standard solution is added analyzing into sample, it is found that the response of sulfate radical is larger, and when containing 3mg/L
The peak area of sulfate radical has 1.0865 μ S.min in the aqueous solution of sulfate radical.
(2) measurement of detection limit
Due to sulfate radical-free ion in blank, therefore select the standard of a fixed concentration molten in 2-5 times for estimating detection limit
7 needle of liquid continuous sample introduction selects 7 needle of standard solution continuous sample introduction of 1.5mg/L, the detection limit measurement result of sulfate radical such as following table institute
Show:
| Detection limit/(mg/L) | |
| 1 | 1.4394 |
| 2 | 1.4203 |
| 3 | 1.4041 |
| 4 | 1.4353 |
| 5 | 1.4198 |
| 6 | 1.4068 |
| 7 | 1.4070 |
| Standard deviation/(mg/L) | 0.0141 |
| T value | 3.143 |
| Detection limit/(mg/L) | 0.0444 |
Thus the detection limit for obtaining this method measurement sulfuric acid mist content is 0.0444mg/L.
(3) precision measures
Under the operating conditions described above, parallel respectively to the standard solution of basic, normal, high concentration to survey after instrumental baseline is stablized
It is 6 times fixed, and the concentration of sulfate radical is calculated, the precision measurement result of sulfate radical is as shown in the table:
Thus the precision of the basic, normal, high concentration of the sulfate radical content measurement obtained is 0.74% respectively, 0.29%,
0.41%.
(4) accuracy calculates
Blank sample is added the standard solution of fixed amount, then Whole Process is referring to determination step, each solution continuously into
Sample 3 times, show that sulfate radical accuracy determination data are as shown in the table:
It is obtained by above data, sample recovery of standard addition is 95.2% and 96.4%.
Comparative example 1: using 30mmol/L sodium hydrate aqueous solution as absorbing liquid.
Change the absorbing liquid in embodiment 1 into 30mmol/L sodium hydrate aqueous solution, the other the same as in Example 1.It will be ready to
Sample with syringe pipette 1mL sample introduction is analyzed, peak area quantification qualitative with retention time.
Fig. 2 is the map that sodium hydrate aqueous solution is absorbing liquid, from figure 2 it can be seen that in 4.5mM NaCO3/1.4mM
NaHCO3Under this leacheate system, when in solution using sodium hydrate aqueous solution as matrix, baseline fluctuation is larger after instrument analysis,
It is unfavorable for the accuracy of data；When a certain amount of sulfate radical standard solution is added analyzing into sample, the response of sulfate radical is found
Value is very small, and when the peak area of sulfate radical in the aqueous solution containing 3mg/L sulfate radical only has 0.0178 μ Smin.
Found by the comparison of embodiment 1 and comparative example 1, use 30mmol/L sodium bicarbonate aqueous solution for absorbing liquid for
Precision and the accuracy for improving analysis result are particularly significant.
In conclusion the sulfuric acid mist in organized exhaust gas is acquired back by way of glass fiber filter cylinder and absorbing liquid real
After testing room, in Dionex IonPacTMUnder conditions of AS22 analytical column and electric conductivity detector, use with sodium carbonate and bicarbonate
The content that sodium mixed solution measures sulfuric acid mist in organized exhaust gas as leacheate, using sodium bicarbonate solution as absorbing liquid is practical
It is feasible.
Claims (6)
1. a kind of method of sulfuric acid mist in organized discharge exhaust gas of measurement, which is characterized in that mixed with sodium carbonate and sodium bicarbonate
Solution is extracted using sodium bicarbonate solution as absorbing liquid using ultrasonic extraction as leacheate, to sulfuric acid mist content
Carry out ion-chromatographic determination.
2. the method according to claim 1, wherein the following steps are included: sample acquisition, standard curve are matched
System, the preparation of sample, the measurement of sample, result calculate.
3. according to the method described in claim 2, sampler used in sample acquisition includes glass fiber filter cylinder and two
The impact type absorption bottle of built-in absorbing liquid, the glass fiber filter cylinder are packed into the filter cylinder folder on the sampler head, and described two
Only the impact type absorption bottle of built-in absorbing liquid is connected on behind smoke dust sampling instrument.
4. according to the method described in claim 3, the absorbing liquid is sodium bicarbonate aqueous solution.
5. according to the method described in claim 2, the preparation of the sample is extracted using ultrasonic extraction, and using colorimetric
Ware pipe constant volume.
6. according to the method described in claim 2, the measurement of the sample uses Dionex IonPacTMAS22 analytical column and electricity
It leads detector and ion-chromatographic determination, peak area quantification qualitative with retention time is carried out to sulfuric acid mist content.
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Cited By (1)
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| CN110470761A (en) * | 2019-08-20 | 2019-11-19 | 谱尼测试集团吉林有限公司 | The measuring method of sulfuric acid mist in a kind of surrounding air |
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