CN100587487C - Combined detection method for high-purity SO3 gas and impurity SO2 gas therein - Google Patents
Combined detection method for high-purity SO3 gas and impurity SO2 gas therein Download PDFInfo
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- CN100587487C CN100587487C CN200610027779A CN200610027779A CN100587487C CN 100587487 C CN100587487 C CN 100587487C CN 200610027779 A CN200610027779 A CN 200610027779A CN 200610027779 A CN200610027779 A CN 200610027779A CN 100587487 C CN100587487 C CN 100587487C
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Abstract
The disclosed combined detection method for high-pure SO3 gas with SO2 as impurity comprises: constant-volume sampling at least 60Deg better 60-80Deg to avoid liquidation of SO3, absorbing with alkalisolution to obtain total volume percentage concentration of high-pure SO3 gas and SO2; processing the absorbed liquid, using iodometric method to obtain SO2 volume percentage concentration and then the SO3 concentration. This invention brings an error less than 0.1%.
Description
Technical field
The present invention relates to high-purity SO
3Gas reaches wherein impurity SO
2The detection method of gas.This method belongs to a kind of centralized procurement sample, constant volume and the Trinitarian detection high-purity of absorption SO
3Gas reaches wherein impurity SO
2The associated detecting method of gas.Specifically relate to the oleum evaporation and resolve production high-purity SO
3Gas reaches wherein impurity SO
2The detection method of gas volume percentage concentration.
Background technology
In a kind of patent process that adopts the synthetic chlorosulfonic acid of high-purity sulfuric anhydride, broken through the traditional concept that can only prepare chlorosulfonic acid originally with the low concentration sulfuric anhydride.And adopting high-concentration sulfur trioxide gas and high concentration chlorination hydrogen directly to carry out synthetic reaction, this method has advantages such as the consumption of raw materials of minimizing, pollution are little, good product quality, facts have proved that the advantage of this process is approved by people.So high-purity SO
3The detection of gas concentration is very important, and the consumption that can be material provides strong scientific basis with clearing.But, because high-purity SO
3Gas has the highly acid strong oxidizing property, be to high-purity SO
3Gas detects and exists very big difficulty, the SO that has reported
3The method of gas detection has multiple, but and is not suitable for high-purity SO
3The detection of gas.
JP55032758A2 is illustrated as Jap.P., by contacting gas efficient selective ground with 320W500 ℃ of carbonaceous material with SO
3Change into SO
2(also analyzer not being caused corrosion) is used for measuring SO
X, SO
3, SO
2Ratio, but only be applicable to SO in burnt gas, the automobile exhaust gas
3, SO
2Detection, belong to the detection of low strength range.
And for example the analytical approach of Jap.P. JP55135743A2 sulfuric anhydride has been introduced in containing the gas of sulfuric anhydride and has been added ammonium, thereby the ammonium salt that collection and analysis sulfuric acid are bonded on the cooling duct can exact grasp SO
3The method of concentration.This method very complicated, and can not be simultaneously with SO
3And SO
2The gas joint-detection.
Jap.P. JP203014633A2SO for another example
3Opacimeter can provide a kind of accurate measurement SO by the pressure of monitoring gas cell under the high temperature
3The opacimeter of content, but this method only is applicable to SO in the flue gas
3The measurement of content, and be not suitable for high concentration SO
3Gas content and SO wherein
2The simultaneous determination of foreign gas content.
Summary of the invention
Because high-purity SO
3Gas has the character of strong oxidizing property and normal temperature easy down liquefy (boiling point is 46.8 ℃), exists high-purity SO for overcoming prior art
3Gas reaches wherein SO
2Blank on the gas concentration detection method and defective the invention provides a kind of high-purity SO
3Reach wherein impurity SO
2The associated detecting method of gas.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of high-purity SO
3Gas reaches wherein impurity SO
2The method of gas concentration joint-detection comprises with absorption plant high-purity SO
1Gas reaches wherein impurity SO
2The gas constant volume of sampling absorbs with aqueous slkali then, obtains high-purity SO
3Gas reaches wherein impurity SO
2The cumulative volume percentage concentration of gas after absorption liquid being handled, adopts direct iodimetric titration to record SO again
2The concentration expressed in percentage by volume of gas is with high-purity SO
3Gas reaches wherein impurity SO
2The cumulative volume percentage concentration of gas deducts SO
2The concentration expressed in percentage by volume of gas is high-purity SO
3Gas concentration is characterized in that, when absorption plant carries out constant-volume sampling, is to carry out in the thermal environment more than at least 60 ℃.
When described absorption plant is sampled constant volume, under 60 ℃～80 ℃ environment, carry out.
In the method for the invention, employed absorption plant is the absorption plant of a band insulation jacket, is filled with 60 ℃～80 ℃ water in insulation jacket.
Described absorption plant includes pipe in the sampling constant volume, and the volume of pipe is 100 ± 0.1ml in the described sampling constant volume, and the scale mark of 95.0-100.0ml is carved with at thin neck place, and scale division value is 0.01ml.
In the method for the invention, employed aqueous slkali is NaOH or KOH solution.
The inventive method is to high-purity SO
3Gas reaches wherein impurity SO
2During the gas concentration joint-detection, during sampling, absorption plant remains on poly-sample under 60 ℃～80 ℃ environment, has avoided SO
3The liquefaction of gas.The related material price of method of the present invention is low and easy and simple to handle, detects high-purity SO
3The precision of measurement of gas is good, and the measurement standard deviation is not more than 0.1%.The inventive method can be used for high-purity SO
3Gas detection is specially adapted to contain a small amount of SO
2The high-purity SO of gas and inert gas
3The detection of gas.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below further set forth the present invention.
High-purity SO
3Reach wherein impurity SO
3The detection method of gas concentration, the absorption plant that this method adopts are the glass device of sampling, constant volume and the absorption of a band insulation jacket.This device includes pipe in the sampling constant volume, and the volume of pipe is 100 ± 0.1ml in the sampling constant volume, and the scale mark of 95.0-100.0ml is carved with at thin neck place, and scale division value is 0.01ml.
As high-purity SO
3Gas reaches wherein impurity SO
2When gas installed by this, the temperature in the control external insulation chuck was 60 ℃～80 ℃; As in insulation jacket, being filled with 60 ℃～80 ℃ water.And make high-purity SO under positive pressure
3Gas reaches wherein impurity SO
2After gas is fully replaced in the pipe, close the import and export tap of pipe in the sampling constant volume in the sampling constant volume, and rapidly rotating gas outlet tap, make pipe internal pressure and atmospheric equilibrium in the constant volume of sampling.To sample then, pipe connects the leveling bottle that fills 200ml0.5mol/LNaOH solution in the constant volume, slowly opens tap after driving residual bubble out of, makes NaOH solution and the interior SO of absorption tube in the leveling bottle
3Gas and SO
2Gas reacts, and reaction mechanism is as follows:
SO
3+2NaOH＝Ns
2SO
4+H
2O (1)
SO
2+2NaOH＝Na
2SO
4+H
2O (2)
Constantly shake absorption bottle, make fully to absorb, after liquid level is chosen same level in leveling bottle and the absorption tube, read the scale V of absorption liquid liquid level
0Because SO
3, SO
2But with the NaOH complete reaction, so this volume V
0Be SO
3With SO
2The cumulative volume percentage concentration of mixed gas.
NaOH absorption liquid in the absorption bottle and the NaOH solution in the leveling bottle are transferred in the volumetric flask of 250ml together, fully clean remain in the absorbent solution of wall after, be settled to mixing in the 250ml volumetric flask, standby to detect SO
2The volumetric concentration of gas.
The absorbent solution of drawing 25ml in the 250ml volumetric flask drips 2-3 and drips phenolphthalein indicator to Erlenmeyer flask, with the H of 0.5mol/L
2SO
4Standard titration solution drips to being become colorless by redness.Its reaction mechanism is;
2NaOH+H
2SO
4＝Na
2SO
4+2H
2O (3)
The solution that above-mentioned drop reaction is intact is used the I of 0.01mol/L again
2Standard titration solution carries out titration, and the sulfaminic acid that adds 1ml40% is as screening agent, to avoid oxides of nitrogen (NOx) in the gas to the interference of titration end-point.Drip the 1ml starch indicator and make sample solution extremely light blue, write down the I of consumption by colourless titration
2The consumption of standard solution is done blank test.Its reaction mechanism is:
Na
2SO
3+I
2+H
2O＝Na
2SO
4+2HI (4)
Calculate SO
2Volumetric concentration, according to formula:
SO
3(V/V)％＝V
0-SO
2(V/V)％
Above-mentioned detection method is a kind of high-purity SO
3The detection method of gas, but the small amount of impurities SO that the while joint-detection is carried secretly
2Gas.Wherein, used alkali lye removes NaOH, can also be KOH.
The preferred temperature of absorption plant insulation jacket part is 60 ℃～80 ℃ in the above-mentioned detection method.
Wherein, CI
2---standard iodine solution amount of substance concentration, mol/L;
V
12---the consumption of standard iodine solution, ml;
V
Blank---the standard iodine liquid measure that sample blank consumes, mL;
10.945---under the standard state, with I
2Suitable SO
2The shared volume of amount of substance, L;
The sampling quantity of V---gas, mL;
P---the atmospheric pressure during operation, Pa;
P
0---the atmospheric pressure under the standard state, Pa;
T
0---absolute temperature, 273 ℃ of constants;
The temperature of t---gaseous sample, ℃.
Below by to carrying impurity SO secretly
2The high-purity SO of gas and inert gas
3The test experience of gas illustrates beneficial effect of the present invention.
Embodiment 1
Test is at 35 ℃ Celsius, and under the 1 atmospheric weather conditions, the temperature in the control insulation jacket is 70 ℃, and gas temperature is 70 ℃.The detection test findings is as follows:
Embodiment 2
Test is at 5 ℃ Celsius, and under the 1 atmospheric weather conditions, the temperature in the control insulation jacket is 70 ℃, and gas temperature is 70 ℃.The detection test findings is as follows:
According to the data and the standard deviation value of above gained, be presented under the stable situation of gas flow high-purity SO in this method
3Gas reaches wherein impurity SO
2The precision of measurement of gas volume percentage concentration is good, and the measurement standard deviation is not more than 0.1%.
Claims (3)
1. high-purity SO
3Gas reaches wherein impurity SO
2The method of gas concentration joint-detection comprises with absorption plant high-purity SO
3Gas reaches wherein impurity SO
2The gas constant volume of sampling absorbs with NaOH solution then, obtains high-purity SO
3Gas reaches wherein impurity SO
2The cumulative volume percentage concentration of gas is settled to 250ml to resulting NaOH absorption liquid again, gets the 25mlNaOH absorption liquid and drips phenolphthalein indicator to wherein dripping 2-3, uses 0.5mol/L H
2SO
4Standard titration solution drips to being become colorless by redness, and then adopts direct iodimetric titration to record SO
2The concentration expressed in percentage by volume of gas is with high-purity SO
3Gas reaches wherein impurity SO
2The cumulative volume percentage concentration of gas deducts SO
2The concentration expressed in percentage by volume of gas is high-purity SO
3Gas concentration, its spy is being, when described absorption plant is sampled constant volume, carries out under 60 ℃ of-80 ℃ of environment.
2. method according to claim 1 is characterized in that, employed absorption plant is the absorption plant of a band insulation jacket, is filled with 60 ℃-80 ℃ water in insulation jacket.
3. method according to claim 1 is characterized in that, described absorption plant includes pipe in the sampling constant volume, and the volume of pipe is 100 ± 0.1ml in the described sampling constant volume, and the scale mark of 95.0-100.0ml is carved with at thin neck place, and scale division value is 0.01ml.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610027779A CN100587487C (en) | 2006-06-19 | 2006-06-19 | Combined detection method for high-purity SO3 gas and impurity SO2 gas therein |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610027779A CN100587487C (en) | 2006-06-19 | 2006-06-19 | Combined detection method for high-purity SO3 gas and impurity SO2 gas therein |
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|---|---|
| CN1865993A CN1865993A (en) | 2006-11-22 |
| CN100587487C true CN100587487C (en) | 2010-02-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102359959A (en) * | 2011-06-24 | 2012-02-22 | 江苏龙源催化剂有限公司 | Method for determining sulfur dioxide oxidation rate of selective catalytic reduction denitration catalyst |
| CN103472061B (en) * | 2013-08-27 | 2016-05-04 | 浙江大学 | The on-line measuring device of sulfur trioxide and method in a kind of flue gas |
| CN104090078B (en) * | 2014-07-17 | 2016-02-10 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | A kind of method and system measuring sulfur dioxide in flue gas and sulfuric anhydride |
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Non-Patent Citations (4)
| Title |
|---|
| "沸腾脱硫炉气中二氧化硫和三氧化硫的测定". 石志圣，谭清云.分析实验室，第1983年卷第02期. 1983 |
| "沸腾脱硫炉气中二氧化硫和三氧化硫的测定". 石志圣，谭清云.分析实验室，第1983年卷第02期. 1983 * |
| 沸腾炉气中二氧化硫和三氧化硫的快速分析. 石志圣，谭清云.冶金分析，第1983卷第01期. 1983 |
| 沸腾炉气中二氧化硫和三氧化硫的快速分析. 石志圣，谭清云.冶金分析，第1983卷第01期. 1983 * |
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