CN102967565A - Method for measuring tar content in gas - Google Patents
Method for measuring tar content in gas Download PDFInfo
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- CN102967565A CN102967565A CN2012104433794A CN201210443379A CN102967565A CN 102967565 A CN102967565 A CN 102967565A CN 2012104433794 A CN2012104433794 A CN 2012104433794A CN 201210443379 A CN201210443379 A CN 201210443379A CN 102967565 A CN102967565 A CN 102967565A
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Abstract
The invention provides a method for measuring tar content in gas. The method for measuring tar content in gas comprises the steps of putting gas into a surge flask at a flow speed of 3.5-4 L/min to be buffered, enabling the gas to enter into an absorption flask filled with an absorbent, absorbing tar in the gas by the absorbent, carrying out centrifugal separation at a rotating speed of 40-50r/m to separate a sample oil layer and a water layer, putting the sample oil layer into a cuvette, and measuring a light absorption value A1 of the sample oil layer at the wavelength of 32nm to obtain the tar content in the gas. The method for measuring tar content in gas can conveniently adjust and control the operation situations of an electrical tar precipitator in time, and efficiently solve the problems of the desulfurizing liquid emulsification, the reduction of the desulfurizing liquid oxidation and regeneration capabilities, the reduction of the desulfurization degree and the like caused by high tar content in the gas, thereby ensuring subsequent processes to be carried out smoothly, and meeting production control requirements.
Description
Technical field
The present invention relates to the assay method of tar content in a kind of coal gas, belong to the analysis and testing technology field.
Background technology
In the coal tar chemical industry was produced, raw gas need to pass through condensation air blast operation, made most of tar be recycled ammonia absorption and condensation is got off, the formation tar product; And small part tar can be carried secretly by coal gas and enters electrical tar precipitator, (requires that tar content should be less than 50mg/m in the coal gas this moment through further removing wherein tar
3) after, could create conditions for post-order process production.In case during the tar content superelevation, can cause emulsification to doctor solution in the coal gas, directly affect doctor solution oxidation regeneration ability, reduce desulfuration efficiency.Therefore, must carry out Accurate Determining to tar content in the coal gas, with the operation conditions of monitoring electrical tar precipitator.Yet prior art is measured the tar in the combustion gas, does not but provide more applicable analytical approach, has directly affected post-order process production.Therefore, must be improved prior art.
Summary of the invention
For promptly and accurately measuring tar content in the coal gas, satisfy the production control needs, the invention provides the assay method of tar content in a kind of coal gas.
The invention provides the assay method of tar content in a kind of coal gas, it is characterized in that comprising the following steps:
1) flow velocity of coal gas with 3.5-4 liter/min of clock passed in the surge flask, after alleviating, enter in the absorption bottle of in-built absorbing agent, by the tar in the absorbing agent absorption coal gas, until the coal gas amount that passes into reaches setting value;
2) with the absorbing agent that is absorbed with tar of step 1), carry out centrifuging with 40～50 rev/mins rotating speeds, isolate oil reservoir sample and water layer;
3) get step 2) the oil reservoir sample in cuvette, at wavelength 320nm place, measure the light absorption value A of this oil reservoir sample
1, simultaneously take pure absorbing agent as reference, measure blank absorbency A
0, draw the actual light absorption value A=A of this oil reservoir sample
1-A
0
4) with the following regression equation calculation of the light absorption value of step 3), namely obtain the tar content of this oil reservoir sample: A=km+b;
In the formula:
A: the light absorption value A=A of oil reservoir sample
I-A
0
M: oil reservoir sample content, mg;
K: according to test condition, the slope of standard curve that calculates through recurrence;
B: according to test condition, the typical curve intercept that calculates through recurrence;
5) the tar content m that step 4) is obtained calculates with following formula, namely obtains the tar content m ˊ in the coal gas under the status of criterion;
Tar content m ˊ (mg/m in the coal gas under the status of criterion
3)=m ÷ (V * K) * 1000
In the formula, the tar content (milligram) in the coal gas of m-tried to achieve by regression equation,
V-sample volume (liter)
K-the be scaled to coal gas volume factor under the status of criterion.
The regression equation A=km+b of described step 4) obtains through following method: with a plurality of different content m
IThe standard tar-like, use respectively 721 spectrophotometers, at wavelength 320nm place, record the value light absorption value A of each standard tar-like
I, simultaneously take pure absorbing agent as reference, measure blank absorbency A
0, the light absorption value A=A of standard tar-like then
I-A
0, with the content m of each standard tar-like
IBe horizontal ordinate, the light absorption value A of each standard tar-like is ordinate, drawing standard tar absorption curve, and calculate regression equation: A=km+b.
Described absorbing agent is the pure dimethylbenzene of commercial analysis.
Described 721 spectrophotometrics are counted commercial product.
The present invention compared with prior art has following advantages and effect: adopt such scheme, can make things convenient for, the tar content in the Accurate Determining coal gas, in order in time regulate and control the operation conditions of postorder electrical tar precipitator, efficiently solve because of tar content height in the coal gas, and the doctor solution emulsification that causes reduces doctor solution oxidation regeneration ability, reduces the problems such as desulfurization degree, guarantee carrying out smoothly of post-order process, satisfy the production control needs.
Description of drawings
Fig. 1 is gas sampling apparatus structure synoptic diagram of the present invention.
Among the figure, 1 is gas main, and 2 is operation valve, and 3 are the sampling arm, and 4 is connecting leg, and 5 is gas outlet, and 6 is gas meter, and 7 is absorption bottle, and 8 is surge flask.
Embodiment
1, the making of standard tar absorption curve
1.1 the preparation of standard tar-like
Get commercial tar product, use routinely xylene soluble, extraction, separating layer after, the dimethylbenzene layer is moved in the 250nml beaker, with beaker be placed on be evaporated on the water-bath remove dimethylbenzene after, beaker is put into 140 ℃ dry 1 hour of thermostatic drying chamber, get the standard tar-like, for subsequent use;
1.2 the preparation of standard color solution and production standard curve
1.2.1 take by weighing 0.1g step 1.1 gained standard tar-like in the 30ml beaker, after an amount of xylene soluble, put into the drying bottle of 100ml capacity, wash beaker 3-4 times with an amount of dimethylbenzene, cleansing solution is incorporated in the 100ml volumetric flask, be settled to 100ml with dimethylbenzene again, the concentration of this standard solution is 1mg/ml;
1.2.2 get respectively step 1.2.1 gained standard solution 0.5ml, 1ml, 2ml, 3ml, 4ml, put into respectively 25 milliliters of color comparison tubes with stopper, be settled to the 25ml scale mark with dimethylbenzene, cover tightly stopper, shake up, obtain five standard tar-like that content is different, the corresponding content m of each standard tar-like
IBe respectively 0.5mg, 1 mg, 2 mg, 3 mg, 4 mg;
1.2.3 on 721 spectrophotometers of routine, at wavelength 320nm place, use the respectively light absorption value A of five standard tar-like of measuring process 1.2.2 of 1cm cuvette
I(i is from 1～5 herein), and make reference with dimethylbenzene and measure blank sample light absorption value A without tar
0, deduct the actual light absorption value A=A of sample behind the blank sample light absorption value
I-A
0
1.2.4 with each tar content m
IBe horizontal ordinate, corresponding light absorption value A is ordinate, the drawing standard curve, and obtain regression equation, and A=km+b, according to test condition, this regression equation is: A=0.1041m+0.009, wherein:
A: for deducting the standard tar light absorption value behind the blank sample light absorption value, A=A
I-A
0
M: the content of standard tar, mg;
K: be constant 0.1041, the slope of standard curve that calculates through recurrence;
B: be constant 0.009, the typical curve intercept that calculates through recurrence;
The standard tar content the results are shown in following table:
2, the mensuration of tar content in the coal gas
2.1 the flow velocity of the coal gas before the electrical tar precipitator with 3.5 liter/mins of clocks passed in the surge flask 8, after releasing the pressure, be equipped with in entering in the 30ml absorption bottle 7 of 25ml dimethylbenzene, to absorb the tar in the coal gas by dimethylbenzene, until the coal gas amount that passes into reaches 20 liters, must be absorbed with the dimethylbenzene of tar;
2.2 step 2.1 gained is absorbed with the dimethylbenzene of tar, carry out centrifuging with 40 rev/mins rotating speeds, isolate oil reservoir sample and water layer, take out the oil reservoir sample;
2.3 get the oil reservoir sample of step 2.2 in the 1cm cuvette, at wavelength 320nm place, measure the light absorption value A of this oil reservoir sample
1Be 0.267, simultaneously take dimethylbenzene as reference, measure the blank dimethylbenzene light absorption value A without tar
0Be 0.004, deduct blank sample light absorption value after, the light absorption value A of this oil reservoir sample is 0.263;
2.4 in step 2.3 gained light absorption value A substitution regression equation A=0.1041m+0.009, draw that tar content m is 2.44mg in the coal gas;
(2) be converted to tar content m ˊ in the coal gas under the status of criterion:
Tar content m ˊ=m ÷ in the coal gas under the status of criterion (V * K) * 1000
=?166.9?mg/m
3；
Following formula is: 2.44 mg ÷ (20 liters * 0.7308) * 1000 liters/m
3=166.9 mg/m
3, gas temperature is 17 ℃ during sampling, and atmospheric pressure is 604.5mmHg, and the COEFFICIENT K that is scaled under the standard state is 0.7308.
Embodiment 2
1, the making of standard tar absorption curve is with embodiment 1.
2, the mensuration of tar content in the coal gas
2.1 the flow velocity of the coal gas behind the electrical tar precipitator with 4 liter/mins of clocks passed in the surge flask 8, after releasing the pressure, be equipped with in entering in the 30ml absorption bottle 7 of 25ml dimethylbenzene, to absorb the tar in the coal gas by dimethylbenzene, until the coal gas amount that passes into reaches 20 liters, must be absorbed with the dimethylbenzene of tar;
2.2 step 2.1 gained is absorbed with the dimethylbenzene of tar, carry out centrifuging with 50 rev/mins rotating speeds, isolate oil reservoir sample and water layer, take out the oil reservoir sample;
2.3 get the oil reservoir sample of step 2.2 in the 1cm cuvette, at wavelength 320nm place, measure the light absorption value A of this oil reservoir sample
1Be 0.105, simultaneously take dimethylbenzene as reference, measure the blank dimethylbenzene light absorption value A without tar
0Be 0.004, deduct blank sample light absorption value after, the light absorption value A of this oil reservoir sample is 0.101
0
2.4 in step 2.3 gained light absorption value A substitution regression equation A=0.1041m+0.009, draw under the operating mode that tar content m is 0.88 mg in the coal gas;
(2) tar content m ˊ in the coal gas after gas sampling volume under the operating mode being converted under the status of criterion:
Tar content m ˊ=m ÷ in the coal gas under the status of criterion (V * K) * 1000
=58.6?mg/m
3；
Following formula is: 0.88 mg ÷ (20 liters * 0.7507) * 1000 liters/m
3=58.6mg/m
3Gas temperature is 27 ℃ during sampling, and atmospheric pressure is 602.25mmHg, and the COEFFICIENT K that is scaled under the standard state is 0.7507.
By the practical application of the inventive method, be 166.9 mg/m to the measured value of tar content in the coal gas before the electrical tar precipitator of people coke-oven plant
3, be 58.6 mg/m to the measured value through tar content in the coal gas behind the electrical tar precipitator capture tar
3, the tar arresting efficiency that obtains thus this electrical tar precipitator is 65%, and is normal.
Claims (2)
1. the assay method of tar content in the coal gas is characterized in that comprising the following steps:
1) flow velocity of coal gas with 3.5-4 liter/min of clock passed in the surge flask, after alleviating, enter in the absorption bottle of in-built absorbing agent, by the tar in the absorbing agent absorption coal gas, until the coal gas amount that passes into reaches setting value;
2) with the absorbing agent that is absorbed with tar of step 1), carry out centrifuging with 40～50 rev/mins rotating speeds, isolate oil reservoir sample and water layer;
3) get step 2) the oil reservoir sample in cuvette, at wavelength 320nm place, measure the light absorption value A of this oil reservoir sample
1, simultaneously take pure absorbing agent as reference, measure blank absorbency A
0, draw the actual light absorption value A=A of this oil reservoir sample
1-A
0
4) with the following regression equation calculation of the light absorption value of step 3), namely obtain the tar content of this oil reservoir sample: A=km+b;
In the formula:
A: the light absorption value A=A of oil reservoir sample
I-A
0
M: oil reservoir sample content, mg;
K: according to test condition, the slope of standard curve that calculates through recurrence;
B: according to test condition, the typical curve intercept that calculates through recurrence;
5) the tar content m that step 4) is obtained calculates with following formula, namely obtains the tar content m ˊ in the coal gas under the status of criterion;
Tar content m ˊ (mg/m in the coal gas under the status of criterion
3)=m ÷ (V * K) * 1000
In the formula, the tar content (milligram) in the coal gas of m-tried to achieve by regression equation,
V-sample volume (liter)
K-the be scaled to coal gas volume factor under the status of criterion.
2. the assay method of tar content in the coal gas as claimed in claim 1 is characterized in that described absorbing agent is the pure dimethylbenzene of commercial analysis.
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|---|---|---|---|
| CN2012104433794A CN102967565A (en) | 2012-11-08 | 2012-11-08 | Method for measuring tar content in gas |
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|---|---|---|---|
| CN2012104433794A CN102967565A (en) | 2012-11-08 | 2012-11-08 | Method for measuring tar content in gas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106997216A (en) * | 2017-05-19 | 2017-08-01 | 云南中烟工业有限责任公司 | A kind of constant pressure storehouse of cigarette smoking machine and its method for suction experiment |
| CN107238549A (en) * | 2017-06-23 | 2017-10-10 | 华中师范大学 | A kind of assay method for the tar in gas content that biomass pyrolytic is produced |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038355A (en) * | 1988-02-05 | 1989-12-27 | 米德公司 | Developer composition |
| EP1203942B1 (en) * | 2000-11-02 | 2007-09-05 | Schlumberger Holdings Limited | Methods and apparatus for optically measuring fluid compressibility downhole |
-
2012
- 2012-11-08 CN CN2012104433794A patent/CN102967565A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1038355A (en) * | 1988-02-05 | 1989-12-27 | 米德公司 | Developer composition |
| EP1203942B1 (en) * | 2000-11-02 | 2007-09-05 | Schlumberger Holdings Limited | Methods and apparatus for optically measuring fluid compressibility downhole |
Non-Patent Citations (2)
| Title |
|---|
| 张仲琼: "紫外分光光度法测定煤气中的焦油含量", 《燃料与化工》, vol. 38, no. 5, 30 September 2007 (2007-09-30) * |
| 张琼芳: "循环氨水中焦油含量的测定", 《燃料与化工》, vol. 35, no. 5, 30 September 2004 (2004-09-30) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106997216A (en) * | 2017-05-19 | 2017-08-01 | 云南中烟工业有限责任公司 | A kind of constant pressure storehouse of cigarette smoking machine and its method for suction experiment |
| CN107238549A (en) * | 2017-06-23 | 2017-10-10 | 华中师范大学 | A kind of assay method for the tar in gas content that biomass pyrolytic is produced |
| CN107238549B (en) * | 2017-06-23 | 2020-01-14 | 华中师范大学 | Method for measuring tar content in gas generated by biomass pyrolysis |
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Application publication date: 20130313 |