CN102384936A - Method for determining hydrogen sulfide concentration in liquid sulfur - Google Patents
Method for determining hydrogen sulfide concentration in liquid sulfur Download PDFInfo
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- CN102384936A CN102384936A CN2010102666589A CN201010266658A CN102384936A CN 102384936 A CN102384936 A CN 102384936A CN 2010102666589 A CN2010102666589 A CN 2010102666589A CN 201010266658 A CN201010266658 A CN 201010266658A CN 102384936 A CN102384936 A CN 102384936A
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Abstract
The invention relates to a method for determining the hydrogen sulfide concentration in liquid sulfur, which comprises the following steps that: M gramme of proper sulfur products are weighed by a dried aspirator bottle, diisopropanolamine is correspondingly added, the aspirator bottle is placed into hot oil for oil bath steam extraction, nitrogen gas is added for stirring, flushing liquid is collected, silver nitrate solution is used for titration, the consumption volume of silver nitrate standard solution and the level value of an automatic potentiostat are recorded, the level value read during each time of titration and the milliliter number of the consumed silver nitrate standard solution are used for making a standard curve pattern, the middle point of the part with the maximum standard curve radian value change is used as a terminal titration point, the volume V of the silver nitrate consumed by the titration is obtained, and the hydrogen sulfide content in the liquid sulfur can be obtained through calculation. The method has the advantages that the diisopropanolamine is adopted for promoting the resolution of the hydrogen sulfide in the liquid sulfur, the steam extraction time is shortened to less than 0.5hour from the original 4hours, in addition, the hydrogen sulfide content is worked out according to the titration volume, the method is simple, and the detecting results are accurate and reliable.
Description
Technical field
The present invention relates to concentration of hydrogen sulfide determination method in a kind of molten sulfur, belong to the technical field of measuring concentration of hydrogen sulfide in the molten sulfur in the petrochemical complex production
Background technology
are at present in handling the natural gas conditioning process; Need carry out desulfurization to rock gas handles; The liquid sulfur of deviating from requires the hydrogen sulfide content in the molten sulfur to be controlled at below the 10PPM, otherwise will produce unfavorable factors such as equipment corrosion and the product sulphur that dispatches from the factory is defective.In order to measure the content of sulfuretted hydrogen in the molten sulfur, (the BLACK & of U.S. BV company; VEAPCH COMPANY) invented concentration of hydrogen sulfide determination method in a kind of molten sulfur.The operation steps and the technological process of this method are: ⑴, take by weighing a certain amount of sulphur sample with dried round-bottomed flask, put into heating jacket and heat; ⑵, overflowing for the gas that prevents sulfur-bearing in the molten sulfur, connect one in the exit and connect conical flask, is the iodine standard solution that moves into 20ml in advance with transfer pipet in the conical flask., treat that sulphur dissolves after, temperature control molten sulfur temperature blasts nitrogen or helium and carries out stripping 30min at 150 ℃; ⑷, extremely faint yellow with the sodium thiosulfate standard solution volumetric soiutions of 0.1mol/L, the record related data; ⑸, add the starch solution (10g/L) of 1～2ml again, with sodium thiosulfate standard solution volumetric soiutions to the colourless terminal point that is of 0.1mol/L, the record related data; ⑹, repetitive process 2 and process 3 again require process 3 to blast N2 or He carries out stripping 90min; Carry out the titration work of process 4 and process 5 again; ⑺, repetitive process 2 and process 3 again require process 3 to blast nitrogen or helium carries out stripping 120min; Carry out the titration work of process 4 and process 5 again; ⑻ the iodine loss in evaporation and the suction process is proofreaied and correct in, employing " blank "; , with stripping time of accumulative total hydrogen sulfide content (ppm (wt)) and accumulative total (hour) make a semilogarithmic plot, hydrogen sulfide content (ppm (wt)) in the extrapolation molten sulfur.This analytical approach heats in heating jacket; There are sample insulation, constant temperature difficulty; And whole operation needs 9 hours at least; Analysis time is oversize, adopts blank iodine loss and a semilogarithmic plot of the standard of employing of proofreading and correct in evaporation and the suction process, the not high shortcoming of accurate rate of hydrogen sulfide content in the molten sulfur of extrapolating.
The patent No. is 200810305539.2 to disclose hydrogen sulfide content device in crude oil in a kind of measuring channel, the rock gas, because molten sulfur compares with original that to have high temperature be that liquid, low temperature solidifies, this device can't satisfy the mensuration of sulfuretted hydrogen in the molten sulfur
Summary of the invention
the present invention seeks to the insulation that exists in the above-mentioned prior art, constant temperature difficulty; Operation, analysis time is long; The not high shortcoming of result of calculation accurate rate; A kind of smooth operation is provided, reduces the working time, concentration of hydrogen sulfide determination method in the molten sulfur of raising measurement data accurate rate.
Operation steps of the present invention is following:
⑴, take by weighing an amount of sulphur sample M gram with dried Drexel bottle, corresponding adding diisopropanolamine places deep fat to carry out the oil bath stripping Drexel bottle;
⑵, connecting conical flask in the Drexel bottle exit, is to move into an amount of iodine standard solution with transfer pipet in advance in the conical flask;
, treat that sulphur dissolves after, in Drexel bottle, add nitrogen and stir;
⑷, dismantle Drexel bottle and stop stripping, collect washing fluid;
, in the buret liquor argenti nitratis ophthalmicus of dress finite concentration C, under buret mouth of pipe immersed in liquid level, an amount of strong aqua of adding in the beaker, and put into the magnetic stirrer electrode is immersed absorption liquid stirs;
⑹, carry out titration by automatic potentiometer, every titration is once treated the volume that the stable back of current potential record silver nitrate standard solution consumes and the potential value of potentiometer automatically;
⑺, repeating step ⑹ make canonical plotting by the potential value that each titration is read with consumption silver nitrate standard solution milliliter number;
⑻, choice criteria curve radian value change the mid point of largest portion and make titration end-point, obtain the liquor argenti nitratis ophthalmicus volume V that titration consumes;
⑼ the hydrogen sulfide content in, the molten sulfur (ppm (wt)) is by computes:
In the formula: V-liquor argenti nitratis ophthalmicus volume, milliliter;
C-liquor argenti nitratis ophthalmicus concentration, mole/milliliter;
The quality of
M-sample, gram.
the present invention adopts diisopropanolamine to promote the parsing of sulfuretted hydrogen in the molten sulfur; The stripping time shortened to less than 0.5 hour by original 4 hours, and titration method is by manually changing automatic potentiometer titration into, and titration data accurately, rationally; Simultaneously; Calculate hydrogen sulfide content according to the titration volumescope, method is simplified, and calculation rationally accurately.
Embodiment:
Embodiment one:
, with dried Drexel bottle take by weighing 100 the gram the sulphur sample, the diisopropanolamine that corresponding adding is 90 milligrams places 130 ℃ deep fat to carry out oil bath Drexel bottle, the oil bath time is 20 minutes;
⑵, overflowing for the gas that prevents sulfur-bearing in the molten sulfur, connect one in the Drexel bottle exit and connect conical flask, is to move into 20 milliliter 15% iodine standard solution in advance with transfer pipet in the conical flask;
, treat that sulphur dissolves after, in Drexel bottle, add nitrogen and stir, the adjustment flow is 500 ml/min, carries out stripping 30 minutes;
⑷, dismantle that Drexel bottle is whole to be stopped gas and carry.Receive socket and pipeline and use distilled water flushing, collect washing fluid;
⑸, dress concentration is 0.01 mole/milliliter liquor argenti nitratis ophthalmicus in the buret; In beaker, add 5 milliliters of strong aquas. put into the magnetic stirrer electrode is immersed absorption liquid; Under titration tip immersed in liquid level. the adjustment stirring rate, to produce strong agitation but do not spill to good;
⑹, carry out titration, after every titration once, treat that the stable back of current potential record vs consumes volume and instrument readings,, can think that current potential is stable when current potential reading amplitude of variation during less than 6 millivolts/minute at automatic potentiometer.
⑺, repeating step ⑹ are+100 millivolts until the current potential reading, make canonical plotting by the potential value that each titration is read with consumption silver nitrate standard solution milliliter number;
⑻, choice criteria curve radian value change the mid point of largest portion and make titration end-point;
, with formula (
) calculate the hydrogen sulfide content (ppm (wt)) in the molten sulfur.
Embodiment two:
The operation steps that embodiment two is carried out is identical with the operation steps that embodiment one is carried out, and the sulphur sample size described in the step is 100 grams, 100 milligrams of diisopropanolamine additions;
Described oil bath temperature is 140 ℃, and the oil bath time is 20 minutes;
Described iodine standard solution is 20%, and volume is 15 milliliters;
The concentration of
described liquor argenti nitratis ophthalmicus is: 0.008 mole/milliliter.
Embodiment three:
The operation steps that embodiment three is carried out is identical with the operation steps that embodiment one is carried out, and the sulphur sample size described in the step is 100 grams, 110 milligrams of diisopropanolamine additions;
Described oil bath temperature is 150 ℃, and the oil bath time is 30 minutes;
Described iodine standard solution is 18%, and volume is 20 milliliters;
The concentration of described liquor argenti nitratis ophthalmicus is: 0.012 mole/milliliter
Claims (5)
1.
Concentration of hydrogen sulfide determination method in a kind of molten sulfur is characterized in that comprising the steps:
⑴, take by weighing an amount of sulphur sample M gram with dried Drexel bottle, corresponding adding diisopropanolamine places deep fat to carry out the oil bath stripping Drexel bottle;
⑵, connecting conical flask in the Drexel bottle exit, is to move into an amount of iodine standard solution with transfer pipet in advance in the conical flask;
, treat that sulphur dissolves after, in Drexel bottle, add nitrogen and stir;
⑷, dismantle Drexel bottle and stop stripping, collect washing fluid;
, in the buret liquor argenti nitratis ophthalmicus of dress finite concentration C, under buret mouth of pipe immersed in liquid level, an amount of strong aqua of adding in the beaker, and put into the magnetic stirrer electrode is immersed absorption liquid stirs;
⑹, carry out titration by automatic potentiometer, every titration is once treated the volume that the stable back of current potential record silver nitrate standard solution consumes and the potential value of potentiometer automatically;
⑺, repeating step ⑹ make canonical plotting by the potential value that each titration is read with consumption silver nitrate standard solution milliliter number;
⑻, choice criteria curve radian value change the mid point of largest portion and make titration end-point, obtain the liquor argenti nitratis ophthalmicus volume V that titration consumes;
⑼ the hydrogen sulfide content in, the molten sulfur (ppm (wt)) is by computes:
In the formula: V-liquor argenti nitratis ophthalmicus volume, milliliter;
C-liquor argenti nitratis ophthalmicus concentration, mole/milliliter;
The quality of
M-sample, gram.
2. concentration of hydrogen sulfide determination method in
molten sulfur according to claim 1, it is characterized in that: the sulphur sample that takes by weighing and the mass ratio of diisopropanolamine are: 900～1100:1.
3. concentration of hydrogen sulfide determination method in
molten sulfur according to claim 1 and 2, it is characterized in that: the temperature of Drexel bottle oil bath in deep fat is: 130～150 ℃; The oil bath time is: 20～30 minutes.
4. concentration of hydrogen sulfide determination method in
molten sulfur according to claim 3, it is characterized in that: the concentration range of iodine standard solution is: 15%～20%, the addition scope is: 15～25 milliliters.
5. concentration of hydrogen sulfide determination method in
molten sulfur according to claim 1 and 2, it is characterized in that: the concentration range of liquor argenti nitratis ophthalmicus is: 0.008～0.012 mole/milliliter.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866219A (en) * | 2016-04-26 | 2016-08-17 | 重庆鹏凯精细化工有限公司 | Quick determination method for sodium chloride content in ethoxyl/hydroxypropyl methyl cellulose |
| CN111474291A (en) * | 2019-01-23 | 2020-07-31 | 中国石油天然气股份有限公司 | Catalyst chemical determination method for total hydrogen sulfide content in liquid sulfur |
| CN111504938A (en) * | 2019-01-30 | 2020-08-07 | 中国石油天然气股份有限公司 | Method for measuring total hydrogen sulfide content in liquid sulfur |
| CN114486800A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Method for measuring content of hydrogen sulfide in liquid sulfur and method for measuring initial content of hydrogen polysulfide in liquid sulfur |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1887406A (en) * | 2005-06-27 | 2007-01-03 | 成都华西化工研究所 | Solvent for eliminating H2S from gas mixture |
| CN101403686A (en) * | 2008-11-13 | 2009-04-08 | 新疆石油管理局试油公司 | Apparatus for measuring hydrogen sulphide content in crude oil and natural gas in pipe |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1887406A (en) * | 2005-06-27 | 2007-01-03 | 成都华西化工研究所 | Solvent for eliminating H2S from gas mixture |
| CN101403686A (en) * | 2008-11-13 | 2009-04-08 | 新疆石油管理局试油公司 | Apparatus for measuring hydrogen sulphide content in crude oil and natural gas in pipe |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866219A (en) * | 2016-04-26 | 2016-08-17 | 重庆鹏凯精细化工有限公司 | Quick determination method for sodium chloride content in ethoxyl/hydroxypropyl methyl cellulose |
| CN111474291A (en) * | 2019-01-23 | 2020-07-31 | 中国石油天然气股份有限公司 | Catalyst chemical determination method for total hydrogen sulfide content in liquid sulfur |
| CN111474291B (en) * | 2019-01-23 | 2022-08-30 | 中国石油天然气股份有限公司 | Catalyst chemical determination method for total hydrogen sulfide content in liquid sulfur |
| CN111504938A (en) * | 2019-01-30 | 2020-08-07 | 中国石油天然气股份有限公司 | Method for measuring total hydrogen sulfide content in liquid sulfur |
| CN114486800A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Method for measuring content of hydrogen sulfide in liquid sulfur and method for measuring initial content of hydrogen polysulfide in liquid sulfur |
| CN114486800B (en) * | 2020-10-27 | 2024-04-26 | 中国石油化工股份有限公司 | Method for measuring content of hydrogen sulfide in liquid sulfur and method for measuring initial content of hydrogen polysulfide in liquid sulfur |
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