CN109613173A - A kind of method that constant-current titration measures mercaptan sulfur in gas - Google Patents
A kind of method that constant-current titration measures mercaptan sulfur in gas Download PDFInfo
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- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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Abstract
The invention discloses the methods of mercaptan sulfur in a kind of constant-current titration measurement gas, it is characterized in that, sample air passes through flashing gasified sampling-fetching device for liquid hydrocarbon, accurate control gas flow rate and gasification temperature, accurate metering absorbs gas volume, the mercaptan sulfur in gas is absorbed with 40% potassium hydroxide solution, with the content of mercaptan sulfur in optimization potentiometric determination absorbing liquid.Flashing gasified sampling-fetching device for liquid hydrocarbon is used to replace wet flow indicator by this method, keep flow control, gasification temperature control and gas metered volume more accurate, by optimizing constant-current titration method, it is precisely controlled titration liquid feeding speed and titration volumes, keep drop reaction more complete, titration end-point judges sensitive, curve perfection, and analysis result accuracy is high.
Description
Technical field
The present invention relates to constant-current titration method fields, and in particular to a kind of constant-current titration measures the side of mercaptan sulfur in gas
Method.
Background technique
The content of liquefied gas mercaptan sulfur is important indicator of the evaluation as fuel service performance after measurement purification.Because of sulphur
The presence of alcohol can not only make liquefied gas have special penetrating odor, can also be changed into toxic, corrosive dioxy in burning
Change sulphur and sulfur trioxide, atmosphere can be polluted in storage, shipment and use.In refinery production, liquefied gas is as deep after purification
It processes raw material, the Con trolling index of mercaptans content is no more than 10ppm.Sulphur in actual production, after extracting is washed in double dealkalizes
Alcohol content only has several ppm or smaller sometimes.
Summary of the invention
In view of the deficienciess of the prior art, the technical problem to be solved by the present invention is to take liquid hydrocarbon is flash vaporized
Sample sample injector is used to replace wet flow indicator, keeps flow control, gasification temperature control and gas metered volume more accurate, passes through optimization electricity
Position titration method is precisely controlled titration liquid feeding speed and titration volumes, keeps drop reaction more complete, titration end-point judge it is sensitive,
Curve is perfect, and analysis result accuracy is high.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of constant-current titration measures sulphur in gas
The method of alcohol sulphur, which comprises the following steps:
(1) vulcanization of new electrode: ten thousand logical composite silver cap electrodes are placed in the sodium sulfide solution of 0.1mol/L and impregnate 1h, are taken
It is rinsed well out with deionized water, electrode silver ring becomes bright black at this time, is put into the electrode casing equipped with electrode protection liquid
In it is spare；
(2) preparation of sample: liquefied gas sampling steel cylinder to be measured is connect with flashing gasified sampling-fetching device for liquid hydrocarbon, gasification
Temperature is controlled at 100 DEG C, and gas flow rate is set as 2L/min, and the sample air after gasification is molten by being filled with appropriate saturated sodium carbonate
Enter the accurate absorption bottle that 40mL40% potassium hydroxide solution is housed after the surge flask of liquid, the volume of absorbed sample air is with liquid
The metering of total amount shown by state hydrocarbon flashing gasified sampling-fetching device, while recording ambient atmosphere pressure；
(3) analysis of sample: 1mol/L sodium hydroxide solution 30mL and 1mol/L ammonia spirit 2.0mL is taken to burn in 100mL
In cup, absorbing liquid 10mL then is drawn in same beaker with pipette.It opens ten thousand logical 809Titrando softwares and enters work
It stands, calls corresponding method, titration unit is connect with computer work, by ten thousand logical composite silver cap electrodes, blender and titrating head
It is rationally fixed, it is immersed in 100ml titrating beaker, starts to carry out automatic Titration, be calculated automatically after the completion of titration according to formula, put down
Row measurement 3 times, is averaged as testing result.
Preferably, the process of titration described in step (3) the following steps are included:
(1) preparation of 0.1mol/L silver nitrate isopropanol standard solution: dissolving 17g AgNO3 in 100mL distilled water, uses
Isopropanol is to 1L.In a brown bottle, calibration is primary weekly for storage.
(2) scaling method: measuring 60mL distilled water in 100mL beaker, and 5 drop nitric acid are added, boil 5min, to be cooled
2mL 0.1mol/L potassium iodide standard solution is accurately measured afterwards in same beaker, carries out current potential drop with silver nitrate alcohol standard solution
It is fixed, it titrates 3 times, calculates accurate molar concentration.
Preferably, the process of titration described in step (3) the following steps are included:
(1) preparation of 0.01mol/L silver nitrate isopropanol standard solution: 10mL0.1mol/L silver nitrate isopropanol mark is drawn
Quasi- solution is in 100mL brown volumetric flask, with isopropanol to groove.Calibration in every 3 days is primary, if it is necessary turbidity and precipitation occur
Separately match.
(2) scaling method: 1mL0.1mol/L potassium iodide standard solution accurately is pipetted in 100mL beaker, 50mL is added to distill
Water carries out constant-current titration with about 0.01mol/L silver nitrate alcohol standard solution is diluted to, titrates 3 times, accurate mole of calculating is dense
Degree.
Compared with prior art, the present invention have it is following the utility model has the advantages that
Flashing gasified sampling-fetching device for liquid hydrocarbon is used to replace wet flow indicator by the present invention, makes flow control, gasification temperature
Control and gas metered volume are more accurate, by optimizing constant-current titration method, using the DET-U step mode of advanced level user, precisely
Control titration liquid feeding speed and titration volumes, keep drop reaction more complete, and titration end-point judges sensitive, curve perfection, analysis knot
Fruit accuracy is high.
Detailed description of the invention
Fig. 1 is the enrichment concentration titration curve of gaseous sample mercaptan.
Fig. 2 is the automatic potentiometric titration curve that parameter optimization later group is measured in parallel.
Specific embodiment
Form by the following examples is described in further detail above content of the invention again, but should not be by this
The range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiment, all technologies based on realization belonging to above content of the present invention
It all belongs to the scope of the present invention.
Embodiment 1
A kind of method that constant-current titration measures mercaptan sulfur in gas, comprising the following steps:
(1) vulcanization of new electrode: ten thousand logical composite silver cap electrodes are placed in the sodium sulfide solution of 0.1mol/L and impregnate 1h, are taken
It is rinsed well out with deionized water, electrode silver ring becomes bright black at this time, is put into the electrode casing equipped with electrode protection liquid
In it is spare；
(2) preparation of sample: liquefied gas sampling steel cylinder to be measured is connect with flashing gasified sampling-fetching device for liquid hydrocarbon, gasification
Temperature is controlled at 100 DEG C, and gas flow rate is set as 2L/min, and the sample air after gasification is molten by being filled with appropriate saturated sodium carbonate
Enter the accurate absorption bottle that 40mL40% potassium hydroxide solution is housed after the surge flask of liquid, the volume of absorbed sample air is with liquid
The metering of total amount shown by state hydrocarbon flashing gasified sampling-fetching device, while recording ambient atmosphere pressure；
(3) analysis of sample: 1mol/L sodium hydroxide solution 30mL and 1mol/L ammonia spirit 2.0m L is taken to burn in 100mL
In cup, absorbing liquid 10mL then is drawn in same beaker with pipette.It opens ten thousand logical 80 9Titrando softwares and enters work
It stands, calls corresponding method, titration unit is connect with computer work, by ten thousand logical composite silver cap electrodes, blender and titrating head
It is rationally fixed, be immersed in 100ml titrating beaker, start to carry out automatic Titration, the process of titration the following steps are included:
(1) preparation of 0.1mol/L silver nitrate isopropanol standard solution: dissolving 17 g AgNO3 in 100mL distilled water,
With isopropanol to 1L.In a brown bottle, calibration is primary weekly for storage.
(2) scaling method: measuring 60mL distilled water in 100mL beaker, and 5 drop nitric acid are added, boil 5 min, to be cooled
2mL 0.1mol/L potassium iodide standard solution is accurately measured afterwards in same beaker, carries out current potential drop with silver nitrate alcohol standard solution
It is fixed, it titrates 3 times, calculates accurate molar concentration.
It is calculated automatically after the completion of titration according to formula, is measured in parallel 3 times, is averaged as testing result.
Embodiment 2
A kind of method that constant-current titration measures mercaptan sulfur in gas, comprising the following steps:
(1) vulcanization of new electrode: ten thousand logical composite silver cap electrodes are placed in the sodium sulfide solution of 0.1mol/L and impregnate 1h, are taken
It is rinsed well out with deionized water, electrode silver ring becomes bright black at this time, is put into the electrode casing equipped with electrode protection liquid
In it is spare；
(2) preparation of sample: liquefied gas sampling steel cylinder to be measured is connect with flashing gasified sampling-fetching device for liquid hydrocarbon, gasification
Temperature is controlled at 100 DEG C, and gas flow rate is set as 2L/min, and the sample air after gasification is molten by being filled with appropriate saturated sodium carbonate
Enter the accurate absorption bottle that 40% potassium hydroxide solution of 40mL is housed after the surge flask of liquid, the volume of absorbed sample air with
The metering of total amount shown by flashing gasified sampling-fetching device for liquid hydrocarbon, while recording ambient atmosphere pressure；
(3) analysis of sample: 1mol/L sodium hydroxide solution 30mL and 1mol/L ammonia spirit 2.0mL is taken to burn in 100mL
In cup, absorbing liquid 10mL then is drawn in same beaker with pipette.It opens ten thousand logical 809Titrando softwares and enters work
It stands, calls corresponding method, titration unit is connect with computer work, by ten thousand logical composite silver cap electrodes, blender and titrating head
It is rationally fixed, be immersed in 100ml titrating beaker, start to carry out automatic Titration, the process of titration the following steps are included:
(1) preparation of 0.01mol/L silver nitrate isopropanol standard solution: 10mL0.1mol/L silver nitrate isopropanol mark is drawn
Quasi- solution is in 100mL brown volumetric flask, with isopropanol to groove.Calibration in every 3 days is primary, if it is necessary turbidity and precipitation occur
Separately match.
(2) scaling method: 1mL0.1mol/L potassium iodide standard solution accurately is pipetted in 100mL beaker, 50mL is added to distill
Water carries out constant-current titration with about 0.01mol/L silver nitrate alcohol standard solution is diluted to, titrates 3 times, accurate mole of calculating is dense
Degree.
It is calculated automatically after the completion of titration according to formula, is measured in parallel 3 times, is averaged as testing result.
Test method
(1) metering, flow control and the temperature control of tested gas are carried out using flashing gasified sampling-fetching device for liquid hydrocarbon
Initially we are measured using traditional wet flow indicator, it is suitable for the gas flow measurement of small flow, are measured
Gas cannot be dissolved in flowmeter internal sealed liquid or with sealing liquid react.It is required that 15 should be maintained at using temperature~
Between 25 DEG C, temperature and the room temperature temperature difference answer≤2 DEG C.At a temperature of this, liquefied gas is not enough to be gasified totally, and a small amount of mercaptan is easy quilt
It is adsorbed in gas circuit, gas chamber or sealing fluid, titration results is caused to can't check；Secondly, the sample of test is high-pressure liquefaction gas, gas
Flow velocity will be suitable for absorbing very much bad, too slow flow control difficulty fastly, lead to gas absorption total volume metering inaccuracy.Therefore, change
Gasified with flashing gasified sampling-fetching device for liquid hydrocarbon to sample, gas flow rate and gasification temperature and needs can be preset
The total volume of absorption.
(2) sample is gasified totally, and the best gasification temperature that mercaptan is not adsorbed by gas circuit selects
Purpose of the liquefied gas from sampling steel cylinder through flashing gasified sampling-fetching device for liquid hydrocarbon is to keep sample complete after purification
Gasification, including trace impurity therein.Gasification temperature is set as 40 DEG C, theoretically can achieve the mesh of gasification for liquefied gas
, but find that, containing a small amount of light dydrocarbon ingredient and micro-moisture in liquefied gas, 40 DEG C of gasification temperature cannot be protected after carefully analyzing
Card sample is gasified totally, and analysis unstable result is caused because of absorption of the pipeline to mercaptan.It will be gasified according to the boiling point of water warm
Degree is set as 100 DEG C by 40 DEG C.By repeatedly testing discovery, since micro water and light dydrocarbon are gasified totally, the suction of sample mercaptan
Receipts are more complete, and titration accuracy is greatly improved.
(3) the enrichment concentration of gaseous sample mercaptan
Gas flow rate control is in 1.5-2L/min, and it is 30-40L that gas, which is arranged, to absorb volume, and sample is through Potential Titration Analysis
It is less prone to jumping, detects unstable result.In order to detect the mercaptan in smaller content gas, absorbing liquid is taken to remain as 40mL
40% potassium hydroxide solution is concentrated to carry out the enrichment of sample, i.e. the absorption volume of increase gaseous sample to 50-80L, such
To titration curve there is apparent jumping, such as Fig. 1.
(4) full-automatic current potential titration method parameter optimization
The setting of this method optimization of main parameter:
Table 1
| Titration parameters | Value before optimizing | Value after optimization |
| Signal drift | 50.0mv/min | 20.0mv/min |
| Minimum incrementss | 50ul | 10ul |
| Measure dot density | 3 | 10 |
| The volume added after up to equivalent point | 0ml | 0.02ml |
| Equivalent point assesses EPC | 30 | 5 |
| Equivalent point identification | 1, greatest | 1, greatest |
For the property of sample, dynamic-current potential DET-U titration mode is selected, is suitble to chemical reaction velocity fast, electrode response
Fastly, the steep reaction type of titration curve jumping.After optimization in titration parameters, the advanced setting step mode of user has been selected, it is minimum
10ul can be accurate to by increasing liquid measure, and equivalent point assessment 5 makes detection reach most sensitive state.Also save titration time, a titration
As long as analysis can be completed for 20-40 seconds.Fig. 2 is the automatic potentiometric titration curve that parameter optimization later group is measured in parallel.
It can see from Fig. 2 titration curve, the standard liquid volume of consumption only has 0.04-0.05ml, mercaptans content 0.9-
1.0ppm, curve is perfect, and titration end-point judges sensitive.
(5) accuracy of analysis method
1) precision of method
It is the measurement situation (n=3) of four samples below:
Table 2
Relative standard deviation RSD≤4.1% of the result of parallel analysis three times of each sample, precision are good.
2) accuracy of method
The degree of closeness of accuracy expression measurement result and true value.Because mercaptan standard specimen is not easy to buy and saves, use
The vulcanized sodium standard liquid of 0.1000mol/L is measured.Titration results are respectively 0.0987mol/L and 0.1008mol/L, analysis
As a result it is respectively 1.3% and 0.8% with the relative error of true value, is less than error 2%, illustrates that the accuracy of analysis method is high.
3) detection sensitivity
As shown in Table 2, it is 0.01mol/L silver nitrate alcohol standard liquid as titrating solution using concentration, 0.9ppm can be accurately detected
Mercaptan, the titrating solution volume of consumption only has 0.04mL or so.Therefore 0.3ppm is limited to by the detection that method is calculated in K=3.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of method of mercaptan sulfur in constant-current titration measurement gas, which comprises the following steps:
(1) vulcanization of new electrode: ten thousand logical composite silver cap electrodes are placed in the sodium sulfide solution of 0.1mol/L and impregnate 1h, takes out and uses
Deionized water is rinsed well, and electrode silver ring becomes bright black at this time, is put into standby in the electrode casing equipped with electrode protection liquid
With；
(2) preparation of sample: liquefied gas sampling steel cylinder to be measured is connect with flashing gasified sampling-fetching device for liquid hydrocarbon, gasification temperature
Control is at 100 DEG C, and gas flow rate is set as 2L/min, and the sample air after gasification is by being filled with appropriate saturated sodium carbonate solution
Enter the accurate absorption bottle that 40% potassium hydroxide solution of 40mL is housed after surge flask, the volume of absorbed sample air is with liquid
The metering of total amount shown by hydrocarbon flashing gasified sampling-fetching device, while recording ambient atmosphere pressure；
(3) analysis of sample: taking 1mol/L sodium hydroxide solution 30mL and 1mol/L ammonia spirit 2.0mL in 100mL beaker,
Then absorbing liquid 10mL is drawn in same beaker with pipette.It opens ten thousand logical 809Titrando softwares and enters work station, call
Corresponding method, titration unit is connect with computer work, and by ten thousand logical composite silver cap electrodes, blender and titrating head are rationally solid
It is fixed, it is immersed in 100ml titrating beaker, starts to carry out automatic Titration, be calculated automatically after the completion of titration according to formula, is measured in parallel
It 3 times, is averaged as testing result.
2. the method for mercaptan sulfur in a kind of constant-current titration measurement gas according to claim 1, which is characterized in that step
(3) process of titration described in the following steps are included:
(1) preparation of 0.1mol/L silver nitrate isopropanol standard solution: 17gAgNO3 is dissolved in 100mL distilled water, uses isopropyl
Alcohol is diluted to 1L.In a brown bottle, calibration is primary weekly for storage.
(2) scaling method: measuring 60mL distilled water in 100mL beaker, and 5 drop nitric acid are added, boil 5min, after cooling accurately
2mL 0.1mol/L potassium iodide standard solution is measured in same beaker, carries out constant-current titration with silver nitrate alcohol standard solution, is dripped
It is 3 times fixed, calculate accurate molar concentration.
3. the method for mercaptan sulfur in a kind of constant-current titration measurement gas according to claim 1, which is characterized in that step
(3) process of titration described in the following steps are included:
(1) it is molten the preparation of 0.01mol/L silver nitrate isopropanol standard solution: to draw 10mL0.1mol/L silver nitrate isopropanol standard
Liquid is in 100mL brown volumetric flask, with isopropanol to groove.Calibration in every 3 days is primary, must be another if there is turbidity and precipitation
Match.
(2) scaling method: accurately pipetting 1mL0.1mol/L potassium iodide standard solution in 100mL beaker, add 50mL distilled water,
Constant-current titration is carried out with about 0.01mol/L silver nitrate alcohol standard solution is diluted to, titrates 3 times, calculates accurate molar concentration.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111983130A (en) * | 2020-09-07 | 2020-11-24 | 赵文建 | Method for detecting complete ammonia distillation based on full-automatic Kjeldahl determination instrument color method |
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| CN111983130A (en) * | 2020-09-07 | 2020-11-24 | 赵文建 | Method for detecting complete ammonia distillation based on full-automatic Kjeldahl determination instrument color method |
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