CN103245622A - Method for measuring total sulfur in fuel oil by using formaldehyde absorption-pararosaniline hydrochloride colorimetric method - Google Patents
Method for measuring total sulfur in fuel oil by using formaldehyde absorption-pararosaniline hydrochloride colorimetric method Download PDFInfo
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- CN103245622A CN103245622A CN2013101475200A CN201310147520A CN103245622A CN 103245622 A CN103245622 A CN 103245622A CN 2013101475200 A CN2013101475200 A CN 2013101475200A CN 201310147520 A CN201310147520 A CN 201310147520A CN 103245622 A CN103245622 A CN 103245622A
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Abstract
The invention discloses a method for measuring total sulfur in fuel oil by using a formaldehyde absorption-pararosaniline hydrochloride colorimetric method. The method comprises the following steps of: combusting the fuel oil, absorbing the emitted sulfur dioxide by using formaldehyde to generate stable hydroxyl methanesulfonic acid, adding alkali to react with pararosaniline hydrochloride, thus obtaining a stable purple red compound, and measuring the absorbance at 565.0nm, wherein the absorbance is in direct proportion to the sulfur content. Compared with the prior art, the method is higher in both measuring sensitivity and accuracy, and the measuring method is simple to operate.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of method of measuring total sulfur in the fuel oil.
Background material
The harm that the existence of sulphur is used petroleum refining process and products thereof is many-sided, as corroding metal equipment, cause in catalyst poisoning, the use contaminated environment etc.Thereby sulfide content is significant in the control fuel oil.The method of measuring at present sulfur content in the fuel oil has: Ignition Lamp Method (GB/T380), energy dispersion X ray fluorescence spectrometry (GB/T17040), coulometry (SH/T0253), nickel reducing process (SH/T 0252), tube oven method ((advance/T387), x-ray spectrometry (GB/T 11140), bomb method (GB/T 388), lamp method (GB/T 11131), coulometry (SH/T 0303) etc.Wherein Ignition Lamp Method (GB/T380) and coulometry (SH/T 0253) are the most frequently used methods.Ignition Lamp Method is arbitration law, but sensitivity is low, and measurement result was unreliable when the sample sulfur content was low, requires more and more lower fuel oil obsolescence for sulfur content, and oil inflame not exclusively can produce organic acid, makes measurement result higher, and minute is oversize.Coulometry needs the high instrument of price, the condition determination harshness, and the technical merit of having relatively high expectations, otherwise the true sulfur content of measurement result and sample is not inconsistent.Other method also has similar shortcoming.The present invention provides methods of total sulfur in the higher mensuration fuel oil of a kind of sensitivity and accuracy in conjunction with Ignition Lamp Method and colourimetry.
Summary of the invention
The technical problem to be solved in the present invention provides the method for total sulfur in a kind of formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil, measure sensitivity and accuracy and all be higher than prior art, and measuring method is simple to operate.
The present invention is achieved through the following technical solutions:
Principle of the present invention is: with oil inflame, the sulphuric dioxide that discharges absorbs the back with formaldehyde and generates stable hydroxymethyl sulfonic acid, generate stable aubergine compound with the hydrochloric acid Pararosaniline after adding alkali, measure its absorbance in the 565.0nm place and be directly proportional with sulfur content.
The method of total sulfur comprises the following steps: in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil
(1) with fuel oil and ethanol by weight with volume be the ratio of 1:0.2-4.0 mix fuel oil to be tested, fuel oil to be tested is placed the glassware internal combustion, absorb burning gases with the buffered formaldehyde absorption liquid, the absorption liquid temperature remains on 23～29 ℃ scope, after treating that the burning gases absorption is finished, add distilled water in the absorption liquid and be settled to 25.00ml, get specimen;
(2) get specimen 10 ml that step (1) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(3) use and the burning of the ethanol of specimen equal volume, absorb burning gases with the buffered formaldehyde absorption liquid, the absorption liquid temperature remains on 23～29 ℃ scope, treat burning gases absorb finish after, add distilled water in the absorption liquid and be settled to 25.00ml, get blank sample;
(4) get blank sample 10 ml that step (3) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(5) absorbance difference that records of the absorbance that records with step (2) and step (4) is looked into the sulfur content typical curve, obtains the specimen sulfur content.
The preparation of buffered formaldehyde absorption liquid, with 0.364 gram disodium ethylene diamine tetraacetate, 2.04 g Potassium Hydrogen Phthalates are dissolved in the low amounts of water, add 36%～38% formalin 5.30ml, are diluted with water to 1000 ml again, are stored in 4 ℃ of bad borders.
The preparation of hydrochloric acid Pararosaniline solution with 0.0625 gram Pararosaniline, adds strong phosphoric acid, 2.10 ml, 37% concentrated hydrochloric acid of 77.0ml 85%, is diluted with water to 250ml, shakes up, and places the back of spending the night and uses.
The collection of step (1), step (3) burning gases: with sample to be tested or with the ethanol of sample equal volume to be tested, place the 5-8ml vial, place an iron pipe to make wick with hospital gauze, wick is inserted in the liquid in the vial, light wick, making the flare height is 6-8mm, and the glassware that has gas outlet with top covers flame, with the flow of sampling thief with 0.5 L/min burning gases is delivered in the buffered formaldehyde absorption liquid of adorning in the fritted glass disk bubbler.
The sulfur content typical curve obtains by following steps:
(5) get 11 of 10 ml color-comparison tubes, add buffered formaldehyde absorption liquid 2.00ml respectively, distilled water 8.00ml, mixing adds 1.2600g/L sodium sulphite standard solution 0.00 more respectively, 10.00,30.00,50.00,70.00,90.00,110.00,130.00,150.00,170.00,190.00 μ l, the solution sulfur-bearing of preparation is respectively 0.00,3.20,9.60,16.00,22.40,28.80,35.20,41.60,48.0.00, the standard model of 54.40,60.80mg/L;
(6) get standard model 10 ml that step (5) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(7) the standard model absorbance that records with (6) is drawn the sulfur content typical curve.
The present invention has the following advantages:
One. the present invention adopts rare buffered formaldehyde absorption liquid to absorb the sulphuric dioxide that oil inflame discharges, and with acid hydrochloride salt Pararosaniline chromogenic assay sulfide content, environmental pollution is little, and analysis cost is low.Measurement result accuracy height, it is highly sensitive to survey the sulphur method than existing fuel oil, favorable reproducibility, the range of linearity is wide, and low or high sulfur-bearing sample all can be measured.
Two. used fuel oil is few, and burning time is short, and minute shortens greatly.
Three. experiment equipment is easy to get, and adopts visual colorimetry to need not any expensive instrument, can extensively promote.
Four. avoid the Ignition Lamp Method fuel oil to burn the organic acid of generation to the influence of measurement result.
Description of drawings
Fig. 1 is sulfur content typical curve synoptic diagram of the present invention.
Fig. 2 collects synoptic diagram for combustion gas among the present invention.
Embodiment
Further specify technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is restriction to technical scheme.
Embodiment 1:
The preparation of buffered formaldehyde absorption liquid, with 0.364 gram disodium ethylene diamine tetraacetate, 2.04 g Potassium Hydrogen Phthalates are dissolved in the low amounts of water, add 36%～38% formalin 5.30ml, are diluted with water to 1000 ml again, preserve in 4 ℃ of environment standby.
0.0625 gram Pararosaniline is got in the preparation of hydrochloric acid Pararosaniline solution, adds concentrated phosphoric acid, 2.10 ml, 37% concentrated hydrochloric acid solution of 77.0ml 85%, is diluted with water to 250ml, shakes up, and is standby after placement is spent the night.
(1) as shown in Figure 2, open a duck eye in a 500ml beaker bottom side, insert a glass tube, and fix with high temperature resistant solid gum, be communicated with glass tube with sebific duct again, the draft tube of the connected porous glass plate of the other end of sebific duct absorption tube, the escape pipe of fritted glass disk bubbler is communicated with sampling thief.The buffered formaldehyde absorption liquid 5.00ml that packs in the fritted glass disk bubbler, distilled water 5.00ml, mixing.Delivery is intended fuel oil (be solvent with the normal octane, contain the analog gasoline of 100.00ppm sulphur with the benzothiophene preparation) 1.0000g, places a 8ml vial, adds 4ml ethanol, and mixing gets specimen.Place a diameter 6mm iron pipe to make wick with hospital gauze, wick is inserted in the specimen in the vial, light wick, making the flare height is 6-8mm, covers flame with beaker 1.In the present embodiment, the TWA-300H air sampler that adopts Jintan City Turner instrument plant to produce.
With the flow gas production of 0.5 L/min, the buffered formaldehyde absorption liquid temperature in the fritted glass disk bubbler remains on 23～29 ℃ scope.Treat the liquid afterburnt in the vial, the absorption liquid of fritted glass disk bubbler changed in the 25.00ml volumetric flask that wash fritted glass disk bubbler with distilled water, its raffinate changes in the 25.00ml volumetric flask, is settled to 25.00ml with distilled water, gets specimen.
(2) get specimen 10 ml that step (1) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then.
(3) use and the burning of the ethanol of specimen equal volume, the same step of operation steps (1) gets blank sample;
(4) get blank sample 10 ml that step (3) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
The difference of the blank sample absorbance that the specimen absorbance that obtains with step (2) and step (4) obtain is looked into the sulfur content typical curve and is obtained sulfur content in the specimen.
The sulfur content typical curve obtains by following steps:
(5) get 11 of 10 ml color-comparison tubes, add buffered formaldehyde absorption liquid 2.00ml respectively, distilled water 8.00ml adds 1.2600g/L sodium sulphite standard solution 0.00,10.00 with microsyringe respectively again, 30.00,50.00,70.00,90.00,110.00,130.00,150.00,170.00,190.00 μ l, the solution sulfur-bearing of preparation is respectively 0.00,3.20,9.60,16.00,22.40,28.80,35.20,41.60,48.0.00, the standard model of 54.40,60.80mg/L.
(6) get standard model 10 ml that step (5) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(7) absorbance that records with step (6) is drawn the sulfur content typical curve.
Specimen is measured precision: the 100.00ppm standard model, 6 relative standard deviations of replication are less than 3.5%.Accuracy: measure 6 100ppm concentration of analog samples, measured value is 95.0ppm ± 2.5(x ± SD).
Embodiment 2:
Determination of total sulfur content in the 97# gasoline
Get 97# gasoline 1.0000g and place a 8ml vial, add 1-4ml ethanol mixing.Contain sulphur concentration in the specimen and look into the sulfur content typical curve.Measure 6 samples, measured value is 240.6ppm ± 9.5(x ± SD).
All the other are implemented as embodiment 1.
Embodiment 3:
Determination of total sulfur content in the 0# of oxidation sweetening diesel oil
The 0# diesel oil 1.0000g of oxidation sweetening of learning from else's experience places a 8ml vial, adds 1-4ml ethanol.Contain sulphur concentration in the specimen and look into the sulfur content typical curve.Measure 6 samples, measured value is 38.4ppm ± 1.5(x ± SD).
Claims (5)
1. the method for total sulfur in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil is characterized in that comprising the following steps:
(1) with fuel oil and ethanol by weight with volume be the ratio of 1:0.2-4.0 mix fuel oil to be tested, fuel oil to be tested is placed the glassware internal combustion, absorb burning gases with the buffered formaldehyde absorption liquid, the absorption liquid temperature remains on 23～29 ℃ scope, after treating that the burning gases absorption is finished, add distilled water in the absorption liquid and be settled to 25.00ml, get specimen;
(2) get specimen 10 ml that step (1) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(3) use and the burning of the ethanol of specimen equal volume, absorb burning gases with the buffered formaldehyde absorption liquid, the absorption liquid temperature remains on 23～29 ℃ scope, treat burning gases absorb finish after, add distilled water in the absorption liquid and be settled to 25.00ml, get blank sample;
(4) get blank sample 10 ml that step (3) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(5) absorbance difference that records of the absorbance that records with step (2) and step (4) is looked into the sulfur content typical curve, obtains the specimen sulfur content.
2. the method for total sulfur in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil according to claim 1, it is characterized in that: the preparation of buffered formaldehyde absorption liquid, with 0.364 gram disodium ethylene diamine tetraacetate, 2.04 g Potassium Hydrogen Phthalate, be dissolved in the low amounts of water, the formalin 5.30ml of adding 36%～38% is diluted with water to 1000 ml again, is stored in 4 ℃ of bad borders.
3. the method for total sulfur in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil according to claim 1, it is characterized in that: the preparation of hydrochloric acid Pararosaniline solution, with 0.0625 gram Pararosaniline, the strong phosphoric acid, 2.10 ml, 37% concentrated hydrochloric acid that add 77.0ml 85%, be diluted with water to 250ml, shake up, place the back of spending the night and use.
4. the method for total sulfur in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil according to claim 1, it is characterized in that: step (1), the collection of step (3) burning gases: with sample to be tested or with the ethanol of sample equal volume to be tested, place the 5-8ml vial, place an iron pipe to make wick with hospital gauze, wick is inserted in the liquid in the vial, light wick, making the flare height is 6-8mm, the glassware that has gas outlet with top covers flame, with the flow of sampling thief with 0.5 L/min burning gases is delivered in the buffered formaldehyde absorption liquid of adorning in the fritted glass disk bubbler.
5. total sulfur method in the formaldehyde absorption-hydrochloric acid Pararosaniline colorimetric method for determining fuel oil according to claim 1, it is characterized in that: the sulfur content typical curve obtains by following steps:
(6) get 11 of 10 ml color-comparison tubes, add buffered formaldehyde absorption liquid 2.00ml respectively, distilled water 8.00ml, mixing adds 1.2600g/L sodium sulphite standard solution 0.00 more respectively, 10.00,30.00,50.00,70.00,90.00,110.00,130.00,150.00,170.00,190.00 μ l, the solution sulfur-bearing of preparation is respectively 0.00,3.20,9.60,16.00,22.40,28.80,35.20,41.60,48.0.00, the standard model of 54.40,60.80mg/L;
(7) get standard model 10 ml that step (6) obtains and place color comparison tube, add 0.50ml 48.0g/L NaOH and 0.50ml 8.0 g/L dithiocarbamic acids, add 2.50ml 0.25g/L hydrochloric acid Pararosaniline solution behind the mixing, mixing places 20 ℃ of water-bath 10min rapidly; On spectrophotometer, measure its absorbance with wavelength 565 nm places then;
(8) the standard model absorbance that records with (7) is drawn the sulfur content typical curve.
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Cited By (5)
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| CN106198431A (en) * | 2016-08-31 | 2016-12-07 | 大工（青岛）新能源材料技术研究院有限公司 | A kind of method of former sulfur content of coal detection |
| CN106525833A (en) * | 2016-11-08 | 2017-03-22 | 江苏中烟工业有限责任公司 | Method for determining sulfur dioxide in cigarette main stream smoke through a continuous flow analyzer |
| CN106769951A (en) * | 2017-02-28 | 2017-05-31 | 江汉大学 | Sodium pyrosulfite detection method of content and its device in analgin bulk drug |
| CN107607483A (en) * | 2017-09-15 | 2018-01-19 | 赣州华兴钨制品有限公司 | The method of sulphur in pararosaniline hydrochloridc Spectrophotometric Determination of Tungsten product |
| CN109932325A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | The measuring method and quantum dot ink formulation method of particle surface ligand content |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198431A (en) * | 2016-08-31 | 2016-12-07 | 大工（青岛）新能源材料技术研究院有限公司 | A kind of method of former sulfur content of coal detection |
| CN106525833A (en) * | 2016-11-08 | 2017-03-22 | 江苏中烟工业有限责任公司 | Method for determining sulfur dioxide in cigarette main stream smoke through a continuous flow analyzer |
| CN106769951A (en) * | 2017-02-28 | 2017-05-31 | 江汉大学 | Sodium pyrosulfite detection method of content and its device in analgin bulk drug |
| CN107607483A (en) * | 2017-09-15 | 2018-01-19 | 赣州华兴钨制品有限公司 | The method of sulphur in pararosaniline hydrochloridc Spectrophotometric Determination of Tungsten product |
| CN109932325A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | The measuring method and quantum dot ink formulation method of particle surface ligand content |
| CN109932325B (en) * | 2017-12-15 | 2021-10-22 | Tcl科技集团股份有限公司 | Method for measuring content of ligand on particle surface and method for preparing quantum dot ink |
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Application publication date: 20130814 |