WO2009123496A1 - Procédé et dispositif pour déterminer la présence d’impuretés dans le pétrole ou des produits pétroliers - Google Patents
Procédé et dispositif pour déterminer la présence d’impuretés dans le pétrole ou des produits pétroliers Download PDFInfo
- Publication number
- WO2009123496A1 WO2009123496A1 PCT/RU2008/000209 RU2008000209W WO2009123496A1 WO 2009123496 A1 WO2009123496 A1 WO 2009123496A1 RU 2008000209 W RU2008000209 W RU 2008000209W WO 2009123496 A1 WO2009123496 A1 WO 2009123496A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silver
- electrode
- measuring
- chamber
- oil
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000012535 impurity Substances 0.000 title claims abstract description 11
- 239000003209 petroleum derivative Substances 0.000 title abstract description 4
- 229910052709 silver Inorganic materials 0.000 claims abstract description 20
- 239000004332 silver Substances 0.000 claims abstract description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- -1 sulphide ions Chemical class 0.000 claims abstract description 8
- 238000005443 coulometric titration Methods 0.000 claims abstract description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000011707 mineral Substances 0.000 claims abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 5
- 239000005486 organic electrolyte Substances 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 3
- 238000004313 potentiometry Methods 0.000 claims abstract description 3
- 238000005070 sampling Methods 0.000 claims abstract description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 5
- 159000000002 lithium salts Chemical class 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 150000001449 anionic compounds Chemical class 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 229910001412 inorganic anion Inorganic materials 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 abstract description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 6
- 150000001805 chlorine compounds Chemical class 0.000 description 5
- 150000003568 thioethers Chemical class 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000012457 nonaqueous media Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 2
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 230000009897 systematic effect Effects 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 229940031993 lithium benzoate Drugs 0.000 description 1
- LDJNSLOKTFFLSL-UHFFFAOYSA-M lithium;benzoate Chemical compound [Li+].[O-]C(=O)C1=CC=CC=C1 LDJNSLOKTFFLSL-UHFFFAOYSA-M 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/44—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte using electrolysis to generate a reagent, e.g. for titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/423—Coulometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
Definitions
- the invention relates to the field of determining the content of mercaptans, chloride and sulfide ions in oil and oil products and can be used for coulometric titration in non-aqueous solutions with potentiometric indication of equivalence points.
- a known method of measuring individual components in non-aqueous media comprising burning a sample, absorbing gases, followed by coulometric titration of the components.
- the disadvantage of this method is that in this method the total content of chlorine and sulfide is determined.
- the voltage applied to the generator and auxiliary electrodes due to the voltage drop in the solution significantly affects the emf of the galvanic cell and does not allow fixing the equivalence points, and thus measure (patent RU 2243552 , 2004).
- the technical result from the use of the present invention is the ability to determine in oil impurities of sulfides, chlorides and mercaptans (as well as bromides and iodides, if present) without the use of titrants, giving a systematic error in the determination, as well as the possibility of automation of the method.
- a method for determining impurities in oil and oil products includes automatic sampling, transferring it to a measuring electrochemical cell, mixing with a mineral or organic electrolyte, homogenizing the resulting mixture, electrochemical generation of silver by anodic oxidation of a silver generator electrode, and sequential coulometric titration of the mixture with generated silver ions with fixing points of equivalence by potentiometric method using indicator sulfur ro-selective electrode.
- Anodic oxidation of silver is mainly carried out in an environment containing an electrolyte with concentrations from 0.001 to O, IM at electrolysis currents from 3 to 0.01 mA.
- an organic electrolyte a solution of lithium salt with an anion of an organic acid is predominantly used.
- a solution of lithium salts with inorganic anions is mainly used as a mineral electrolyte.
- Lithium salts such as hexafluorophosphate, pechlorate, etc., are good electrolytes and have high solubility in organic solvents.
- a pH sensitive glass electrode is usually used as a reference electrode.
- the proposed device for implementing this method includes a chamber with a mixing device and fittings for supplying and removing liquids.
- the chamber consists of two interconnected electrochemical cells located one below the other.
- a generating cell with two horizontally mounted plate electrodes, of which the lower is a cathode and made of platinum, and the upper is made of silver and has openings for communication with the measuring electrochemical cell located above.
- This cell includes a measuring ion-selective electrode and a reference electrode.
- the most suitable mixing device is a magnetic stirrer, which is located between the electrodes of the generating cell.
- the cathode of the generating cell can be mounted in the bottom of the chamber. It is desirable that the area of the holes in the anode of the generating cell be at least 30% of the total surface of the plate of the anode, which will provide more complete and reliable homogenization of the mixture in the chamber.
- the measuring device is shown in Fig. L and is a cylindrical chamber 1 with a nozzle 9 for supplying liquids and a nozzle 10 for withdrawing the mixture. Preferred dimensions of the chamber 1: inner diameter - 40-50 mm; height - 60 mm.
- the generating electrochemical cell includes two horizontal plate electrodes 6 and 7.
- the lower electrode, cathode 7, can be mounted in the bottom of chamber 1, and the second electrode, anode 6, is located at a distance not exceeding 20 mm from cathode 7.
- the device is a magnetic stirrer 5, which functions from external influences — a source 8 of an alternating magnetic field.
- the plate of the upper electrode - anode 6 has holes, which allows homogenization of the measured solution in the entire volume of both cells of chamber 1.
- the area of the holes in the anode 6 of the generating cell is at least 30% of the total surface area of the anode plate.
- Measuring silver-selective electrode 2 is a modification of the ion-selective electrode IONIKS 122 (LLC IOHIKC alpha). Which is made in the form of a tube, at the end of which an element sensitive to silver ions is fixed.
- the reference electrode 3 can be selected, for example, pH is a sensitive sensor.
- a device in which the proposed method is implemented operates as follows.
- a sample of a fixed volume for example, taken from an oil pipeline using an automatic peristaltic pump, is supplied into the chamber 1 through the nozzle 9. Then, a fixed volume of electrolyte is supplied to chamber 1 in the same way.
- the mixture of liquids is homogenized - mixed with a magnetic stirrer 5 for 2-3 minutes.
- the EMF of the measuring cell 4 composed of a glass electrode 3 used as a reference electrode, and a silver-selective measuring electrode 2 (indicator electrode of the IONIKS 122 type) is recorded.
- a constant voltage is applied to the electrodes 6 and 7 of the generating electrochemical cell and the change in the EMF of the measuring cell 4 in time is recorded.
- the equivalence points are successively reached, the amount of electricity spent on electrolysis is measured, and based on the combined Faraday law, the amount of this or that impurity contained in the sample is calculated.
- the mixture of liquids is removed from the chamber 1 through the nozzle 10 using a pump.
- the chamber 1 is washed with a washing reagent with a working magnetic stirrer 5.
- mineral and organic salts for example, lithium perchlorate or lithium benzoate
- the horizontally located indicator and generator electrodes with a mixing device between them and a galvanic measuring cell located above them allow measurements in organic media, while eliminating the influence of voltage in the generator part on the potential of the measuring measuring cell.
- the device of the claimed design allows to increase the accuracy of determination of chlorides, mercaptans and sulfides in oil by eliminating errors associated with the standardization of titrant, simplify the design of the analyzer and, as a result, increase the accuracy of the determination.
- FIG. 2 A typical sequential coulometric titration curve of sulfides, mercaptans and chlorides is shown in FIG. 2. The curve was obtained at a concentration of sulfides, mercaptans and chlorides equal to 10 "4 mEq / L. The current strength was 0.98 mA. A 0.0 IM solution of lithium perchlorate in a mixed solvent of equal volumes of toluene and decyl alcohol was used as an electrolyte. Prior to titration of the admixture mixture, equivalence points on the control samples were determined, each of which contained only one of these impurities.
- Determination of the content of mercaptans is possible in the concentration range from 10 to 200 mg / l. In the concentration range of less than 1 mg / L, a relatively small jump in the potentiometric detector does not allow us to fix the equivalence point; when the concentration of mercaptans is above 200 mr / L, the determination error associated with a decrease in current efficiency increases.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Immunology (AREA)
- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
L’invention concerne la détermination de la teneur du pétrole ou de produits pétroliers en mercaptans ou en ions de chlorure ou de sulfure. Le procédé consiste à effectuer la sélection automatique d’un échantillon, à transférer l’échantillon dans une cellule électrochimique, à le mélanger avec un électrolyte minéral ou organique, à homogénéiser le mélange obtenu, à effectuer une génération électrochimique de l’argent par l’oxydation anodique de l’électrode d’argent pour générateurs et à effectuer le titrage coulonométrique sériel du mélange par des ions d’argent générés en fixant les points d’équivalence par procédé potentiométrique et en utilisant une électrode d’indication sélectrice d’argent. L’oxydation anodique de l’argent est effectuée dans un milieu contenant l’électrolyte à des concentrations de 0,001 à 0,1 M et des valeurs de courant de 3 à 0,01 mA. Le dispositif pour détecter la présence d’impuretés comprend une chambre avec un dispositif de mélangeage et des tubulures d’amenée et d’évacuation de liquides. La chambre est constituée de deux cellules électrochimiques disposées l’une au-dessus de l’autre. Dans la partie inférieure de la chambre on a monté une cellule génératrice avec deux électrodes en plaques montées horizontalement dont l’électrode inférieure est une cathode en platine et l’électrode supérieure est une anode en argent et possède des orifices de communication avec la cellules électrochimique de mesure disposées plus haut, qui comprend une électrode sélectrice d’ions de mesure et une électrode de comparaison.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/RU2008/000209 WO2009123496A1 (fr) | 2008-04-03 | 2008-04-03 | Procédé et dispositif pour déterminer la présence d’impuretés dans le pétrole ou des produits pétroliers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/RU2008/000209 WO2009123496A1 (fr) | 2008-04-03 | 2008-04-03 | Procédé et dispositif pour déterminer la présence d’impuretés dans le pétrole ou des produits pétroliers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2009123496A1 true WO2009123496A1 (fr) | 2009-10-08 |
Family
ID=41135768
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/RU2008/000209 WO2009123496A1 (fr) | 2008-04-03 | 2008-04-03 | Procédé et dispositif pour déterminer la présence d’impuretés dans le pétrole ou des produits pétroliers |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2009123496A1 (fr) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110108836A (zh) * | 2019-05-30 | 2019-08-09 | 岭东核电有限公司 | 核电厂废液处理系统中氯离子浓度的测定方法及其应用 |
| RU2735372C1 (ru) * | 2020-05-29 | 2020-10-30 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Способ определения содержания сульфидов в отложениях в нефтепромысловом оборудовании |
| RU2743783C1 (ru) * | 2020-06-30 | 2021-02-25 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Способ определения состава отложений, образующихся в оборудовании для подготовки нефти |
| CN112964826A (zh) * | 2021-03-17 | 2021-06-15 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | 高温燃烧水解-电位滴定测定油中氯离子的捕集装置和方法 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU320772A1 (fr) * | Специальное конструкторское бюро автоматике нефтепереработке | |||
| GB972172A (en) * | 1962-10-24 | 1964-10-07 | Beckman Instruments Inc | Coulometric reagent generator |
| SU443301A1 (ru) * | 1972-12-15 | 1974-09-15 | Предприятие П/Я Х-5498 | Устройство дл кулонометрического титровани |
| SU645077A1 (ru) * | 1977-05-03 | 1979-01-30 | Предприятие П/Я А-7564 | Способ количественного определени алифатических и ароматических спиртов в углеводородах |
| GB2237387A (en) * | 1989-09-25 | 1991-05-01 | Petrochem Analysis Limited | Coulometric titration system |
-
2008
- 2008-04-03 WO PCT/RU2008/000209 patent/WO2009123496A1/fr active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU320772A1 (fr) * | Специальное конструкторское бюро автоматике нефтепереработке | |||
| GB972172A (en) * | 1962-10-24 | 1964-10-07 | Beckman Instruments Inc | Coulometric reagent generator |
| SU443301A1 (ru) * | 1972-12-15 | 1974-09-15 | Предприятие П/Я Х-5498 | Устройство дл кулонометрического титровани |
| SU645077A1 (ru) * | 1977-05-03 | 1979-01-30 | Предприятие П/Я А-7564 | Способ количественного определени алифатических и ароматических спиртов в углеводородах |
| GB2237387A (en) * | 1989-09-25 | 1991-05-01 | Petrochem Analysis Limited | Coulometric titration system |
Non-Patent Citations (1)
| Title |
|---|
| B.A. LOPATIN. ET AL.: "Teoreticheskie osnovy elektrokhimicheskikh metodov analiza. Moskva", VYSSHAYA SHKOLA, vol. 47, 1975, pages 70,71, - 83,84 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110108836A (zh) * | 2019-05-30 | 2019-08-09 | 岭东核电有限公司 | 核电厂废液处理系统中氯离子浓度的测定方法及其应用 |
| RU2735372C1 (ru) * | 2020-05-29 | 2020-10-30 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Способ определения содержания сульфидов в отложениях в нефтепромысловом оборудовании |
| RU2743783C1 (ru) * | 2020-06-30 | 2021-02-25 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Способ определения состава отложений, образующихся в оборудовании для подготовки нефти |
| CN112964826A (zh) * | 2021-03-17 | 2021-06-15 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | 高温燃烧水解-电位滴定测定油中氯离子的捕集装置和方法 |
| CN112964826B (zh) * | 2021-03-17 | 2023-10-17 | 中国大唐集团科学技术研究院有限公司华中电力试验研究院 | 高温燃烧水解-电位滴定测定油中氯离子的捕集装置和方法 |
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