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SU1549328A1 - Method of analysis of vanadium in oil and petroleum products - Google Patents

Method of analysis of vanadium in oil and petroleum products Download PDF

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Publication number
SU1549328A1
SU1549328A1 SU874309948A SU4309948A SU1549328A1 SU 1549328 A1 SU1549328 A1 SU 1549328A1 SU 874309948 A SU874309948 A SU 874309948A SU 4309948 A SU4309948 A SU 4309948A SU 1549328 A1 SU1549328 A1 SU 1549328A1
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SU
USSR - Soviet Union
Prior art keywords
vanadium
analysis
extraction
oils
petroleum
Prior art date
Application number
SU874309948A
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Russian (ru)
Inventor
А.А. Каплин
С.В. Рябова
Н.М. Дубова
С.В. Образцов
Original Assignee
Научно-исследовательский институт ядерной физики при Томском политехническом институте им.С.М.Кирова
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Application filed by Научно-исследовательский институт ядерной физики при Томском политехническом институте им.С.М.Кирова filed Critical Научно-исследовательский институт ядерной физики при Томском политехническом институте им.С.М.Кирова
Priority to SU874309948A priority Critical patent/SU1549328A1/en
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Publication of SU1549328A1 publication Critical patent/SU1549328A1/en

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Abstract

Изобретение относитс  к аналитической химии и может быть использовано дп  определени  ванади  в неф- т х и нефтепродуктах. Цель изобретени  повышение селективности и экс- прес .ности анализа. Ь качестве экст- рагентг и фонового раствора дл  гра- фировани  ванади  использован водный раствор хлористого аммони  при . Экстракцию ванади  провод т на переменном асимметричном токе в непроточную катодную камеру двухкамерного электролизера. I ил.The invention relates to analytical chemistry and can be used in determining vanadium in petroleum and petroleum products. The purpose of the invention is to increase the selectivity and efficiency of the analysis. An aqueous solution of ammonium chloride was used for extracting vanadium as background extract and background solution. Vanadium extraction is conducted on an alternating asymmetric current into the non-flowing cathode chamber of a two-chamber electrolyzer. I il.

Description

Изобретение относитс  к аналитической химии и может быть использовано дл   анализа ванади  в нефт х и нефтепродуктах.This invention relates to analytical chemistry and can be used to analyze vanadium in petroleum and petroleum products.

Целью изобретени   вл етс  повышение селективности и экспрессности анализа ванади  в нефт х и нефтепродуктах .The aim of the invention is to increase the selectivity and rapidity of analysis of vanadium in petroleum and petroleum products.

Предлагаемый способ иллюстрируетс  чертежом.The proposed method is illustrated in the drawing.

Способ анализа ванадир в нефт х и нефтепродуктах реализуетс  следующим образом.The method of analysis of vanadir in petroleum and petroleum products is implemented as follows.

Навеску нефти раствор ют в толуоле . Полученный раствор подают в анодную камеру 1 электролизера с нерастворимыми графитовыми электродами 2, которые отделены от рабочих камер защитными мембранами 3. Катодна  ка- мера 4 непроточна и заполнена 0,1 М раствором хлористого аммони  (рН 7-9) куда опущены измерительный графитовый 5 и вспомогательный каломельный 6 электроды. Анодна  и катодна  камеры разделены инертней разделительной мембраной 7. Электрохимическую экстракцию ванади  провод т на переменном асимметричном токе частотой 47,5-1 Гц с соотношением iq/iy (1-9):10, который подаетс  от источника 8. После того как весь раствор нефти пропущен через электролизер отключают источник переменного асимметричного тока и через 1-2 мин провод т пол рографическое определение ванади  в объеме катодной камеры 4. Дл  этого включают пол рогра 9 и провод т электронакопление определ емого элемента на поверхности графитового электрода 2 в течени 10 мин приCfэ -1,4 В при непрер зной продувке раствора инертным газ t - гелием через штуцер 10. Затем помощью крана перекрывают лото инертного газа и спуст  1-2 мин рем  успокоени  раствора) прово г электрорастворение осадка ванз   с поверхности графитового электр j 5 с реа СОA portion of the oil is dissolved in toluene. The resulting solution is fed to the anode chamber 1 of the electrolytic cell with insoluble graphite electrodes 2, which are separated from the working chambers by protective membranes 3. The cathode chamber 4 is not flowing and filled with a 0.1 M ammonium chloride solution (pH 7-9) where the graphite measuring 5 is lowered and auxiliary calomel 6 electrodes. The anodic and cathodic chambers are separated by an inert separator membrane 7. Vanadium electrochemical extraction is carried out at an alternating asymmetric current of 47.5-1 Hz with iq / iy ratio (1-9): 10, which is supplied from source 8. After the entire solution oil is passed through the electrolyzer and the source of alternating asymmetric current is disconnected and after 1-2 minutes a polarographic determination of vanadium is carried out in the volume of the cathode chamber 4. To do this, turn on the floor 9 and electron accumulation of the element being detected on the surface of graphite electrode 2 for 10 minutes at Cfe -1.4 V with continuous solution of the solution with an inert gas t - helium through the nozzle 10. Then, using a crane, block the inert gas lotto and after 1-2 minutes a solution reassurance solution) wire dissolves surface graphite electr j 5 with pea CO

ff

ЛL

ЈJ

toto

Ј0 Ю 00Ј0 S 00

гистрацией на самописце 11 аналитического сигнала - анодного пика ванадий. Врем  анализа 2,Ь ч, предел обнаружени  г/л.on the recorder 11 by analytic signal - vanadium anode peak. The analysis time is 2 h, the detection limit is g / l.

Claims (1)

Способ анализа ванади  в нефт х и нефтепродуктах менее трудоемок, чем традиционно используемые способы анализа , св занные с сухим и мокрым озо- ю асимметримиом.токе частотой 47,5 Гц, лением образца или с экстракционным при соотношении ia/iK(1-9): 10 в вариантом-определени . В способе ис- непроточную катодную камеру двухкакислот и нефтей, требующие специального выт жного оборудовани , Формула изобретени  Способ анализа ванади  в нефт х и. нефтепродуктах, включающий растворение пробы в органическом растворителе с последующей экстракцией ванади  в водную фазу на переменномThe method of analysis of vanadium in petroleum and petroleum products is less labor intensive than the traditionally used methods of analysis associated with dry and wet ozone asymmetry at a frequency of 47.5 Hz, sample extraction or extraction at a ratio of ia / iK (1-9) : 10 in option-definition. In the method, a flow-through cathode chamber of two acids and oils that require special exhaust equipment. Claims of Invention A method for analyzing vanadium in oils and. oil products, including the dissolution of the sample in an organic solvent, followed by extraction of the vanadium into the aqueous phase at variable асимметримиом.токе частотой 47,5 Гц, при соотношении ia/iK(1-9): 10 в непроточную катодную камеру двухкакислот и нефтей, требующие специального выт жного оборудовани , Формула изобретени  Способ анализа ванади  в нефт х и. нефтепродуктах, включающий растворение пробы в органическом растворителе с последующей экстракцией ванади  в водную фазу на переменном47.5 Hz asymmetry with a current ratio of ia / iK (1-9): 10 to the non-flowing cathode chamber of dycic acids and oils that require special exhaust equipment. Claim for analysis of vanadium in oils and. oil products, including the dissolution of the sample in an organic solvent, followed by extraction of the vanadium into the aqueous phase at variable ключаютс  потери определ емого элемента , св занные с трудоемкими химическими операци ми, а также устран етс  наличие дополнительных загр знений привнесенных используемыми химическими реактивами, что  вл етс  очень важным дл  такого услови  труда химика-аналитика , ( так как отсутствуют операции, св занные с испарени миthe loss of the element to be determined, associated with laborious chemical operations, and the presence of additional contaminants introduced by the chemical reagents used, which is very important for such working conditions of the analytical chemist, is eliminated (since there are no operations associated with evaporation mi мерного электролизера и пол рографи- рованием полученного раствора, о т личающийс  тем, что, сdimensional electrolyzer and the polarization of the resulting solution, which is characterized in that целью повышени  экспрессности и селективности анализа, в качестве экст- рагента и фона дл  пол рографического определени  ванади  использованThe goal of increasing the expressivity and selectivity of the analysis, as an extractant and background, was used for the polarographic determination of vanadium. водный раствор хлористого аммони  с .ammonium chloride aqueous solution
SU874309948A 1987-09-28 1987-09-28 Method of analysis of vanadium in oil and petroleum products SU1549328A1 (en)

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SU874309948A SU1549328A1 (en) 1987-09-28 1987-09-28 Method of analysis of vanadium in oil and petroleum products

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SU874309948A SU1549328A1 (en) 1987-09-28 1987-09-28 Method of analysis of vanadium in oil and petroleum products

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102778495A (en) * 2012-08-03 2012-11-14 西安石油大学 Electrochemical gaging method for content of metal vanadium in crude oil
CN105548320A (en) * 2015-12-16 2016-05-04 广东石油化工学院 Method for researching cracking of organic chlorine in crude oil

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Авторское свидетельство СССР № 1475170, кл. G 01 N 27/48, 15.10.86. *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102778495A (en) * 2012-08-03 2012-11-14 西安石油大学 Electrochemical gaging method for content of metal vanadium in crude oil
CN102778495B (en) * 2012-08-03 2014-07-23 西安石油大学 Electrochemical gaging method for content of metal vanadium in crude oil
CN105548320A (en) * 2015-12-16 2016-05-04 广东石油化工学院 Method for researching cracking of organic chlorine in crude oil

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