SU1672351A1 - Method of chromatographic analysis of organic solutions containing water and acid components - Google Patents

Method of chromatographic analysis of organic solutions containing water and acid components Download PDF

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SU1672351A1
SU1672351A1 SU884364636A SU4364636A SU1672351A1 SU 1672351 A1 SU1672351 A1 SU 1672351A1 SU 884364636 A SU884364636 A SU 884364636A SU 4364636 A SU4364636 A SU 4364636A SU 1672351 A1 SU1672351 A1 SU 1672351A1
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containing water
solutions containing
mea
column
organic solutions
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Людмила Георгиевна Малиевская
Надежда Ивановна Цырульник
Ольга Борисовна Кравченко
Светлана Николаевна Пивоварова
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Всесоюзный Научно-Исследовательский И Проектный Институт По Переработке Газа
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/286—Phases chemically bonded to a substrate, e.g. to silica or to polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3206—Organic carriers, supports or substrates
    • B01J20/3208—Polymeric carriers, supports or substrates
    • B01J20/3212—Polymeric carriers, supports or substrates consisting of a polymer obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
    • B01J20/3244—Non-macromolecular compounds
    • B01J20/3246—Non-macromolecular compounds having a well defined chemical structure
    • B01J20/3248—Non-macromolecular compounds having a well defined chemical structure the functional group or the linking, spacer or anchoring group as a whole comprising at least one type of heteroatom selected from a nitrogen, oxygen or sulfur, these atoms not being part of the carrier as such
    • B01J20/3251—Non-macromolecular compounds having a well defined chemical structure the functional group or the linking, spacer or anchoring group as a whole comprising at least one type of heteroatom selected from a nitrogen, oxygen or sulfur, these atoms not being part of the carrier as such comprising at least two different types of heteroatoms selected from nitrogen, oxygen or sulphur
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Изобретение относитс  к газохроматографическому анализу гликольаминовых растворов, содержащих воду и кислые компоненты, и может быть использовано в нефт ной, газовой и химической промышленности. Цель изобретени  - повышение селективности и безопасности способа и снижение его трудоемкости. В качестве насадки хроматографической колонки используют полисорб-1, модифицированный 2% 1, 2, 3-трис-(β-цианэтокси) пропана. Разделение на колонке ведут последовательно в двух режимах: вначале изотермическом при 60°С, а затем в режиме ступенчатого программировани  с конечной температурой 176°С. 1 ил.This invention relates to gas chromatographic analysis of glycolamine solutions containing water and acidic components, and can be used in the petroleum, gas, and chemical industries. The purpose of the invention is to increase the selectivity and safety of the method and reduce its complexity. Polysorb-1 modified with 2% 1, 2, 3-tris- (β-cyanoethoxy) propane was used as a chromatographic column packing. The separation on the column is carried out sequentially in two modes: initially isothermal at 60 ° C, and then in the step programming mode with a final temperature of 176 ° C. 1 il.

Description

Изобретение относитс  к газохрома- тографическим способам анализа многокомпонентных жидких смесей и может быть использовано в нефт нной, газовой и химической отрасл х промышленности.The invention relates to gas chromatographic methods for analyzing multicomponent liquid mixtures and can be used in the oil, gas and chemical sectors of the industry.

Цель изобретени  - повышение селективности и безопасности способа и снижение его трудоемкости.The purpose of the invention is to increase the selectivity and safety of the method and reduce its complexity.

Способ осуществл ют следующим образом .The method is carried out as follows.

Анализируемую смесь ввод т в поток газа-носител , раздел ют на колонке, заполненной полисорбом-1, модифицированным 2% 1,2,3-трис{/ -цианэтокси) пропана, и ведут разделение последовательно сначала в изотермическом режиме, при t 60°C, дл  разделени  кислых компонентов, а затем в режиме ступенчатого программировани  с Тконечм 176°С. дл  разделени  воды, МЭА иThe analyzed mixture is introduced into a carrier gas stream, separated on a column filled with polysorb-1, modified with 2% 1,2,3-tris {/ -cyanoethoxy) propane, and the separation is carried out sequentially, first in an isothermal mode, at t 60 ° C, to separate the acidic components, and then in a step programming mode with a terminal of 176 ° C. for the separation of water, MEA and

ДЭГа, причем количественную регистрацию осуществл ют на детекторе по теплопроводности .DEG, moreover, quantitative registration is carried out on a thermal conductivity detector.

Пример. Анализ гликольаминового раствора, содержащего диоксид углерода, сероводород и воду провод т на хроматографе с детектором по теплопрводности на хроматографической колонке из нержавеющей стали или стекла длиной 3 м, диаметром 3 мм, заполненной полисорбом-1, модифицированным 2% 1,2,3-трис-{/ -цианэтокси) пропана. Перед началом анализа колонку насыщают МЭА путем двухкратного ввода 1 - 2 мкл концентрированного МЭА в испаритель хроматографа с помощью микрошприца . Затем аналогичным образом ввод т анализируемую пробу в количестве 1 - 2 мкл и при скорости потока газа-носител  гели  60 см /мин при температуре испарител Example. Analysis of glycolamine solution containing carbon dioxide, hydrogen sulfide and water is carried out on a chromatograph with a detector of heat conduction on a chromatographic column of stainless steel or glass 3 m long and 3 mm in diameter filled with Polysorb-1 modified by 2% 1,2,3-tris - {/ -cyanethoxy) propane. Before starting the analysis, the column is saturated with MEA by double injection of 1 - 2 μl of concentrated MEA into the chromatograph evaporator using a microsyringe. Then, the sample to be analyzed is injected in the same way in an amount of 1 to 2 µl and at a flow rate of the carrier gas helium 60 cm / min at an evaporator temperature

ОABOUT

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ю соyu so

СПSP

250°С, температуре термостата детектора 2ПО°С, температуре термостата детектора 200°С, температуре термостата колонок 60°С в изотермическом режиме фиксируютс  сигналы кислых газов. После выхода сероводорода начинаетс  подьем температуры (Тконечма  176°С) и наблюдают выход сигналов воды, МЭА и ДЭГа.250 ° C, the temperature of the thermostat of the detector 2PO ° C, the temperature of the thermostat of the detector 200 ° C, the temperature of the column thermostat 60 ° C in an isothermal mode, the signals of acid gases are fixed. After the release of hydrogen sulphide, the temperature rises (T-End 176 ° C) and the signals of water, MEA and DEG are observed.

На чертеже представлена хроматограм- ма гликольаминного раствора, содержащего воду и кислые компоненты.The drawing shows a chromatogram of a glycolamine solution containing water and acidic components.

На чертеже обозначено: 1 С02, 2 H2S, 3 Н20;4 МЭА, 5ДЭГ.In the drawing: 1 CO2, 2 H2S, 3 H2O, 4 MEA, 5DEG.

Ток детектора равен 120 тА, скорость диаграммной ленты вторичного прибора дл  диоксида углерода 1800, сероводорода и воды 720, МЭА 240, ДЭГа 60 мм/ч. Продолжительность анализа составл ет 35 мин. Массова  дол  каждого компонента определ етс  методом внутренней нормализации по формулеThe current of the detector is 120 mA, the speed of the graph tape of the secondary device for carbon dioxide 1800, hydrogen sulfide and water 720, MEA 240, DEG 60 mm / h. The analysis time is 35 minutes. The mass fraction of each component is determined by the method of internal normalization using the formula

г SlAl19° 28,КГ g SlAl19 ° 28, KG

где Si - площадь пика определ емого компонента , мм2 (при автоматическом обсчете условные единицы интегрирующего устройства );where Si is the peak area of the component being defined, mm2 (in case of automatic calculation, the conventional units of the integrating device);

KI - массовый коэффициент чувствительности данного компонента по отношению к стандарту (МЭА), определ емый по формулеKI is the mass sensitivity coefficient of this component in relation to the standard (MEA), determined by the formula

KiKi

ГП| SCT ГПгт S|GP | SCT GPGT S |

где mi - масса определ емого компонента в градуировочной смеси;where mi is the mass of the component being determined in the calibration mixture;

гпст масса стандарта (МЭА) в i радуиро- вочной смеси, г:gpst mass of standard (MEA) in i of the navigation mix, g:

5ст и Si - соответственно площади пиков стандарта (МЭА) и определ емого компонента, мм (условные единицы интегрирующего устройства).5CT and Si are, respectively, the peak areas of the standard (MEA) and the component to be determined, mm (conditional units of the integrator).

Дл  определени  массовых коэффициентов чувствительности готовили следующие градуировочные смеси: вода МЭА-ДЭГ, вода - МЭА - ДЭГ диоксид углерода и вода - МЭА - ДЭГ - сероводород. Смеси МЭА с ДЭГом готов т во флакончиках с м гкими пробками, в которые помещают в нужных соотношени х взвешенные с точностью до 0,02 г, перегнанные под вакуумом 97 98%- ные МЭА и ДЭГ, содержащие воду Каждую полученную смесь анализировали не менее 5 раз Оценку погрешности приготовлени  смесей провод т согласно МИ-216-80.To determine the mass sensitivity coefficients, the following calibration mixtures were prepared: water MEA-DEG, water - MEA - DEG carbon dioxide and water - MEA - DEG - hydrogen sulfide. Mixes of MEA with DEG are prepared in flasks with soft stoppers, into which weighted particles with accuracy up to 0.02 g, distilled under vacuum 97 are placed in the right ratios. 98 98% of MEA and DEG containing water Each mixture was analyzed at least 5 The evaluation error for the preparation of mixtures is carried out according to MI-216-80.

Дл  получени  градуировочных смесей вода МЭА ДЭГ- диоксид углерода и вода - МЭА - ДЭГ - сероводород во флакончики (не менее п ти) помещают раствор МЭА сTo obtain calibration mixtures, water MEA DEG - carbon dioxide and water - MEA - DEG - hydrogen sulfide in bottles (at least five) place the solution of MEA with

массовой долей 15% в ДЭГе, фиксируют массу раствора с точностью до 0,0002 г и с помощью стекл нного наконечника от пипетки , соединенного вакуумным шлангом с источником газа (аппарат Киппа или камера с диоксидом углерода), пропускают газ в каждый флакончик соответственно 1,2,3,4,5 мин. Массу поглощенного газа определ ют взвешиванием на аналитических весах, учитыва  поправку на уменьшениеmass fraction of 15% in DEG, fix the mass of the solution with an accuracy of 0.0002 g and using a glass tip from a pipette connected with a vacuum hose to a gas source (Kipp apparatus or carbon dioxide chamber), pass the gas into each vial correspondingly 1, 2,3,4,5 minutes The mass of the absorbed gas is determined by weighing on an analytical balance, taking into account the correction for reducing

массы диэтиленгликолевого раствора МЭА, оставшегос  на наконечнике, взвешива  последний до и после пропускани  газа. Каждую полученную смесь с сероводородом анализируют немедленно. Предварительно хроматографически определ ют степень чистоты диоксида углерода и сероводорода .the mass of diethylene glycol MEA solution remaining on the tip, weighing the latter before and after passing the gas. Each resulting mixture with hydrogen sulfide is analyzed immediately. The degree of purity of carbon dioxide and hydrogen sulfide is pre-chromatographed.

Получены следующие значени  массовых коэффициентов чувствительности.The following values of mass sensitivity coefficients were obtained.

Ксо20,89; Кн25 1,01, Кц2о 0,81; Кдэг 0.99 приXo20.89; Kn25 1.01, Cz2o 0.81; Cdag 0.99 at

КмЭА (стандарт) 1.CMEA (standard) 1.

Количественное содержание компонентов в пробе рассчитано методом внутренней нормализации и соответствует массовой до- ле, %: С02 0,86, H2S 0,30, Н20 1,68, МЭА 18,28, ДЭГа 78,88. Метод позвол ет проводить определение содержани  компонентов с массовой долей от 0,01 % и выше.The quantitative content of the components in the sample was calculated by the method of internal normalization and corresponds to the mass fraction,%: CO2 0.86, H2S 0.30, H2 1.68, MEA 18.28, DEG 78.88. The method allows to determine the content of components with a mass fraction of 0.01% and higher.

Улучшает услови  работы с вреднымиImproves working conditions with harmful

веществами, значительно уменьша  врем substances, significantly reducing the time

контактировани  с ними, и  вл етс  безопасным .contact with them is safe.

Claims (1)

Формула изобретени  Способ газохроматографического анализа органических растворов, содержащих воду и кислые компоненты, включающий введение анализируемой смеси в поток газа-носител , разделение ее на колонке с насадкой в виде твердого носител  с нанесенной на него жидкой фазой и последующее детектирование и регистрацию, отличающийс  тем, что, с целью повышени  селективности и безопасности способа и снижени  его трудоемкости, в качестве насадки колонки используют полисорб-1, модифицированный 2% 1,2,3-трис-( / -цианэтокти) пропана, а разделение на колонке ве последовательно в двух режимах: вначале изотермическом при 60°С, аClaims A gas chromatographic method for analyzing organic solutions containing water and acidic components, comprising introducing the analyzed mixture into a carrier gas stream, separating it on a column with a nozzle as a solid carrier with a liquid phase applied to it, and then detecting and recording, characterized in , in order to increase the selectivity and safety of the method and reduce its labor intensity, Polysorb-1 modified with 2% 1,2,3-tris- (/ -cyanoethoctyl) propane is used as a column nozzle, and ix to ve column successively in two modes: first, isothermal at 60 ° C, and затем в режиме ступенчатого программировани  с конечной температурой 17б°С.then in a step programming mode with a final temperature of 17b ° C. ЖF MUU 30 25 20 15 О 5MUU 30 25 20 15 О 5 ОABOUT
SU884364636A 1988-01-13 1988-01-13 Method of chromatographic analysis of organic solutions containing water and acid components SU1672351A1 (en)

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Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Нефт нна промышленность. Сборник НТИ. сер. Нефтепромысловое дело и транспорт нефти. Вып. 2. М., 1985. с. 22 23. Панина Л.И. и др. Полимерные носители дл газовой хроматографии. М , 1980. *

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