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Capillary column gas chromatography method for N-methyldiethanolamine decarbonizer component

A methyldiethanolamine decarburizing agent and gas chromatography analysis technology, which is applied in the field of capillary gas chromatography analysis, can solve the problems of not being able to simultaneously analyze MDEA and PIP at the same time, poor anti-interference ability, cumbersome pretreatment, etc. Accurate results and fast analysis

Inactive Publication Date: 2013-07-10
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above methods have disadvantages such as cumbersome pre-processing and poor anti-interference ability, and cannot simultaneously analyze MDEA and PIP at the same time, which cannot meet the requirements of current industrial production.

Method used

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  • Capillary column gas chromatography method for N-methyldiethanolamine decarbonizer component
  • Capillary column gas chromatography method for N-methyldiethanolamine decarbonizer component
  • Capillary column gas chromatography method for N-methyldiethanolamine decarbonizer component

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1) Gas chromatography conditions:

[0050] Gas chromatograph: Shimadzu GC2010;

[0051] Chromatographic column: Rtx-5 capillary column (30m×0.25mm i.d×0.25μm);

[0052] Column temperature: 80°C, hold for 0min, then program temperature rise to 100°C at 10°C / min, hold for 0min; program temperature rise to 150°C at 20°C / min, hold for 0min; ℃, keep 0min;

[0053] Injection port temperature: 270°C;

[0054] Hydrogen flame ion detector temperature: 320°C;

[0055] Carrier gas: high-purity nitrogen;

[0056] Column flow rate: 1.03mL / min (constant flow);

[0057] Makeup flow rate: 30mL / min;

[0058] Hydrogen flow rate: 40mL / min;

[0059] Air flow rate: 400mL / min;

[0060] Split ratio: 49:1;

[0061] Injection volume: 1μL;

[0062] 2) Preparation of standard curves for N-methyldiethanolamine and piperazine: Accurately weigh 1.0000g of N-methyldiethanolamine and 1.0000g of piperazine in a beaker, and set the volume to 100mL as the standard stock solution. Standard stoc...

Embodiment 2

[0066] 1) Gas chromatography conditions:

[0067] Gas phase-mass spectrometer: Shimadzu GC-MS2010Plus;

[0068] Chromatographic column: DB-5 capillary column (30m×0.25mm i.d×0.25μm);

[0069] Column temperature: 80°C, hold for 0min, then program temperature rise to 100°C at 10°C / min, hold for 0min; program temperature rise to 150°C at 20°C / min, hold for 0min; ℃, keep 0min;

[0070] Injection port temperature: 270°C;

[0071] Mass spectrometry conditions: EI ion source, temperature 200°C; electron energy: 70eV; scan mode: full scan mode, scan range m / z: 10-510, database: NIST27.LIB, WILEY7.LIB;

[0072] Carrier gas: high-purity nitrogen;

[0073] Column flow rate: 1.03mL / min (constant flow);

[0074] Makeup flow rate: 30mL / min;

[0075] Hydrogen flow rate: 40mL / min;

[0076] Air flow rate: 400mL / min;

[0077] Split ratio: 49:1;

[0078] Injection volume: 1μL;

[0079] 2) Preparation of standard curves for N-methyldiethanolamine and piperazine: Accurately weigh 1.0000g...

Embodiment 3

[0082] 1) Gas chromatography conditions:

[0083] Chromatograph: Agilent-7890A;

[0084] Chromatographic column: HP-5 capillary column (30m×0.25mm i.d×0.25μm);

[0085] Column temperature: 80°C, hold for 0min, then program temperature rise to 100°C at 10°C / min, hold for 0min; program temperature rise to 150°C at 20°C / min, hold for 0min; ℃, keep 0min;

[0086] Injection port temperature: 270°C;

[0087] Hydrogen flame ion detector temperature: 320°C;

[0088] Carrier gas: high-purity nitrogen;

[0089] Column flow rate: 1.03mL / min (constant flow);

[0090] Makeup flow rate: 30mL / min;

[0091] Hydrogen flow rate: 40mL / min;

[0092] Air flow rate: 400mL / min;

[0093] Split ratio: 49:1;

[0094] Injection volume: 1μL;

[0095] 2) Preparation of standard curves for N-methyldiethanolamine and piperazine: Accurately weigh 1.0000g of N-methyldiethanolamine and 1.0000g of piperazine in a beaker, and set the volume to 100mL as the standard stock solution. Standard stock solut...

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Abstract

The invention relates to a capillary column gas chromatography method for an N-methyldiethanolamine decarbonizer component. Gas chromatography conditions of the method comprise: a column temperature of 280 DEG C; an introduction port temperature of 270 DEG C; a detector temperature of 320 DEG C; a column flow rate of 1.03 mL / min; and a split ratio of 49:1. Heating procedures of the column temperature comprise: maintaining a temperature of 80 DEG C for 0 min; then heating to a temperature of 100 DEG C at a rate of 10 DEG C / min and maintaining the temperature of 100 DEG C for 0 min; heating to a temperature of 150 DEG C at a rate of 20 DEG C / min and maintaining the temperature of 150 DEG C for 0 min; and heating to a temperature of 280 DEG C at a rate of 50 DEG C / min and maintaining the temperature of 280 DEG C for 0 min. The gas chromatography conditions further comprise: a make-up flow velocity of 30 mL / min, a hydrogen flow velocity of 40 mL / min and an air flow velocity of 400 mL / min, The method provided by the invention is accurate, sensitive, easy and convenient, has high separation efficiency, does not need derivatization and pretreatment, shows a fast analysis speed and can totally satisfy quality inspection requirements of actual production in the process of production quality inspection in a factory.

Description

technical field [0001] The invention relates to a capillary gas chromatography analysis method for components of an N-methyldiethanolamine decarburizing agent. Background technique [0002] MDEA (N-methyldiethanolamine) decarburization and desulfurization agent is widely used in refinery tail gas dehydrogenation 2 Decarbonization and purification of acid gases in mixed gases such as S and natural gas, oilfield gas, synthesis gas and coal gas, and can absorb H well under certain conditions 2 S, CO 2 and other acid gases. Its main component is N-methyldiethanolamine. The concentration of N-methyldiethanolamine is generally 15%~50%, the water content is 0.99%~26.58%, and the general index requires the water content to be ≤1%. If it is greater than 1%, it can be supplemented by the manufacturer according to the requirements of the index. At present, my country's petrochemical enterprises mostly use the active MDEA solution patented by BASF, the model is aMDEA03, the concent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 赖宏萍黎曙新陈军华薛爱玲郭显璐佟志鹏刘勇万伟张彦代杰杨甲强毛辉陶冬梅滑晓燕
Owner PETROCHINA CO LTD
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