Method for measuring hydrogen sulfide content in desulfurized amine

A technology of desulfurization amine solution and determination method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of reduced absorption efficiency, long analysis time, poor repeatability and accuracy, and achieve reduced production costs, stable chromatographic baseline, The effect of saving purchase cost

Active Publication Date: 2013-12-11
CHINA PETROLEUM & CHEM CORP
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  • Application Information

AI Technical Summary

Problems solved by technology

The lean liquid can be recycled, and the hydrogen sulfide content in it is too high, which will reduce the absorption efficiency and affect the desulfurization effect. Therefore, it is necessary to control and analyze the hydrogen sulfide content in the lean liquid
[0003] At present, the analysis of hydrogen sulfide content in desulfurized amine solution mainly adopts the iodometric method. The method is cumbersome and needs to be titrated twice to measure a sample; the analysis time is long, and it takes about 30 minutes to analyze a sample; there are many interference factors, repeatability and accuracy Poor performance; the sample has an unpleasant smell and is highly toxic to analysts
Because the content of hydrogen sulfide in the lean liquid is very low, the control index is less than 2g / L, and the hydrogen sulfide content in the lean liquid is determined by direct injection chromatography, because the sensitivity of the thermal conductivity cell detector (TCD) is not high, plus When the content of hydrogen sulfide is very low, it binds firmly with methyldiethanolamine, and the sample cannot be completely decomposed into hydrogen sulfide in the gasification chamber after sample injection, resulting in the undetected results of most samples
Use direct injection chromatography to analyze the poor solution, the sample will pollute the chromatographic column and the injection port, the chromatographic baseline will be unstable, and continuous analysis cannot be performed. Therefore, it is not suitable to use the direct injection chromatography to determine the poor solution

Method used

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  • Method for measuring hydrogen sulfide content in desulfurized amine
  • Method for measuring hydrogen sulfide content in desulfurized amine
  • Method for measuring hydrogen sulfide content in desulfurized amine

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 1. Instruments and reagents

[0018] 6820 gas chromatograph with TCD detector (Agilent); Porapak S, 3 m × 1 / 8 inch (OD) stainless steel column (Agilent); 5 mL gas-tight syringe with lock valve; 10 μL manual Syringe (Agilent); 100μL syringe, 2mL domestic syringe; 20mL headspace bottle and bottle cap, sealing clamp (Agilent).

[0019] Hydrogen sulfide standard gas: hydrogen sulfide content is 9.57%, nitrogen is the base gas (Foshan Kedi Gas Co., Ltd.); methyldiethanolamine (imported); 30% dilute sulfuric acid solution (volume ratio, self-prepared).

[0020] 2. Chromatographic operating conditions

[0021] Through a large number of experiments, the chromatographic operating conditions are determined as follows: the carrier gas is hydrogen; the flow rate of the carrier gas is 15 mL / min, the flow rate of the auxiliary gas is 1 mL / min, and the reference gas is 50 mL / min; The temperature is 180°C; the range is 0, and the injection volume is 50 μL (when the concentra...

Embodiment 2

[0040] Use a 2mL pipette to take 2mL of the sample into a 20mL headspace bottle, and seal the bottle cap with a bottle clamp. Take 2mL of 18% (by weight) dilute hydrochloric acid solution with a domestic syringe, inject it into a sealed headspace sampling bottle, shake it repeatedly, let it stand, and cool it to room temperature. Measure the peak area of ​​hydrogen sulfide in the headspace gas phase component of the sample according to the method for measuring the standard solution, and calculate the content of hydrogen sulfide in the sample according to the correction factor of hydrogen sulfide in the standard solution. When using the standard solution to calibrate the instrument and measure the correction factor of hydrogen sulfide in the standard solution, the added dilute acid is 2mL of 18% (weight ratio) dilute hydrochloric acid, and the others are the same as in Example 1.

Embodiment 3

[0042] Use a 2mL pipette to take 2mL of the sample into a 20mL headspace bottle, and seal the bottle cap with a bottle clamp. Use a domestic syringe to take 2mL of 34% (volume ratio) dilute phosphoric acid solution, inject it into a sealed headspace sampling bottle, shake it repeatedly, let it stand, and cool it to room temperature. Measure the peak area of ​​hydrogen sulfide in the sample according to the method for measuring the standard solution, and calculate the content of hydrogen sulfide in the sample according to the correction factor of hydrogen sulfide. When using the standard solution to calibrate the instrument, when measuring the correction factor of hydrogen sulfide in the standard solution, the added dilute acid is 2mL of 34% (volume ratio) dilute phosphoric acid, and the others are the same as in Example 1.

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Abstract

The invention relates to a method for measuring hydrogen sulfide content in desulfurized amine, which is used for measuring the hydrogen sulfide content in the desulfurized amine for refining and chemical enterprises. The method comprises the following steps of: adding a sample into a headspace bottle, sealing, adding dilute acid, shaking uniformly, and reacting the dilute acid with the sample to separate out hydrogen sulfide; standing, cooling to room temperature, performing chromatographic analysis on a headspace gas-phase component, and detecting by using a thermal conductivity cell detector; and calculating the hydrogen sulfide content in a barren solution in the desulfurized amine by using hydrogen sulfide standard gas configuration and a standard liquid calibrator according to the hydrogen sulfide content in a standard liquid, a peak area of the headspace gas-phase component hydrogen sulfide, and a peak area of a headspace gas-phase component hydrogen sulfide of the sample. By the method, the analysis is quick, and a chromatographic column and an injection port are prevented from being polluted by the sample and impurities, so that a chromatogram baseline is stable, peak shapes of hydrogen sulfide are symmetric, the interference of other substances on analysis is eliminated, and the analysis accuracy is improved.

Description

technical field [0001] The invention relates to the determination of the hydrogen sulfide content in the desulfurized amine liquid of refining and chemical enterprises, and is especially suitable for the determination of the hydrogen sulfide content in the barren liquid. Background technique [0002] The desulfurization amine solution contains methyldiethanolamine (desulfurizer), water, hydrogen sulfide and ferrous sulfide and other sulfides, carbon dioxide, hydrocarbon gas, oily substances, thermally stable salts and solid sundries, etc. The sample is dirty and Smelly, darker in color, and more complex in composition. The desulfurization amine solution is divided into rich solution and lean solution. The rich solution has a relatively high hydrogen sulfide content and becomes a lean solution after heating and decomposing hydrogen sulfide. The lean solution has a relatively low hydrogen sulfide content and becomes a rich solution after absorbing hydrogen sulfide. The lean l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 单石文曾运星黎仕克刘宁
Owner CHINA PETROLEUM & CHEM CORP
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