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Method for measuring trace chloride ions in methanol

A determination method and technology for chloride ions, which are used in measurement devices, material separation, instruments, etc., to achieve the effects of good reproducibility, sensitive method and high precision

Inactive Publication Date: 2011-04-13
SHAANXI SHENMU CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the problems existing in the prior art, solve the measurement problem of trace chlorine in the organic matter (methanol), that is to say, carry out pretreatment to sample, eliminate organisms, and the sample is concentrated to provide a method for the determination of trace chloride ions in methanol

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  • Method for measuring trace chloride ions in methanol
  • Method for measuring trace chloride ions in methanol
  • Method for measuring trace chloride ions in methanol

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Analysis of standard samples:

[0031] According to the solution preparation method in the embodiment, the rinse stock solution, the rinse use solution, the sodium chloride standard stock solution, and the standard use solution are prepared.

[0032] Follow the operation steps of the ion chromatograph, turn on the machine, connect the instrument, set parameters, etc. in sequence. After the instrument parameters are adjusted, the pump can be started. First, rinse the flow path of the instrument with degassed deionized water for about fifteen minutes. Then turn off the pump and replace with eluent, and turn on the pump. Adjust the current to around 50mA. After fifteen minutes, the baseline is collected. If the baseline is stable and the baseline is stable within 100mv, it can be analyzed.

[0033] Determination and calibration of standard points: After the instrument is stable, use the prepared standard liquid for sample injection analysis (its concentration is close ...

Embodiment 2

[0039] Analysis of Methanol Samples:

[0040] According to the solution preparation method in the embodiment, the rinsing stock solution, the rinsing use solution, the sodium chloride standard stock solution, and the use solution are prepared.

[0041] According to the content of the invention, the sample is processed: take 100ml of methanol sample in an evaporating dish, add 10-20ml of washing solution, and evaporate in a 70°C water bath until the methanol is basically evaporated to dryness. Transfer to a 100ml volumetric flask, dilute to the mark with eluent and mix well for later use.

[0042] Follow the operation steps of the ion chromatograph, turn on the machine, connect the instrument, set parameters, etc. in sequence. After the instrument parameters are adjusted, the pump can be started. First, rinse the flow path of the instrument with degassed ultrapure water for about fifteen minutes. Then turn off the pump and replace with eluent, and turn on the pump. Adjust t...

Embodiment 3

[0049] Sample + standard sample (do standard recovery test):

[0050] According to the solution preparation method in the embodiment, the rinse stock solution, the rinse use solution, the sodium chloride standard stock solution, and the working solution are prepared.

[0051]According to the content of the invention, the sample is processed: take 100ml of methanol sample in an evaporating dish, add 10-20ml of rinse solution, and add 0.05mg of standard sample at the same time, evaporate in a 70°C water bath until the methanol is basically evaporated to dryness. Transfer to a 100ml volumetric flask, dilute to the mark with eluent and mix well for later use. Put the injection valve handle at the load position, inject the sample with a syringe, the injection volume should not be less than 1ml, and then pull the injection valve handle to the analysis (inject) position to complete a sample injection process. (Before sample injection and analysis, first clean the injection valve wit...

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Abstract

The invention relates to the field of analysis and measurement of trace ions in the methanol industry, in particular to a method for measuring trace chloride ions in methanol. The method comprises the steps of: firstly, preparing an elution stock solution, an elution working solution, a sodium chloride standard stock solution and a chloride ion standard working solution from deionized water for later use, then adding an elution solution into a methanol sample and evaporating to dryness, removing organic matters, concentrating and metering volume, finally taking the treated methanol sample, measuring the chloride ions in the methanol through an ion chromatograph, and carrying out data processing and analysis. The invention can accurately analyze chlorides above 10ppb in a methanol product and determine whether to provide the methanol product to a high-end user according to the content so as to increase stable high-end user sources and client satisfaction degrees for enterprises.

Description

Technical field [0001] The invention relates to the field of analysis and determination of trace ions in the methanol industry, in particular to a method for measuring trace chloride ions in methanol. Background technique [0002] With the continuous increase of methanol production capacity, customers have increasingly stringent requirements on the quality of methanol. In addition to the inspection items required by national standards, some high-end users have also put forward requirements for the content of chloride ions in methanol. Since the national standard does not require the content of chloride ions in methanol, there is currently no clearly defined analysis method. Traditional analysis methods include turbidimetry, electrode potential method, titration method, etc., and the measurement range is mostly above 1mg / L, such as the range of silver method is 5-500mg / L, the range of mercury method is 1-100mg / L, ion selective electrode Method 9-1000mg / L, detection limit of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14G01N30/08
Inventor 李芳黄晔叶春芙
Owner SHAANXI SHENMU CHEM IND
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