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),

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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
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1

[0030] Analysis of standard samples:

[0031] 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 standard use solution are prepared.

[0032] According to the operation steps of the ion chromatograph, turn on the instrument, connect the instrument, and set parameters in sequence. After the instrument parameters are adjusted, the pump can be turned on. First flush the flow path section of the instrument with degassed deionized water for about fifteen minutes. Then turn off the pump, replace with the eluent, and turn on the pump. Adjust the current to around 50mA. Fifteen minutes later, the baseline was collected. If the baseline was stable, and the baseline was stable within 100mv, the analysis could be performed.

[0033] Determination and calibration of standard points: After the instrument is stable, inject and analyze with the prepar...

Example Embodiment

[0038] Example 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] Process the sample according to the content of the invention: take 100ml of sample methanol in an evaporating dish, add 10-20ml of rinsing liquid, 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 using solution and mix well for later use.

[0042] According to the operation steps of the ion chromatograph, turn on the instrument, connect the instrument, and set parameters in sequence. After the instrument parameters are adjusted, the pump can be turned on. First flush the flow path section of the instrument with degassed ultrapure water for about fifteen minutes. Then turn off the pump, replace with ...

Example Embodiment

[0048] Example 3

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

[0050] 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 working solution are prepared.

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

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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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