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Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid

A technology of trichloroacetaldehyde and analysis method, which is applied in the field of analytical chemistry, can solve the problems of no analysis of trichloroacetic acid content, high sampling requirements, single determination, etc., and achieve the effect of rapid detection, high separation efficiency and accurate quantification

Inactive Publication Date: 2015-04-08
NANNING CHEMICAL INDUSTRY CO LTD
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Problems solved by technology

Alkalimetric chemical analysis is simple and fast, suitable for the determination of high concentrations of trichloroacetaldehyde, and due to the presence of ethyl trichloroacetate, dichloroacetaldehyde, and monochloroacetaldehyde, the results are too high, so it is not suitable for the analysis of low-concentration waste Chloral in sulfuric acid; Determination of trace chloral in waste sulfuric acid by the pyrazolone spectrophotometric method based on the State Environmental Protection Administration (HJ / T50-1999), which is more stable in color than the pyridine alkali method and has high precision , but only single determination of chloral in waste sulfuric acid of chloral; high performance liquid chromatography detection can accurately and sensitively determine chloral in the air of the workplace, but this method has high sampling requirements and complicated process , and is suitable for determining the content of chloral in the air of the workplace; gas chromatography is suitable for the determination of low-concentration chloral in water or waste sulfuric acid, using external standard method and using n-hexane, n-octane, etc. The internal standard method, which is an internal standard, is simple to operate and accurate in quantification. It is more suitable for the determination of low-concentration organic compounds in sewage or waste sulfuric acid from pesticide factories. The content of acetaldehyde, the content of other organic substances such as trichloroacetic acid, ethyl trichloroacetate and diethyl sulfate were not analyzed

Method used

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  • Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid
  • Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid
  • Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid

Examples

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Embodiment 1

[0025] The initial temperature of the chromatographic column of the gas chromatograph in the present invention is room temperature, the temperature is raised to 100-200°C at a heating rate of 10°C / min, and the carrier gas flow rate is 1-3mL / min. In order to meet the complete separation of the peaks of the internal standard and all the components in the sample, combined with the boiling point of each substance, determine the optimal chromatographic analysis conditions as follows:

[0026] Chromatographic analyzer analysis conditions

[0027] Chromatographic column: 30m×0.32mm SE-54 chromatographic column; carrier gas: N 2 ; Carrier gas flow rate: 1mL / min; Chromatographic column temperature: 120°C; Injection volume: 0.4μL; Vaporization chamber temperature: 250°C;

Embodiment 2

[0029] (1) Preparation of standard solution: Dissolve 0.10g, 0.20g, 0.30g, 0.40g, and 0.50g of chloral in ethanol and add it to a 10mL volumetric flask. Chloroacetaldehyde standard solution. The standard solution preparation method of ethyl trichloroacetate and diethyl sulfate is the same as the preparation method of chloral standard solution.

[0030] (2) Preparation of internal standard solution: Accurately weigh 0.20 g of p-xylene, add it to a beaker, and add an appropriate amount of ethanol. Shake well and add to a 10mL volumetric flask, add ethanol to make up to the mark. After shaking and shaking, a 20 mg / mL p-xylene solution was obtained.

[0031] (3) Determination of the retention time of organic matter: take 0.5 mL each of the above-mentioned 20.0 g / L standard solution and internal standard solution, mix well, inject a sample into the chromatograph with a syringe, carry out qualitative analysis, and obtain the solvent under the above-mentioned chromatographic condit...

Embodiment 3

[0033] The drawing of the standard curve: the chromatographic column is passed through the carrier gas N 2 After aging for 24 hours, pass gas H 2 And auxiliary gas (compressed air), gas H2 The volume ratio with the supporting gas is controlled at 1:10, adjust the parameters of the gas chromatograph as shown in the examples, and ignite after constant temperature for half an hour. Measure 2mL of the standard solution and 1mL of the internal standard solution prepared in Example 2 respectively, add them to a 5mL volumetric flask, dilute to the mark with ethanol, mix evenly, take 0.4 μL of the mixed solution with a 0.5 μL microsampler, and use Analyzed by gas chromatography, draw a standard curve according to the data obtained by the N2000 chromatographic workstation, after a group of samples are injected 5 times for parallel analysis, take the average value, according to m i / m S (the ratio of the mass of the sample to the mass of the internal standard substance) and A i / A S...

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Abstract

The invention discloses an analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid. The analysis method comprises the following steps: firstly, extracting organic matters in the trichloracetic aldehyde waste sulfuric acid with nitrobenzene; carrying out gas chromatography quantitative analysis on the organic matters in the trichloracetic aldehyde waste sulfuric acid by virtue of a gas chromatograph and a hydrogen hydrogen flame ionization detector by adopting paraxylene as an internal standard substance under the condition that the chromatographic column temperature of the gas chromatograph is 100-200 DEG C and the flow rate of carrier gas is 1-3mL / min; and accurately detecting the content of the organic matters such as trichloracetic aldehyde, trichloroacetic acid, diethyl sulfate and ethyl trichloroacetate in the trichloracetic aldehyde waste sulfuric acid. The method disclosed by the invention is easy to operate, accurate to quantify, and rapid to detect; the quantitative result is irrelevant to the sample amount within the range that a chromatographic column does not overload; the content of the organic matters can be quantified as long as a detected substance and the internal standard substance are out of the peak and can be completely separated.

Description

technical field [0001] The present invention belongs to the field of analytical chemistry. Specifically, it is an analysis method for organic matter in chloral waste sulfuric acid, and in particular relates to a method for quantitatively analyzing organic matter in chloral waste sulfuric acid by using a gas chromatography internal standard method. Background technique [0002] Chloral is an important pesticide intermediate and the main raw material of trichlorfon, a backbone pesticide necessary for agricultural production. my country's chloral production currently adopts the process route of multi-stage ethanol chlorination and concentrated sulfuric acid dehydration, and a large amount of waste sulfuric acid containing organic impurities such as chloral (acid) will be produced in the production process. The concentration of sulfuric acid in waste sulfuric acid is 60% to 70%, and the content of organic impurities is 4% to 15%, mainly chloral, trichloroacetic acid, ethyl trich...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 秦祖赠覃卫国陈军龙锋
Owner NANNING CHEMICAL INDUSTRY CO LTD
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