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

2 Cites 5 Cited by

AI-Extracted Technical Summary

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...

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.

Application Domain

Component separation

Technology Topic

Chromatographic columnChloral +15

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Examples

Experimental program(4)

Example Embodiment

[0024] Example 1

[0025] In the present invention, the initial temperature of the chromatographic column of the gas chromatograph is room temperature, the temperature rise rate is 10°C/min to a temperature of 100-200°C, and the carrier gas flow rate is 1 to 3 mL/min. In order to meet the complete separation of the peaks of the internal standard substance and all components in the sample, combined with the boiling point of each substance, the optimal chromatographic analysis conditions are determined 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; Detector temperature: 240°C; Detector: FID detector.

Example Embodiment

[0028] Example 2

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

[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. After shaking, add it to a 10mL volumetric flask, and add ethanol to make the volume up to the mark. After shaking well, a 20 mg/mL p-xylene solution was obtained.

[0031] (3) Determination of the retention time of organic matter: Take 0.5mL of the 20.0g/L standard solution and internal standard solution, mix them uniformly, and use a syringe to inject the sample into the chromatograph for qualitative analysis to obtain the solvent under the above chromatographic conditions The retention time of ethanol, chloroacetaldehyde, p-xylene, ethyl trichloroacetate, diethyl sulfate, nitrobenzene and other organic substances, the results are as attached figure 1 Shown.

Example Embodiment

[0032] Example 3

[0033] Standard curve drawing: chromatographic column with carrier gas N 2 After aging for 24 hours, pass gas H 2 And supporting gas (compressed air), gas H 2 The volume ratio of the gas to the combustion-supporting gas is controlled at 1:10, and the parameters of the gas chromatograph are adjusted as shown in the embodiment, and the ignition is performed after a constant temperature for half an hour. Measure the 2mL standard solution and 1mL internal standard solution prepared in Example 2 respectively, add them to a 5mL volumetric flask, dilute to the mark with ethanol, mix well, use a 0.5μL micro-injector to take 0.4μL of the mixed solution, and use Analyze by gas chromatography, draw a standard curve based on the data obtained by N2000 chromatographic workstation, and take the average value after 5 injections of a group of samples for parallel analysis. i /m S (The ratio of the mass of the sample to the mass of the internal standard) and A i /A S (The ratio of the peak area of the sample to the peak area of the internal standard) as a function to obtain the standard curve, as attached figure 2 Shown.

[0034] Table 1 Standard curve of chloroacetaldehyde

[0035]

[0036] Table 2 Standard curve of ethyl trichloroacetate

[0037]

[0038] Table 3 Standard curve of diethyl sulfate

[0039]

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Classification and recommendation of technical efficacy words

Fast separation

Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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