Analysis method of organic matters in trichloracetic aldehyde waste sulfuric acid

[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.

[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 fo

[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