Co-detection method for trace organic impurities in complex water sample
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A technology of organic impurities and detection methods, applied in the field of environmental detection, can solve tedious and time-consuming problems
Inactive Publication Date: 2014-03-12
JILIN INST OF CHEM TECH
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Problems solved by technology
These methods require pretreatment of water samples to remove interferences, which is tedious and time-consuming, and requires the use of large amounts of organic solvents
SPE method can simplify sample processing, but still requires a series of adsorption and desorption processes
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Embodiment 1
[0015] Prepare a mixed aqueous solution of phenol and m-cresol in a 50 mL volumetric flask, the concentration of phenol is 3.06 mg / L, and the concentration of m-cresol is 0.10 mg / L. After mixing evenly, take 4 mL of the mixed solution in the extraction bottle, add a stirring bar, Stir at 40°C for 20 min, take out the solid-phase microextraction device, place it in the gas chromatographic inlet, perform high-temperature thermal desorption and detect it in the gas chromatograph, the chromatogram is as follows figure 1 shown.
Embodiment 2
[0017] Prepare mesityl oxide, 3-methylcyclopentanone, and acetophenone aqueous solution in a 50 mL volumetric flask, the concentration of mesityl oxide is 0.08 mg / L, the concentration of 3-methylcyclopentanone is 0.09 mg / L, The concentration of acetophenone is 0.21 mg / L. After mixing evenly, take 4 mL of the mixed solution into the extraction bottle, add a stirring bar, stir at 40°C for 20 min, take out the solid-phase microextraction device, and place it in the gas chromatography inlet. After high-temperature thermal desorption, it is detected in gas chromatography, and its chromatogram is as follows: figure 2 shown.
Embodiment 3
[0019] Prepare phenol, m-cresol, mesityl oxide, 3-methylcyclopentanone, and acetophenone aqueous solution in a 50 mL volumetric flask, the concentration of phenol is 1.53 mg / L, and the concentration of m-cresol is 0.05 mg / L, The concentration of mesityl oxide is 0.04 mg / L, the concentration of 3-methylcyclopentanone is 0.05 mg / L, and the concentration of acetophenone is 0.11 mg / L. After mixing evenly, take 4 mL of the mixed solution in the extraction bottle, add Stirring bar, stirred at 40°C for 20 min, took out the solid-phase microextraction device, placed it in the gas chromatographic inlet, and carried out high-temperature thermal desorption and then detected it in the gas chromatograph. The chromatogram is as follows: image 3 shown.
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Abstract
The invention discloses a co-detection method for trace organic impurities (phenols and ketone) in a complex water sample, belonging to the field of environment analysis. According to the co-detection method, a headspace solid phase micro-extraction and gas chromatography coupling technology is utilized for carrying out qualitative and quantitative analysis on the trace organic impurities in water. The method is characterized in that solid phase micro-extraction and high-temperature desorption are carried out before the sample is analyzed by a gas chromatography; a solid phase micro-extraction head is carboxyethyl-polydimethylsiloxane fibers; a coating thickness is 30-100 microns, an extraction temperature is 30-70 DEG C, a rotary speed is 200-400 revolutions, extraction time is 15-45 minutes, a desorption temperature is 220-250 DEG C and desorption time is 30-150 seconds. The co-detection method can be used for analyzing the various impurities in the water sample simultaneously and is applicable to analyzing the trace organic impurities. The method has the advantages of convenience in operation, low cost, high precision and the like and has very important meanings on further researching on organic pollution components in the water and improving the water quality testing.
Description
technical field [0001] The invention relates to an analysis method for trace organic impurities in complex water samples, belonging to the technical field of environmental detection. Background technique [0002] In recent years, with the rapid development of the industrial field, more and more pollutants are emitted to nature. The discharge of these pollutants will have a great impact on the environment and people's lives. Some of the pollutants are carcinogenic. Reproductive toxicity, endocrine disrupting toxicity, etc. Therefore, it is very necessary to establish a simple, rapid, accurate, and highly selective water quality detection method for the study of environmental pollution by organic compounds. [0003] At present, the commonly used concentration and enrichment methods include liquid-liquid extraction (L-L), solid phase extraction (SPE) and so on. These methods require pretreatment of water samples to remove interferences, which is tedious and time-consuming, an...
Claims
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