| Monochloronaphthalene is an important part of Polychlorinated naphthalenes(PCNs).Since the 1980 s,it was mass-produced by the industry and applied to the power industry and surface packaging,such as insulating oils,flame retardants,lubricants,plasticizing and so on.PCNs(including monochloronaphthalene)has been ceased from the production and the use in the world since the 1980 s.China has no experience in producing monochloronaphthalene and the currently existing monochloronaphthalene mainly comes from unintentional generation process such as waste incinerations,synthesis of organic chlorides,waste metal recycling and other industrial procedures.Long term exposuring to high-concentration monochloronaphthalene could cause sensitive toxicity.Environmental research of monochloronaphthalene has been a hot topic on environmental issues.However,there is not yet a unified standard analysis method.On the basis of literature research,this paper determines the principle of the method,specifies the sampling method,the selection of internal standard(naphthalene-d8),preparating a standard calibration curve and optimizing the instrumental conditions.The results showed that the instrument detection limit of monochloronaphthalene and linear range concentration range were 2 ?g/L,10-40000 ?g/L,respectively.The different parameters were examined to reduce interference.Blank samples of activated carbon and solvent were designed to ensure that the analytical method meet the quality control and quality management requirements.The evaluation on method performance of PCN-1 and PCN-2 including sample pretreatment and instrument analysis using gas chromatography-mass spectrometry(GC/MS),inducated that the method detection limits,accuracy and precision,were satisfied with the requirements by comparing with the US EPA 23 and CHN HJ 77.2-2008 methods for PCDD/Fs analysis.By examining parameters such as methods for elution of target material in sampling medium,penetration efficiency of sampling tube,purification method of extraction liquid,concentration condition of solvent,and interference of blank.It was found that the control of evaporation conditions was particularly important to(1)sampling method section;(2)volatile monochloronaphthalene.The obtained results showed that the purification procedure using acid silica gel was beneficial to the removal of matrix interference.For the sample evaporation,the speed of the solvent effluent was controlled at one drop/second when using rotary evaporation,and nitrogen blow was gentle with no solvent disturbance.With no significant difference in the retention time deviation of PCN-1 and PCN-2.The minimum and maximum deviation values were-0.099 min and 0.068 min,respectively.Universally,when the absolute deviation of the retention time was less than ±0.10 min,the instrumental analysis of monochloronaphthalene was reproducinle.From the examination on time and temperature of storage by using spiked standard,it was found that monochloronaphthalene had strong volatility and could not be stored for long time and at high temperatures.At-2 ?,4 ? and 30 ?,the recoveries of monochloronaphthalene for 3 days were 78.3%-92.1%,78.4%-87.0% and 75.1%-90.7%,respectively.The relative standard deviations were less than 20%.The results met the requirements by comparing with the US EPA 23 and CHN HJ 77.2-2008 methods for PCDD/Fs analysis.The developed method was applied for the analysis of spiked smoke matrix samples.Results from method blank,method detection limit,accuracy and precision were used to veridate the method performance.Recovery of PCN-1 and PCN-2 were 72.0%-97.0%,75.7%-107.0%,respectively.The relative standard deviations were 0.8%-6.2% and 0.6%-6.8%,respectively.Furthermore,the method was successfully applied for the analysis of the samples from petrochemical industry,household garbage,medical waste,and hazardous waste incineration for the levels of monochloronaphthalene in various flue gas samples. |
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