Research Of The Primary Screening Technology Of Toxic Components In Oil Sludge

Purification toxic substance in oil sludge was investigated in detail. At the same time, the research and analysis of the pre-treatment of these hazardous substances were carried out.The major investigated contents and results were listed below:(1) Three detection technologies including HS-GC-MS(Head space-gas chromatography–mass Spectrometer), GC-MS(Gas chromatography-mass spectrometer) and XRF(X-ray fluorescence spectrum),were used complete preliminary qualitative analysis. The results showed that by HS-GC-MS detected of oil sludge, the main volatile organic compounds were BTEXs and saturated hydrocarbons. For GC-MS detection, the toxic substances included acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene,pyrene and saturated hydrocarbons. After XRF detected, there are many kinds of metal elements in the sample. Different oil sludge exist about Cr, Cd, Pb, V and so on.The content of various metal elements need to be verified by further experiments.(2) An analytical method based on gas chromatography-mass spectrometry(GC-MS)developed for determining 16 kinds of polycyclic aromatic hydrocarbons(PAHs) in oil sludge.Three extraction methods including ultrasonic extraction(UE),soxhlet extraction(SE),supercritical fluid extraction(SFE), were compared for PAHs. The results showed that the recovery ranges were from 52.80% to149.66% of ultrasonic extraction, and about the soxhlet extraction, the recoveries were in the range of 60.20%~149.66%. For supercritical fluid extraction method, accept for acenaphthene and acenaphthylene had lower recovery and other target substances recovery in the 79.73%~111.03%.(3) 13 kinds of main BTEXs were selected for further studying, they are benzene,toluene,chlorobenzene, ethyltoluene, m-xylene, p-xylene, styrene, o-xylene, isopropylbenzene,4-ethyltoluene,1,2,4-trimethylbenzene,1,2,4,5-tetramethylbenzene,1,2,4-trichlorobenzene and by HS-GC-MS analysis. For BTEXS of the sample, the suitable assisted solution is the matrix correction fluid, the headspace equilibrium temperature is 80℃, the headspace equilibrium time is 40 min. The results indicated that the calibration curves had a good liner relationship(r2>0.9992) and the LOD were range0.009μg/L to 0.222 μg/L(S/N=3). The recovery rangeswere from 73.02% to 103.39%.with the RSD≤12.74% for 13 BTEXS. Therefore, the method was accurate, simple and rapid to analyze BTEXs in oil sludge.(4) A rapid detection method on 13 kinds of heavy metal from oil sludge were established by using ICP-AES. The precision of the sample tests RSD ≤ 3.87% for dissolution method, and RSD≤3.84% for microwave digestion method. The precision meet the challenge of analysis for two methods. The standard addition recovery of the dissolution method was 77.48%~116.65%. The standard addition recovery for HNO3-HCl-H2O2 system of microwave digestion method was 73.80%~113.86%. and, the standard addition recovery for HNO3-HCl-HF-H2O2 system of microwave digestion method was 83.88%~104.99%.