(1) Method for determining heavy metal content of oil sludge
The content of heavy metals in oil sludge was determined by inductively coupled plasma mass spectrometry after atmospheric pressure digestion; the digestion procedure of sludge was referred to CJ/221-2005 municipal sewage treatment plant sludge test method.
(2) Analysis method of oil phase components of oil sludge
The oil phase components of the oil sludge were analyzed by total hydrocarbon gas chromatography. The analysis was carried out with reference to SY/T 5779-2008 petroleum and sedimentary organic hydrocarbon gas and chromatographic method. The instrument was tested by Agilent 7890A gas chromatograph. It is a high purity nitrogen gas (99.999%), an inlet temperature of 300 ° C, and a detector FID temperature of 300 ° C. The carrier gas flow rate was constant flow 1 ml/min, split injection, and the split ratio was 20:1. Column: HP-1 elastic quartz capillary column (60m x 0.25mm x 0.25um); Guiwen: initial temperature 40 ° C, hold for 10min, 4 ° C warm to 70 ° C, then increase the temperature to 300 ° C at 8 ° C / min, Keep it for 40 minutes.
The oil phase components used in the analysis were extracted by Soxhlet extraction, and the extraction reagent was CH2Cl2. The extraction temperature was 40 ° C and the extraction time was 72 h. The oil phase used for the analysis obtained after extracting the extractant by steaming off the obtained liquid by a rotary evaporator.
(3) Analysis method of slag phase composition of oil sludge
The composition analysis of the oil sludge slag phase was analyzed by X-ray diffractometer and X-ray fluorescence spectrometer. The test instrument was analyzed for solid products using a D8FOCUS XRD diffractometer from AXS, Germany, and a LAB CENTRE XRF-1800 XPF spectrometer from SHADIZU, Japan. The test sample is prepared as follows: the slag phase component obtained after the oil sludge is extracted is subjected to dry grinding and the test sample is prepared by a 325 mesh (44 um) sample.
(4) Thermogravimetric analysis method for oil sludge
The thermogravimetric analysis of the oil sludge was carried out by the STA7300 type thermogravimetric differential thermal analyzer manufactured by HITACHI Co., Ltd., and the TG and DTG curves obtained by the experiment were analyzed. The experimental carrier gas was high purity nitrogen (99.999%), the flow rate was 100 ml/min, the heating rate was 10 ° C / min, and the temperature was raised from room temperature to 1000 ° C.