(1) Method for determining moisture content of oil sludge
At present, the laboratory determines that the water content of the oil sludge is mostly by the drying method. At 105 ° C, the water escapes in the form of water vapor, and the moisture content of the sample is obtained by the mass change of the sample before and after drying. However, this method is not suitable for the determination of the moisture content of oil sludge, because some of the low-boiling oil will also escape together during the drying process, resulting in uncertain measurement errors; therefore, the water content of crude oil can be compared with GB8929-2006. Method Distillation is used to determine the moisture content of oil sludge.
The specific measurement method is as follows; weigh the appropriate amount of oil sludge sample into the flask, add enough xylene (in accordance with GB3407 superior grade) solvent to the flask, in order to prevent bumping, add 3-5 glass beads, according to the experimental device Connect the device to the condensate tube and heat it back. The initial stage is followed by slow heating. After the boiling speed is stabilized, the heating rate is adjusted so that the distillate is dropped into the receiver at a rate of 2-5 drops per second, and the distillation is continued until no part of the instrument is visible except the receiver. Water is visible, and the volume of water in the receiver does not change within 5 minutes. The distillation is stopped. After cooling to room temperature, the volume of water in the receiver is recorded as V2; only the above-mentioned same volume of xylene reagent is repeated. The volume of water in the receiver is recorded as V1. Three parallel samples were made for each set of experiments to avoid operational errors affecting the accuracy of the experiment.
(2) Method for determining oil content and slag content of oil sludge
Determination of oil content and slag content of oil sludge is designed according to the method for determining mineral oil in the sludge test method of CJ/T221-2005 municipal sewage treatment plant. The method adopts a Soxhlet extractor to extract the oil phase in the oil sludge, and then the remaining residue is dried and weighed to obtain the slag-containing rate of the oil sludge, and then the oil content of the oil sludge is obtained by the reduction method. rate.
The specific measurement method is as follows: Weigh an appropriate amount of oil sludge sample, put it into the filter paper bag of mass MO in advance and soak it with carbon tetrachloride, wrap it in the extraction cylinder of Soxhlet extractor, and put it into the flask. Add enough carbon tetrachloride solvent, connect the device according to the experimental device diagram, start heating after the water is condensed, and heat it in a water bath. After the first reflux, the reflux time is controlled at 20-25 minutes. After the carbon tetrachloride in the extraction cylinder is clarified and colorless, and the total extraction time is not less than 6 hours, the extraction is completed. After cooling to room temperature, the device is disassembled, and the filter paper package of the sample wrapped in the extraction cylinder is taken out and placed. The oven was cooled to a constant weight in an oven at a temperature of 120 ° C, and placed in a desiccator to cool to room temperature, and the mass of the filter paper package was found to be m 2 . Three parallel samples were made for each set of experiments to avoid operational errors affecting the accuracy of the experiment.