CN107290242B - Method for detecting oil content in waste oil containing metallurgical slag - Google Patents
Method for detecting oil content in waste oil containing metallurgical slag Download PDFInfo
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- CN107290242B CN107290242B CN201610202897.5A CN201610202897A CN107290242B CN 107290242 B CN107290242 B CN 107290242B CN 201610202897 A CN201610202897 A CN 201610202897A CN 107290242 B CN107290242 B CN 107290242B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention relates to a method for detecting the oil content in waste oil containing metallurgical slag, which mainly solves the technical problem that the oil content in the waste oil containing the metallurgical slag can not be accurately detected. The technical scheme of the invention is as follows: a method for detecting the oil content in waste oil containing metallurgical slag comprises the following steps: weighing a waste oil sample, placing the waste oil sample in a separating funnel, adding water, sodium chloride and a dilute sulfuric acid solution, stirring, adding petroleum ether, performing oscillation extraction, standing, transferring an upper-layer solution into a beaker A, adding petroleum ether into a lower-layer solution, performing oscillation extraction, standing, and transferring the upper-layer solution into an original beaker A; adding anhydrous sodium sulfate into the beaker A solution, stirring, filtering to a beaker B with constant weight, putting the beaker B into a hot water bath, heating and evaporating, transferring the beaker B into an oven, drying, cooling and weighing; and calculating the oil content in the sample. The method is simple and convenient to operate, and the detection data is accurate and reliable.
Description
Technical Field
The invention relates to a method for detecting the oil content in waste oil, in particular to a method for detecting the oil content in waste oil containing metallurgical slag, and belongs to the technical field of chemical analysis in the ferrous metallurgy industry.
Background
Steel enterprises can produce a large amount of waste oil in the production process, such as waste hydraulic oil, waste lubricating oil, waste emulsified oil, waste antirust oil and the like. If the waste oil is directly discharged, the waste oil not only causes great pollution to the environment, but also causes certain economic loss to iron and steel enterprises. Generally, the waste oil is recycled by a professional oil treatment mechanism, so that the problem of environmental pollution can be solved, and certain economic benefit can be generated. Before the waste oil is recycled, the oil content in the waste oil must be accurately detected, so that the recycling price of the waste oil is reasonably evaluated, and data support is provided for reasonable and efficient processing of the waste oil. The waste oil is produced in a large-scale steel production environment, contains a large amount of metallurgical slag samples such as steel slag, iron slag and other steel smelting slag samples, and also contains various solid impurities such as metal particles, metal oxides and the like, so that the complex composition causes great difficulty in detection.
Chinese patent application CN200510079803.1, entitled a method for measuring oil content in water by using fluorescence method and other methods, discloses a detection method for measuring oil content in water by using fluorescence method, mainly scanning spectrum by using fluorescence spectrum measuring method, directly measuring oil content spectrum of solvent-free extraction water sample by using fluorescence method under the same condition, and calculating oil content in water by contrasting with standard oil concentration curve; the method can not be used for detecting the oil content in waste oil containing metallurgical slag, and mainly has the following problems: (1) the waste slag-containing oil in ferrous metallurgy contains a large amount of solid microparticle substances, and an accurate fluorescence spectrum cannot be obtained; (2) the method needs to prepare the standard substance oil with the same type by a certain gradient oil-containing concentration curve, and the standard substance oil with the same type is difficult to collect by the ferrous metallurgy slag-containing waste oil. The technology is only suitable for detecting the content of petroleum in water on line and is not suitable for detecting the oil content in the waste oil containing slag in metallurgical production. The Chinese patent application CN201210444737.3, entitled waste oil characteristic detection method, discloses a technical scheme for applying infrared spectroscopic analysis technology-multielement analysis spectrum quantitative and qualitative research, detecting waste oil characteristics by integrating multidisciplinary knowledge, and judging oil quality change information by comparing characteristics of new and old oil products, and the technical scheme is not suitable for detecting oil content in waste oil containing residues.
The prior art can not accurately detect the oil content in the waste oil containing the metallurgical slag.
Disclosure of Invention
The invention aims to provide a method for detecting the oil content in waste oil containing metallurgical slag, which mainly solves the technical problem that the oil content in the waste oil containing metallurgical slag cannot be accurately detected.
The technical scheme adopted by the invention is as follows: a method for detecting the oil content in waste oil containing metallurgical slag comprises the following steps:
1) accurately weighing 10.00-15.00 g of waste oil sample containing metallurgical slag, placing the waste oil sample into a 250ml separating funnel, adding 20-30 ml of water, 15-20g of sodium chloride and 5-10 ml of dilute sulfuric acid solution with the volume concentration of 1:6, stirring, adding 30-50 ml of petroleum ether, performing oscillation extraction, standing for 20-30 min, transferring the upper layer solution into a beaker A, adding 30-50 ml of petroleum ether into the lower layer solution, performing oscillation extraction again, standing for 20-30 min, and transferring and combining the upper layer solution into the original beaker A again;
2) adding 10-15 g of anhydrous sodium sulfate into the solution in the beaker A, fully stirring, filtering to a beaker B with constant weight, placing the beaker B in a hot water bath at 80-90 ℃, heating and evaporating for 40-50 min to remove most of petroleum ether, transferring the beaker B to an oven at 70-80 ℃, drying for 10-20 min, placing the beaker B in a dryer, cooling to 15-25 ℃, and weighing the beaker B;
3) calculating the oil content of the sample according to the formula C ═ m2-m1) Calculated by the weight percent of/m × 100%, wherein C is the weight percent of oil in the sampleContent, in%; m is1The mass of the beaker B with constant weight is g; m is2The mass sum of the oil dried by the oven and the beaker B is g; m is the mass of the sample in g.
The method of the invention realizes the accurate measurement of the oil content in the waste oil containing the metallurgical slag by adopting the method of pretreating the waste oil containing the metallurgical slag and then extracting and separating petroleum ether.
The method provides accurate data support for the recovery and treatment of waste oil containing metallurgical slag and the price evaluation in the waste oil transaction.
Compared with the prior art, the invention has the following positive effects: 1. the method fills the technical blank of detecting the oil content in the waste oil containing the metallurgical slag. 2. The method has the advantages of high data detection accuracy, simple and convenient operation and low labor intensity.
Detailed Description
A method for detecting the oil content in waste oil containing metallurgical slag comprises the following steps:
1) accurately weighing 15.00g of waste oil sample containing metallurgical slag, placing the waste oil sample into a 250ml separating funnel, adding 25ml of water, 15g of sodium chloride and 5ml of dilute sulfuric acid solution with the volume concentration of 1:6, stirring, adding 40ml of petroleum ether, fully shaking and extracting, standing for 30min, transferring the upper-layer solution into a beaker A, adding 40ml of petroleum ether into the lower-layer solution, shaking and extracting again, standing for 30min, transferring and combining the upper-layer solution into the original beaker A again;
2) adding 10g of anhydrous sodium sulfate into the solution in the beaker A, fully stirring, filtering to a beaker B with constant weight, putting the beaker B in a hot water bath at 85 ℃, heating and evaporating for 50min, transferring the beaker B into a 75 ℃ oven, drying for 15min, putting the beaker B in a drier, cooling to 20 ℃, and weighing the beaker B;
3) calculating the oil content of the sample according to the formula C ═ m2-m1) M × 100 is calculated by 100 percent, wherein C is the mass percent of oil in the sample and is expressed in percent1The mass of the beaker B with constant weight is g; m is2Is the sum of the mass of the oil dried by the oven and the beaker BIn units of g; m is the mass of the sample in g.
The water bath used in the hot water bath in the embodiment of the invention is a digital display constant temperature water bath with model number HH-6 produced by China electric appliance Limited.
The oven used in the examples of the present invention was model number LC-213 from shanghai esteek environmental equipment ltd.
The accuracy and precision of the method are confirmed by a standard addition recovery experiment and a precision experiment of the sample.
And (3) a recovery experiment, namely accurately adding the product oil into the waste oil sample to be measured, detecting according to the method disclosed by the invention, calculating the standard addition recovery rate, and obtaining the test result shown in the following table 1.
TABLE 1 sample recovery test with addition of standard
Precision experiment, the oil content in 3 groups of waste oil containing metallurgical slag was subjected to 11 precision experiments, and the analysis results are shown in table 2 below.
TABLE 2 sample precision test
The experimental results show that the recovery rate of the oil content in the waste oil containing the metallurgical slag is measured to be 99.0-101.7% by adopting the method, the recovery rate is high, the detection data statistics RSD is far less than 1%, the detection data precision is good, the method is accurate and reliable, the evaluation requirement of the oil content in the waste oil containing the metallurgical slag is completely met, and data support is provided for recycling the waste oil containing the metallurgical slag.
Claims (1)
1. A method for detecting the oil content in waste oil containing metallurgical slag is characterized by comprising the following steps:
1) accurately weighing 10.00-15.00 g of waste oil sample containing metallurgical slag, placing the waste oil sample into a 250ml separating funnel, adding 20-30 ml of water, 15-20g of sodium chloride and 5-10 ml of dilute sulfuric acid solution with the volume concentration of 1:6, stirring, adding 30-50 ml of petroleum ether, performing oscillation extraction, standing for 20-30 min, transferring the upper layer solution into a beaker A, adding 30-50 ml of petroleum ether into the lower layer solution, performing oscillation extraction again, standing for 20-30 min, and transferring and combining the upper layer solution into the original beaker A again;
2) adding 10-15 g of anhydrous sodium sulfate into the solution in the beaker A, fully stirring, filtering to obtain a beaker B with constant weight, putting the beaker B in a hot water bath at 80-90 ℃, heating and evaporating for 40-50 min, transferring the beaker B into an oven at 70-80 ℃, drying for 10-20 min, putting the beaker B in a dryer, cooling to 15-25 ℃, and weighing the beaker B;
3) calculating the oil content of the sample according to the formula C ═ m2-m1) M × 100 is calculated by 100 percent, wherein C is the mass percent of oil in the sample and is expressed in percent1The mass of the beaker B with constant weight is g; m is2The mass sum of the oil dried by the oven and the beaker B is g; m is the mass of the sample in g.
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| CN107884303A (en) * | 2017-11-24 | 2018-04-06 | 东隆环保科技有限公司 | A kind of greasy filth oil content measuring method |
| CN108918486A (en) * | 2018-06-13 | 2018-11-30 | 中国石油天然气股份有限公司 | The measurement method and device of a kind of oily sludge Central Plains oil content |
| CN109932269A (en) * | 2019-03-16 | 2019-06-25 | 天能电池集团股份有限公司 | A kind of test method of lead powder oil content |
| CN111458257A (en) * | 2020-04-03 | 2020-07-28 | 青岛天祥食品集团有限公司 | Method for detecting content of filter aid and phospholipid in pressed peanut oil filter residue |
| CN113092612A (en) * | 2021-03-31 | 2021-07-09 | 武汉钢铁有限公司 | Method for detecting oil content in cold rolling oil sludge |
| CN113970500B (en) * | 2021-10-27 | 2023-08-29 | 北京新风航天装备有限公司 | Rapid determination method for oil content of greasy dirt solid waste |
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| CN1945277B (en) * | 2006-10-19 | 2010-04-07 | 武汉理工大学 | Method for detecting insoluble matter dispersiveness in solution |
| CN101251460A (en) * | 2008-03-25 | 2008-08-27 | 天津商业大学 | Method for measuring moisture and oil content in recovered refrigerant |
| CN102778409B (en) * | 2012-06-05 | 2013-12-25 | 中国石油大学(北京) | Device and method used for measuring content of oil and/or liquid water in sample |
| CN104089844A (en) * | 2014-07-16 | 2014-10-08 | 安徽鑫科新材料股份有限公司 | Method for measuring content of oil in scrap copper |
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| 第六节 石油产品的回收与再生;水利电力部物资局;《非金属材料》;水利电力部物资局;19830731;第126-128页 * |
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