CN107290242A - The detection method of oil content in a kind of waste oil containing metallurgical slag - Google Patents

The detection method of oil content in a kind of waste oil containing metallurgical slag Download PDF

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Publication number
CN107290242A
CN107290242A CN201610202897.5A CN201610202897A CN107290242A CN 107290242 A CN107290242 A CN 107290242A CN 201610202897 A CN201610202897 A CN 201610202897A CN 107290242 A CN107290242 A CN 107290242A
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beaker
oil
sample
waste oil
oil content
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CN107290242B (en
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周桂海
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Shanghai Meishan Iron and Steel Co Ltd
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Shanghai Meishan Iron and Steel Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing 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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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The present invention relates to a kind of detection method of oil content in waste oil containing metallurgical slag, the technical problem that oil content can not be detected accurately in the waste oil containing metallurgical slag is mainly solved.The technical scheme is that:The detection method of oil content, comprises the following steps in a kind of waste oil containing metallurgical slag:Waste oil sample is weighed to be placed in separatory funnel, add after water, sodium chloride and dilution heat of sulfuric acid stirring, stood after adding petroleum ether concussion extraction, upper solution is transferred in beaker A, stood after petroleum ether concussion extraction is added in lower floor's solution, then upper solution is transferred in former beaker A;Then add after anhydrous sodium sulfate stirring, be filled into constant weight beaker B into beaker solution A, beaker B is placed in heating evaporation in hot bath, then beaker B is transferred to dried in baking oven after cool down, weigh;Calculate oil content in sample.The inventive method is easy to operate, and detection data are accurately and reliably.

Description

The detection method of oil content in a kind of waste oil containing metallurgical slag
Technical field
The present invention relates to a kind of detection method of oil content in waste oil, oil in more particularly to a kind of waste oil containing metallurgical slag The detection method of content, belongs to iron and steel metallurgical industry chemical analysis technology field.
Background technology
Iron and steel enterprise can produce substantial amounts of waste oil in process of production, such as waste hydraulic oil, waste lubricating oil, waste emulsified oil, useless Antirust oil etc..If the directly discharge of these waste oil not only causes greatly pollution to environment, certain economy is also caused to iron and steel enterprise Loss.Generally, these waste oil carry out recycling recycling by professional oil product processing mechanism, on the one hand can solve ring Border pollution problem, while certain economic benefit can also be produced.These waste oil are before recycling, it is necessary to oil-containing in waste oil Amount is accurately detected that this not only contributes to rationally assess these waste oil unit take-back costs, while also rationally high for waste oil Effect processing provides data supporting.Produced due to these waste oil under the big production environment of steel, contain a large amount of metallurgical slag specimen such as steel The smelting iron and steel slag specimen such as slag, scum, while also containing various solid impurities such as metal particulate, metal oxides, composition is complicated Extreme difficulties are caused to detection.
Chinese patent application CN200510079803.1, entitled one kind makes fluorescence method measure oil in water with other methods to contain The method that amount has comparativity, discloses a kind of detection method of oil content in fluorescence spectrometry water, mainly passes through fluorescence pattern Assay method scanning spectra, directly determines the oil content collection of illustrative plates of solvent free extract water sample with fluorescence method under the same conditions, then right The quasi- oil concentration curve of sighting target, calculates oil content in water outlet;This method cannot be used for the detection of oil content in waste oil containing metallurgical slag, It is primarily present following method problem:(1) substantial amounts of Solid micro material is contained in Ferrous Metallurgy slag inclusion waste oil, it is impossible to To accurate fluorescence spectrum;(2) this method needs to prepare, and there is certain gradient oil concentration curve to be to need same type standard substance Oil, and Ferrous Metallurgy slag inclusion waste oil is difficult to collect same type standard substance oil.The technology is only suitable for on-line checking water petrochina class The detection of content, is not suitable for oil content detection in slag inclusion waste oil in metallurgical production.Chinese patent application CN201210444737.3, Entitled waste oil liquid characteristic detection method, discloses a kind of application Infrared Spectrum Technology-multielement analysis quantitative spectrometric and determines Property research, detection of the comprehensive multi-disciplinary knowledge to waste oils properties judge oil product product by the characteristic of relatively new and old oil product Qualitative change information technology solution, the technical scheme does not apply to the detection of oil content in slag inclusion waste oil.
Prior art can not accurately be detected to oil content in the waste oil containing metallurgical slag.
The content of the invention
It is an object of the invention to provide a kind of detection method of oil content in waste oil containing metallurgical slag, mainly solve to contain The technical problem that oil content can not be detected accurately in the waste oil of metallurgical slag.
The technical solution adopted by the present invention is:The detection method of oil content in a kind of waste oil containing metallurgical slag, including with Lower step:
1) accurately weigh the waste oil sample that 10.00~15.00g contains metallurgical slag to be placed in 250ml separatory funnels, add water 20~30ml, sodium chloride 15-20g and volumetric concentration are 1:6 5~10ml of dilution heat of sulfuric acid, agitated rear addition petroleum ether 30~ 50ml carries out concussion extraction, and upper solution is transferred in beaker A after standing 20~30min, oil is added in lower floor's solution 30~50ml of ether carries out concussion extraction again, stands and upper solution transfer is incorporated into former beaker A again after 20~30min;
2) 10~15g of anhydrous sodium sulfate is added in the solution in beaker A, constant weight beaker B is filled into after being sufficiently stirred for In, beaker B first is placed in into 40~50min of heating evaporation in 80~90 DEG C of hot baths, to remove most of petroleum ether, then will burn Cup B is transferred in 70~80 DEG C of baking ovens 10~20min of drying, then beaker B is placed in drier be cooled to it is right after 15~25 DEG C Beaker B weighs;
3) sample oil content is calculated, sample oil content presses formula C=(m2-m1)/m × 100% is calculated, and in formula, C is sample Middle oily weight/mass percentage composition, unit is %;m1For the quality of constant weight beaker B, unit is g;m2For the oil after oven for drying With beaker B quality sum, unit is g;M is the quality of sample, and unit is g.
The inventive method by first being pre-processed to the waste oil containing metallurgical slag after again using petroleum ether extraction separate Method, realizes the accurate measurement of oil content in the waste oil containing metallurgical slag.
The inventive method is the recycling of the waste oil containing metallurgical slag, and price evaluation provides accurate number in waste oil transaction According to support.
The present invention has following good effect compared with prior art:1st, the inventive method has filled up the waste oil containing metallurgical slag The detection technique blank of middle oil content.2nd, the data precision is high, easy to operate, labor intensity is low for the inventive method detection.
Embodiment
The detection method of oil content, comprises the following steps in a kind of waste oil containing metallurgical slag:
1) it is accurate to weigh the waste oil sample that 15.00g contains metallurgical slag and be placed in 250ml separatory funnels, add water 25ml, chlorine It is 1 to change sodium 15g and volumetric concentration:6 dilution heat of sulfuric acid 5ml, the agitated rear petroleum ether 40ml that adds carries out fully shaking extraction, quiet Put after 30min and upper solution be transferred in beaker A, petroleum ether 40ml is added in lower floor's solution and carries out concussion extraction again, Stand and upper solution transfer is incorporated into former beaker A again after 30min;
2) anhydrous sodium sulfate 10g is added in the solution in beaker A, is filled into after being sufficiently stirred in constant weight beaker B, first Beaker B is placed in heating evaporation 50min in 85 DEG C of hot baths, then beaker B is transferred in 75 DEG C of baking ovens and dries 15min, then Beaker B is placed in drier to be cooled to after 20 DEG C beaker B is weighed;
3) sample oil content is calculated, sample oil content presses formula C=(m2-m1)/m × 100% is calculated, and in formula, C is sample Middle oily weight/mass percentage composition, unit is %;m1For the quality of constant weight beaker B, unit is g;m2For the oil after oven for drying With beaker B quality sum, unit is g;M is the quality of sample, and unit is g.
Water-bath used in hot bath is the digital display perseverance that Guo Hua Electrical Appliances Co., Ltd produces model HH-6 in the embodiment of the present invention Warm water bath.
Baking oven used is Shanghai ESPEC Environment Equipment Co., Ltd. production model LC-213 in the embodiment of the present invention.
The inventive method degree of accuracy and precision are confirmed by the recovery testu and Precision Experiment of sample.
Recovery experiment, it is accurate in waste oil sample to be determined to add product oil, detected by the inventive method, calculate mark-on and return Yield, result of the test see the table below 1.
The sample recovery testu of table 1
Precision Experiment, oil content in the waste oil of metallurgical slag is contained to 3 groups and carries out 11 Precision Experiments, analysis result is shown in Table 2 below.
The sample Precision Experiment of table 2
It is above-mentioned test result indicates that, using the inventive method determine the waste oil containing metallurgical slag in the oil content rate of recovery exist Between 99.0~101.7%, the rate of recovery is higher, and detection data statistics RSD is much smaller than 1%, and detection data precision is good, and method is accurate It is really reliable, fully meet oil content in the waste oil containing metallurgical slag and assess requirement, also reclaim again sharp for the waste oil containing metallurgical slag With offer data supporting.

Claims (1)

1. the detection method of oil content in a kind of waste oil containing metallurgical slag, it is characterized in that, it the described method comprises the following steps:
1) the waste oil sample that 10.00~15.00g contains metallurgical slag is accurately weighed to be placed in 250ml separatory funnels, add water 20~ 30ml, sodium chloride 15-20g and volumetric concentration are 1:6 5~10ml of dilution heat of sulfuric acid, 30~50ml of agitated rear addition petroleum ether Concussion extraction is carried out, upper solution is transferred in beaker A after standing 20~30min, petroleum ether 30 is added in lower floor's solution ~50ml carries out concussion extraction again, stands and upper solution transfer is incorporated into former beaker A again after 20~30min;
2) 10~15g of anhydrous sodium sulfate is added in the solution in beaker A, is filled into after being sufficiently stirred in constant weight beaker B, first Beaker B is placed in 40~50min of heating evaporation in 80~90 DEG C of hot baths, then beaker B is transferred in 70~80 DEG C of baking ovens 10~20min is dried, then beaker B is placed in drier to be cooled to after 15~25 DEG C beaker B is weighed;
3) sample oil content is calculated, sample oil content presses formula C=(m2-m1)/m × 100% is calculated, in formula, and C is oil in sample Weight/mass percentage composition, unit is %;m1For the quality of constant weight beaker B, unit is g;m2For the oil and burning after oven for drying Cup B quality sum, unit is g;M is the quality of sample, and unit is g.
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Cited By (6)

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Publication number Priority date Publication date Assignee Title
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
CN113970500A (en) * 2021-10-27 2022-01-25 北京新风航天装备有限公司 Method for rapidly measuring oil content of oil stain solid waste

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN113970500A (en) * 2021-10-27 2022-01-25 北京新风航天装备有限公司 Method for rapidly measuring oil content of oil stain solid waste
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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