CN112014545A - Method for detecting oily sludge - Google Patents
Method for detecting oily sludge Download PDFInfo
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- CN112014545A CN112014545A CN202010621092.0A CN202010621092A CN112014545A CN 112014545 A CN112014545 A CN 112014545A CN 202010621092 A CN202010621092 A CN 202010621092A CN 112014545 A CN112014545 A CN 112014545A
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- oily sludge
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- 239000010802 sludge Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001514 detection method Methods 0.000 claims abstract description 31
- 239000007787 solid Substances 0.000 claims abstract description 13
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 7
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 8
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 4
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002910 solid waste Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for detecting oily sludge, which comprises the following steps: stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample; standing the paste sample for 15-30min, solidifying to obtain a solid sample, taking out the solid sample, grinding in a porcelain mortar to obtain a powdery sample, placing the powdery sample in a Soxhlet extractor, extracting with carbon tetrachloride as an extractant for 3-5 h, and detecting. By the mode, the method for detecting the oily sludge disclosed by the invention uniformly stirs and mixes the oily sludge to be detected, so that the components of the oily sludge are uniformly distributed, the detection result is accurate, and the phenomenon that the detection result is not high or low due to different selected positions of oily sludge samples is avoided.
Description
Technical Field
The invention relates to the technical field of solid waste oily sludge treatment, in particular to a detection method of oily sludge.
Background
The solid waste oil-containing sludge is a concomitant product of petrochemical production, is a main pollution source of petroleum production and has complex components. In order to meet the discharge requirement, the oily sludge needs to be detected.
However, in the conventional method, the oily sludge is sampled randomly, and the detection results of the oily sludge meeting the requirement of the same batch to be processed are high and low due to different selected positions of the oily sludge samples, which brings difficulty to the detection of the oily sludge of the same batch of solid wastes.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for detecting oily sludge, which uniformly mixes the oily sludge to be detected to uniformly distribute the components of the oily sludge, so that the detection result is accurate, and the phenomenon that the detection result is not high or low due to different selected positions of oily sludge samples can be avoided.
In order to solve the technical problems, the invention adopts a technical scheme that: provided is a method for detecting oil-containing sludge, which is characterized by comprising: stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample; standing the paste sample for 15-30min, solidifying to obtain a solid sample, taking out the solid sample, grinding in a porcelain mortar to obtain a powdery sample, placing the powdery sample in a Soxhlet extractor, extracting with carbon tetrachloride as an extractant for 3-5 h, and detecting.
Further, the step of obtaining the detection sample comprises the steps of dividing the oily sludge sampling sample in the stirrer into four parts by a quartering method, and taking out two parts from the four parts according to a diagonal method to obtain the detection sample.
Further, the step of preparing the test sample into a uniform paste sample comprises: weighing 15-25g of detection sample, adding 20-30g of magnesium sulfate into the detection sample, and stirring to obtain a uniform paste sample.
Further, the step of obtaining the same batch of oily sludge to be detected comprises the following steps: and (3) placing the same batch of oily sludge to be detected into a vacuum collection bottle at a collection site.
The invention has the beneficial effects that: different from the prior art, the detection method of the oily sludge disclosed by the invention comprises the following steps: stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample; standing the paste sample for 15-30min, solidifying to obtain a solid sample, taking out the solid sample, grinding in a porcelain mortar to obtain a powdery sample, placing the powdery sample in a Soxhlet extractor, extracting with carbon tetrachloride as an extractant for 3-5 h, and detecting. By the mode, the method for detecting the oily sludge disclosed by the invention uniformly stirs and mixes the oily sludge to be detected, so that the components of the oily sludge are uniformly distributed, the detection result is accurate, and the phenomenon that the detection result is not high or low due to different selected positions of oily sludge samples is avoided.
Drawings
FIG. 1 is a schematic flow chart of the method for detecting oily sludge according to the present invention.
Detailed Description
As shown in fig. 1, the method for detecting the oily sludge comprises the following steps:
step S101: and obtaining the same batch of oily sludge to be detected.
In this embodiment, the step of obtaining the same batch of oily sludge to be detected includes: and (3) placing the same batch of oily sludge to be detected into a vacuum collection bottle at a collection site. It should be understood that the vacuum collection bottle is used for collecting the oily sludge to be detected in the same batch, so that the components of the oily sludge are not easy to lose.
Step S102: and stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample.
It should be understood that in the present embodiment, the oily sludge is uniformly stirred, so that the components of the oily sludge are uniformly distributed, and therefore, for the same batch of oily sludge to be detected, no matter where the oily sludge sample is selected, the detection results are not very different.
Preferably, the same batch of oily sludge to be detected is stirred and mixed uniformly by a stirrer in a dust-free space environment. Or the stirrer is controlled in an automatic mode to stir and mix the same batch of oily sludge to be detected in a vacuum environment.
In this embodiment, the step of obtaining the test sample in step S102 includes dividing the oily sludge sample in the stirrer into four parts by a quartering method, and taking out two parts from the four parts by a diagonal method to obtain the test sample. It should be understood that the oily sludge is divided into four parts by the quartering method, which belongs to random operation and has better operation effect.
Further, in other embodiments, the step of obtaining the detection sample in step S102 includes taking out the oil-containing sludge uniformly stirred from the stirrer; the evenly stirred oily sludge is in a vacuum environment and flattened; sludge is collected in the flat oily sludge at intervals and stirred and mixed to obtain a detection sample.
Step S103: the test sample was prepared as a homogeneous paste sample.
In this embodiment, the step of rendering the test sample into a uniform paste sample in step S103 includes:
step S1031: the test sample is weighed at 15-25g (g). It will be appreciated that the test sample needs to be ground in a porcelain mortar and therefore only 15-25g need be weighed.
Step S1032: to the test sample, 20-30g of magnesium sulfate was added and stirred to form a uniform paste sample.
It is understood that the addition of 20-30g magnesium sulfate is only sufficient for 15-25g of test sample.
Step S104: the paste sample was left to stand for 15-30min (minutes) until it solidified into a solid sample.
It will be appreciated that in some embodiments, during the 15-30min curing of the paste sample, the paste sample may be placed in a vibrator (e.g. an ultrasonic vibrator or a mechanical vibrator) such that during the curing of the paste sample, the paste sample is also in a state of vibration such that molecules within the sample remain in motion and the components of the sample are uniformly distributed.
Step S105: the solid sample was removed and ground in a porcelain mortar to form a powder sample.
Step S106: the powdery sample was placed in a soxhlet extractor.
It will be appreciated that the powder sample is placed in the siphon of a soxhlet extractor, wherein the paper package height of the siphon should be 1-1.5cm (cm) below the highest point of the siphon of the soxhlet extractor.
Step S107: extracting with carbon tetrachloride as extractant for 3-5 hr with Soxhlet extractor, and detecting. It should be understood that the detection result of step S107 is accurate.
In summary, the method for detecting oily sludge disclosed by the invention comprises the following steps: stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample; standing the paste sample for 15-30min, solidifying to obtain a solid sample, taking out the solid sample, grinding in a porcelain mortar to obtain a powdery sample, placing the powdery sample in a Soxhlet extractor, extracting with carbon tetrachloride as an extractant for 3-5 h, and detecting. By the mode, the method for detecting the oily sludge disclosed by the invention uniformly stirs and mixes the oily sludge to be detected, so that the components of the oily sludge are uniformly distributed, the detection result is accurate, and the phenomenon that the detection result is not high or low due to different selected positions of oily sludge samples is avoided.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (4)
1. A method for detecting oily sludge is characterized by comprising the following steps:
acquiring the same batch of oily sludge to be detected;
stirring and uniformly mixing the same batch of oily sludge to be detected by using a stirrer, and obtaining a detection sample;
making the detection sample into a uniform paste sample;
standing the paste sample for 15-30min, and curing the paste sample into a solid sample;
taking out the solid sample, and grinding the solid sample in a porcelain mortar to form a powdery sample;
placing the powdery sample in a Soxhlet extractor;
extracting with carbon tetrachloride as extractant for 3-5 hr with Soxhlet extractor, and detecting.
2. The method for detecting oily sludge according to claim 1, wherein the step of obtaining a detection sample comprises:
and dividing the oily sludge sampling sample in the stirrer into four parts by utilizing a quartering method, and taking out two parts from the four parts according to a diagonal method to obtain a detection sample.
3. The method for detecting oily sludge according to claim 2, wherein the step of preparing a sample for detection into a uniform paste sample comprises:
weighing 15-25g of detection sample;
to the test sample, 20-30g of magnesium sulfate was added and stirred to form a uniform paste sample.
4. The method for detecting oily sludge according to claim 1, wherein the step of obtaining the same batch of oily sludge to be detected comprises:
and (3) placing the same batch of oily sludge to be detected into a vacuum collection bottle at a collection site.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010621092.0A CN112014545A (en) | 2020-07-01 | 2020-07-01 | Method for detecting oily sludge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010621092.0A CN112014545A (en) | 2020-07-01 | 2020-07-01 | Method for detecting oily sludge |
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| Publication Number | Publication Date |
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| CN112014545A true CN112014545A (en) | 2020-12-01 |
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| CN202010621092.0A Pending CN112014545A (en) | 2020-07-01 | 2020-07-01 | Method for detecting oily sludge |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102608053A (en) * | 2012-02-23 | 2012-07-25 | 北京水泥厂有限责任公司 | Detection method for mineral oil in sludge |
| CN107044964A (en) * | 2017-04-27 | 2017-08-15 | 中国石油化工股份有限公司 | A kind of Sludge in Oilfields content of humic acid assay method |
| CN107064057A (en) * | 2017-04-18 | 2017-08-18 | 中国石油化工股份有限公司 | A kind of method for rapidly testing of low-water-content oil field sludge oil content |
| CN109142264A (en) * | 2017-06-16 | 2019-01-04 | 中国石油天然气股份有限公司 | The method that oil field sludge oil content determines |
-
2020
- 2020-07-01 CN CN202010621092.0A patent/CN112014545A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102608053A (en) * | 2012-02-23 | 2012-07-25 | 北京水泥厂有限责任公司 | Detection method for mineral oil in sludge |
| CN107064057A (en) * | 2017-04-18 | 2017-08-18 | 中国石油化工股份有限公司 | A kind of method for rapidly testing of low-water-content oil field sludge oil content |
| CN107044964A (en) * | 2017-04-27 | 2017-08-15 | 中国石油化工股份有限公司 | A kind of Sludge in Oilfields content of humic acid assay method |
| CN109142264A (en) * | 2017-06-16 | 2019-01-04 | 中国石油天然气股份有限公司 | The method that oil field sludge oil content determines |
Non-Patent Citations (3)
| Title |
|---|
| 中华人民共和国建设部: "《中华人民共和国城镇建设行业标准 CJ/T221-2005》", 30 December 2005 * |
| 叶建雄: "《建筑材料基础实验》", 30 November 2016 * |
| 许晗 等: "索氏提取法测定含油污泥含油量的实验研究", 《现代盐化工》 * |
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Application publication date: 20201201 |