CN104374630A - Method for detecting and pretreating polycyclic aromatic hydrocarbon in oily sludge - Google Patents
Method for detecting and pretreating polycyclic aromatic hydrocarbon in oily sludge Download PDFInfo
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Abstract
The invention provides a method for detecting and pretreating polycyclic aromatic hydrocarbon in oily sludge. The method comprises the steps of taking the oily sludge, feeding kieselguhr into the oily sludge, grinding, sieving, adding a substitute, evenly mixing and then extracting with extract liquor; collecting the extract liquor, and concentrating to obtain extract concentrated solution; filling a chromatographic column; after the chromatographic column is balanced, feeding the extract concentrated solution sample onto the chromatographic column, eluting the chromatographic column with n-hexane after the chromatographic column comes into full contact with the extract concentrated solution; eluting the chromatographic column with a mixed eluant of dichloromethane and n-hexane; collecting the eluant until the mixed eluant of dichloromethane and n-hexane completely flows outside, thus obtaining the mixed liquid of the polycyclic aromatic hydrocarbon; concentrating the mixed liquid of the polycyclic aromatic hydrocarbon, and carrying out nitrogen purging concentration to obtain the polycyclic aromatic hydrocarbon sample. With adoption of the rapid extraction method, the use amount of an organic solvent is small, the pretreatment time is short and operation is simple.
Description
Technical field
The present invention relates to the detection preprocess method of palycyclic aromatic in a kind of oily sludge, belong to contained Mud Treatment Technology field.
Background technology
Oily sludge is the main solid waste of oil field and Petrochemical Enterprises discharge, it is mainly made up of materials such as crude oil, moisture, clay mineral, biological organic matter and chemical addition agents, general oil content is about 10%, and high reached at 20%-30% is the difficult problem of environmental protection of petroleum and petrochemical industry always.Oily sludge is put into " National Hazard refuse register ", and domestic and international government organs, non-government organization, scientific research institution and production enterprises and institutions all pay much attention to environmental management and the Environmental capacity of oily sludge.
Palycyclic aromatic (PAHs) is modal organic contaminant, and have strongly carcinogenic, teratogenesis, mutagenesis, having low-solubility and stronger hydrophobic nature, is also the main poisonous and harmful substance in oily sludge petroleum hydrocarbon component.
Therefore, need to carry out detection control to the palycyclic aromatic in oily sludge, go before testing to carry out pre-service to the palycyclic aromatic in oily sludge, to facilitate detection, make accuracy of detection and sensitivity higher; But, also there is no the special preprocess method for the palycyclic aromatic in oily sludge at present.In prior art, preprocess method mainly soxhlet extraction, the chromatography purification of the palycyclic aromatic in soil, this preprocess method also exists the problems such as complicated operation, extraction solvent consumption are large, length consuming time, and the method carries out pre-service for the palycyclic aromatic in soil, and can not for this content of organic matter of oily sludge the high and material of complexity.
Summary of the invention
In view of the defect that above-mentioned prior art exists, the object of the invention is the detection preprocess method proposing palycyclic aromatic in a kind of oily sludge, the high and oily sludge of complexity of the content of organic matter can be applicable to.
Object of the present invention is achieved by the following technical programs:
In oily sludge, a detection preprocess method for palycyclic aromatic, comprises the steps:
Preparation of samples: get oily sludge, adds zeyssatite, and grinding, sieves, obtain oily sludge sample;
The rapid extraction of palycyclic aromatic: get oily sludge sample, add substitute, mixing obtains oily sludge potpourri;
Extracted by oily sludge potpourri extract, extraction temperature is 75 DEG C-125 DEG C, and extracting pressure is 1500-1700psi, extracts 3-6 time, each 3-5 minute quiet cycle; Collect extract, extract is concentrated to 1mL-5mL, is extracted concentrate;
The purification of palycyclic aromatic: the filling of chromatographic column: column chromatography silica gel is used methylene chloride soaked overnight after 120-130 DEG C of activation 16-18h, adopt wet method to fill out post, fill out after post completes, layer of silica gel is filled the anhydrous sodium sulfate that 1cm-2cm is thick, with normal hexane drip washing chromatographic column, displacement methylene chloride;
Collect: after chromatographic column balance, concentrate application of sample will be extracted on chromatographic column, abundant contact 5min-10min, use 20mL normal hexane drip washing chromatographic column again, then the mixing eluent drip washing chromatographic column of 20mL-70mL methylene chloride and normal hexane is used, collect eluent, until the mixing eluent of methylene chloride and normal hexane all flows out, obtain the mixed liquor of palycyclic aromatic;
Concentrated: the mixed liquor of concentrated palycyclic aromatic, and nitrogen purges and is concentrated into 0.7mL-0.9mL and obtains polyaromatic hydrocarbon samples, completes the detection pre-service of palycyclic aromatic in oily sludge.
According to the specific embodiment of the present invention, preferably, in above-mentioned oily sludge, the detection preprocess method of palycyclic aromatic can comprise following concrete steps:
Preparation of samples:
Get oily sludge, remove the foreign material such as stone, add zeyssatite, grinding, sieves, obtains oily sludge sample;
The rapid extraction of palycyclic aromatic:
Get oily sludge sample, add substitute, mixing obtains oily sludge potpourri;
Inserted in the stainless steel abstraction pool of accelerated solvent extraction by oily sludge potpourri, extract with extract, extraction temperature is 75 DEG C-125 DEG C, and extracting pressure is 1500psi, extracts 3-6 time, each 3-5 minute quiet cycle;
Collect extract, extract Rotary Evaporators is concentrated to 1mL-5mL, is extracted concentrate, use to be clean;
The purification of palycyclic aromatic:
The filling of chromatographic column: column chromatography silica gel is used methylene chloride soaked overnight after 130 DEG C of activation 18h, wet method is adopted to fill out post, fill out after post completes, layer of silica gel is filled the anhydrous sodium sulfate that 1cm-2cm is thick, the tapping of chromatographic column lower end, when methylene chloride liquid level close on post bed along time with normal hexane (20mL-30mL) drip washing chromatographic column, displacement methylene chloride;
Collect:
After chromatographic column balance, namely drip washing is close to terminating, normal hexane liquid level close on post bed along time, concentrate application of sample will be extracted on chromatographic column, abundant contact 5min-10min, open piston, the tapping of chromatographic column lower end, when load solution liquid level close on post bed along time, use 20mL normal hexane drip washing chromatographic column again, then when normal hexane leacheate liquid level close on post bed along time, with the mixing eluent drip washing chromatographic column of 20mL-70mL methylene chloride and normal hexane, control out flow velocity to become to drip and noncontinuum flow, collect eluent, until the mixing eluent of methylene chloride and normal hexane all flows out, obtain the mixed liquor of palycyclic aromatic,
Concentrated:
With the mixed liquor of Rotary Evaporators at 30 DEG C-40 DEG C concentrated palycyclic aromatics, and nitrogen purges and is concentrated into 0.7mL-0.9mL and obtains polyaromatic hydrocarbon samples, completes the detection pre-service of palycyclic aromatic in oily sludge.
In above-mentioned preprocess method, adding diatomaceous object is absorb the moisture in oily sludge, and makes oily sludge can be convenient to grinding; Grinding, the object of sieving is that oily sludge and zeyssatite are mixed, thus makes oily sludge uniform component distribution, representative to guarantee sieving rear sample; Wherein add zeyssatite except making oily sludge uniform component distribution, also play dry effect.This step of the purification of above-mentioned palycyclic aromatic, its objective is that a large amount of organic impurities in extraction concentrate is removed in purification.
In above-mentioned preprocess method, ASE350 accelerated solvent extraction can be adopted to carry out rapid extraction to palycyclic aromatic in oily sludge.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, this preprocess method also comprises and in polyaromatic hydrocarbon samples, to add mark in PAHs and the step of constant volume.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, described oily sludge and diatomaceous amount ratio are 100-200g: 100-200g.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, described in sieve as crossing 70-100 mesh sieve.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, substitute is for monitoring the method performance of sample; Preferably, described substitute comprises the combination of one or more in naphthalene-D8, lettuce-D12, perylene-D12 etc.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, the amount ratio of greasy dirt sample and substitute is 0.2-0.5g: 0.1-1mg.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, described extract comprises the combination of one or more in methylene chloride, acetone and acetonitrile etc.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, the ratio of the consumption of the silica gel that column chromatography is used and the consumption of oily sludge sample is 8-12g: 0.2-0.5g.
In above-mentioned oily sludge palycyclic aromatic detection preprocess method in, preferably, in the mixing eluent of described methylene chloride and normal hexane, the volume ratio of methylene chloride and normal hexane is 2:3-3:7.
Outstanding effect of the present invention is:
Adopt Rapid Extraction method, organic solvent use amount be few, pretreatment time is short, simple to operate; Use the inventive method, pre-service can be carried out in oily sludge sample by 16 kinds of Determination of Trace Polycyclic Aromatic Hydrocarbons that environmental area emphasis is monitored, the convenient detection to these palycyclic aromatics.
Embodiment
Below by specific embodiment, method of the present invention is described, be easier to make technical solution of the present invention understand, grasp, but the present invention is not limited thereto.Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1
The present embodiment provides the detection preprocess method of palycyclic aromatic in a kind of oily sludge, comprises the steps:
Preparation of samples:
Get oil content 28.35% oily sludge (clear tank greasy filth), remove the foreign material such as stone, get in 100 grams of oily sludges and add zeyssatite 100g, be placed in grinding in mortar, cross 100 mesh sieves after grinding, make its uniform component distribution, obtain oily sludge sample.
The rapid extraction of palycyclic aromatic:
Take 0.2g oily sludge sample, add substitute (naphthalene-D8) 0.1mg in oily sludge sample, mixing obtains oily sludge potpourri;
Inserted in the stainless steel abstraction pool of ASE350 accelerated solvent extraction by oily sludge potpourri, extract with methylene chloride, extraction temperature is 100 DEG C, and pressure is 1500psi, extracts 3 times, the quiet cycle of each 5 minutes;
Collect extract, extract Rotary Evaporators is concentrated to about 3mL, is extracted concentrate, use to be clean.
The purification of palycyclic aromatic:
10g chromatographic silica gel is used methylene chloride soaked overnight after 130 DEG C of activation 18h.Adopt wet method to fill out post, fill out after post completes, layer of silica gel is filled the anhydrous sodium sulfate that 2cm is thick.Chromatographic column tapping, when methylene chloride liquid level close on post bed along time, with 20mL normal hexane drip washing chromatographic column, displacement methylene chloride;
When normal hexane liquid level close on post bed along time, namely after chromatographic column balance, draw extraction concentrate application of sample on chromatographic column with clean suction pipe, and with normal hexane cleaning suction pipe application of sample in the lump, fully contact 5min.Open piston setting-out, when load solution liquid level close on post bed along time, with 20mL normal hexane drip washing chromatographic column.When leacheate liquid level close on post bed along time, concentration tube is placed at chromatographic column end opening, with the mixing eluent drip washing chromatographic column of 20mL methylene chloride and normal hexane (volume ratio 2:3), control out flow velocity to become to drip and noncontinuum flow, and collect eluent, until the mixing eluent of methylene chloride and normal hexane all flows out the mixed liquor obtaining palycyclic aromatic.
Concentrated:
Collect liquid with Rotary Evaporators is concentrated, and nitrogen purging is concentrated into about 0.9mL, takes out concentration tube, is cooled to room temperature, obtains polyaromatic hydrocarbon samples, namely complete the detection pre-service of palycyclic aromatic in oily sludge; Add the interior mark of PAHs and be settled to 1mL, being transferred in the brown sample injection bottle of 2mL, namely can be used for detecting.
The polyaromatic hydrocarbon samples good to constant volume detects, and its testing result is as shown in table 1 (1#, 2# are parallel laboratory test for clear tank greasy filth palycyclic aromatic analysis result, unit mg/kg):
Table 1
| Sequence number | Project | 1# | 2# |
| 1 | Naphthalene | 56.1 | 61.2 |
| 2 | Acenaphthylene | 141 | 159 |
| 3 | Acenaphthene | <0.1 | <0.1 |
| 4 | Fluorenes | <0.1 | <0.1 |
| 5 | Luxuriant and rich with fragrance | <0.1 | <0.1 |
| 6 | Anthracene | <0.1 | <0.1 |
| 7 | Fluoranthene | <0.1 | <0.1 |
| 8 | Pyrene | <0.1 | <0.1 |
| 9 | Benzo (a) anthracene | <0.1 | <0.1 |
| 10 | Bend | 3.09 | 2.98 |
| 11 | Benzo (b) fluoranthene | <0.1 | <0.1 |
| 12 | Benzo (k) fluoranthene | <0.1 | <0.1 |
| 13 | Benzo (a) pyrene | 2.1 | 2.8 |
| 14 | Indeno (1,2,3-cd) pyrene | <0.1 | <0.1 |
| 15 | Dibenzo (a, h) anthracene | <0.1 | <0.1 |
| 16 | Benzo (g, h, i) perylene | <0.1 | <0.1 |
Embodiment 2
The present embodiment provides the detection preprocess method of palycyclic aromatic in a kind of oily sludge, comprises the steps:
Preparation of samples:
Get oil content 18.68% oily sludge (ground sludge), remove the foreign material such as stone, get in 100 grams of oily sludges and add zeyssatite 100g, be placed in grinding in mortar, cross 100 mesh sieves after grinding, make its uniform component distribution, obtain oily sludge sample.
The rapid extraction of palycyclic aromatic:
Weigh 0.5g oily sludge sample, add (naphthalene-D8) 0.5mg in oily sludge sample, mixing obtains oily sludge potpourri;
Inserted in the stainless steel abstraction pool of ASE350 accelerated solvent extraction by oily sludge potpourri, extract with acetone, extraction temperature is 100 DEG C, and pressure is 1500psi, extracts 2 times, the quiet cycle of each 5 minutes;
Collect extract, extract Rotary Evaporators is concentrated to about 3mL, is extracted concentrate, use to be clean.
The purification of palycyclic aromatic:
10g chromatographic silica gel is used methylene chloride soaked overnight after 130 DEG C of activation 18h.Adopt wet method to fill out post, fill out after post completes, layer of silica gel post is filled the anhydrous sodium sulfate that 2cm is thick, chromatographic column tapping, when methylene chloride liquid level close on post bed along time, with 20mL normal hexane drip washing chromatographic column, displacement methylene chloride;
When normal hexane liquid level close on post bed along time, namely after chromatographic column balance, draw extraction concentrate application of sample on chromatographic column with clean suction pipe, and with normal hexane cleaning suction pipe application of sample in the lump, fully contact 7min.Open piston setting-out, when load solution liquid level close on post bed along time, with 20mL normal hexane drip washing chromatographic column.When leacheate liquid level close on post bed along time, concentration tube is placed at chromatographic column end opening, with the mixing eluent drip washing chromatographic column of 50mL methylene chloride and normal hexane (volume ratio 3:7), control out flow velocity to become to drip and noncontinuum flow, and collect eluent, until the mixing eluent of methylene chloride and normal hexane all flows out, obtain the mixed liquor of palycyclic aromatic.
Concentrated:
Collect liquid with Rotary Evaporators is concentrated, and nitrogen purging is concentrated into about 0.7mL, takes out concentration tube, is cooled to room temperature, obtains polyaromatic hydrocarbon samples, namely complete the detection pre-service of palycyclic aromatic in oily sludge; Add the interior mark of PAHs and be settled to 1mL, being transferred in the brown sample injection bottle of 2mL, namely can be used for detecting.
The polyaromatic hydrocarbon samples good to constant volume detects, and its testing result is as shown in table 2 (1#, 2# are parallel laboratory test for ground sludge palycyclic aromatic analysis result, unit mg/kg):
Table 2
| Sequence number | Project | 1# | 2# |
| 1 | Naphthalene | 81.4 | 79.8 |
| 2 | Acenaphthylene | 175 | 168 |
| 3 | Acenaphthene | <0.1 | <0.1 |
| 4 | Fluorenes | <0.1 | <0.1 |
| 5 | Luxuriant and rich with fragrance | <0.1 | <0.1 |
| 6 | Anthracene | <0.1 | <0.1 |
| 7 | Fluoranthene | <0.1 | <0.1 |
| 8 | Pyrene | <0.1 | <0.1 |
| 9 | Benzo (a) anthracene | <0.1 | <0.1 |
| 10 | Bend | 2.94 | 2.44 |
| 11 | Benzo (b) fluoranthene | <0.1 | <0.1 |
| 12 | Benzo (k) fluoranthene | <0.1 | <0.1 |
| 13 | Benzo (a) pyrene | 3.66 | 2.89 |
| 14 | Indeno (1,2,3-cd) pyrene | <0.1 | <0.1 |
| 15 | Dibenzo (a, h) anthracene | <0.1 | <0.1 |
| 16 | Benzo (g, h, i) perylene | <0.1 | <0.1 |
Therefore the inventive method can be applicable to the high and oily sludge of complexity of the content of organic matter, can be carried out pre-service in oily sludge sample by 16 kinds of Determination of Trace Polycyclic Aromatic Hydrocarbons that environmental area emphasis is monitored, the convenient detection to these palycyclic aromatics.
Claims (9)
1. the detection preprocess method of palycyclic aromatic in oily sludge, comprises the steps:
Preparation of samples: get oily sludge, adds zeyssatite, and grinding, sieves, obtain oily sludge sample;
The rapid extraction of palycyclic aromatic: get oily sludge sample, add substitute, mixing obtains oily sludge potpourri;
Extracted by oily sludge potpourri extract, extraction temperature is 75 DEG C-125 DEG C, and extracting pressure is 1500-1700psi, extracts 3-6 time, each 3-5 minute quiet cycle; Collect extract, extract is concentrated to 1mL-5mL, is extracted concentrate;
The purification of palycyclic aromatic: the filling of chromatographic column: column chromatography silica gel is used methylene chloride soaked overnight after 120-130 DEG C of activation 16-18h, adopt wet method to fill out post, fill out after post completes, layer of silica gel is filled the anhydrous sodium sulfate that 1cm-2cm is thick, with normal hexane drip washing chromatographic column, displacement methylene chloride;
Collect: after chromatographic column balance, concentrate application of sample will be extracted on chromatographic column, abundant contact 5min-10min, use 20mL normal hexane drip washing chromatographic column again, then the mixing eluent drip washing chromatographic column of 20mL-70mL methylene chloride and normal hexane is used, collect eluent, until the mixing eluent of methylene chloride and normal hexane all flows out, obtain the mixed liquor of palycyclic aromatic;
Concentrated: the mixed liquor of concentrated palycyclic aromatic, and nitrogen purging is concentrated into 0.7mL-0.9mL, obtains polyaromatic hydrocarbon samples, completes the detection pre-service of palycyclic aromatic in oily sludge.
2. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: this preprocess method also comprises and add mark in PAHs and the step of constant volume in polyaromatic hydrocarbon samples.
3. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: described oily sludge and diatomaceous amount ratio are 100-200g: 100-200g.
4. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: described in sieve as crossing 70-100 mesh sieve.
5. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: described substitute comprises the combination of one or more in naphthalene-D8, lettuce-D12, perylene-D12.
6. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1 or 5, is characterized in that: the amount ratio of greasy dirt sample and substitute is 0.2-0.5g: 0.1-1mg.
7. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: described extract comprises the combination of one or more in methylene chloride, acetone and acetonitrile.
8. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, is characterized in that: the ratio of the consumption of the silica gel that column chromatography is used and the consumption of oily sludge sample is 8-12g: 0.2-0.5g.
9. the detection preprocess method of palycyclic aromatic in oily sludge according to claim 1, it is characterized in that: in the mixing eluent of described methylene chloride and normal hexane, the volume ratio of methylene chloride and normal hexane is 2:3-3:7.
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