CN110361465A - The component method of separating and assaying of total petroleum hydrocarbon in soil - Google Patents

The component method of separating and assaying of total petroleum hydrocarbon in soil Download PDF

Info

Publication number
CN110361465A
CN110361465A CN201910566015.7A CN201910566015A CN110361465A CN 110361465 A CN110361465 A CN 110361465A CN 201910566015 A CN201910566015 A CN 201910566015A CN 110361465 A CN110361465 A CN 110361465A
Authority
CN
China
Prior art keywords
hydrocarbon
chromatographic column
total petroleum
column
soil
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910566015.7A
Other languages
Chinese (zh)
Inventor
凌冰
黄晓
高巨鹏
张�林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Baosteel Industry Technological Service Co Ltd
Original Assignee
Shanghai Baosteel Industry Technological Service Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Baosteel Industry Technological Service Co Ltd filed Critical Shanghai Baosteel Industry Technological Service Co Ltd
Priority to CN201910566015.7A priority Critical patent/CN110361465A/en
Publication of CN110361465A publication Critical patent/CN110361465A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a kind of component method of separating and assaying of total petroleum hydrocarbon in soil, pedotheque is extracted into organic solvent with accelerated solvent extraction mode by this method, and extract liquor is concentrated after the completion of extraction;Aluminium oxide is inserted in chromatographic column, the extract liquor of concentration is flowed through into chromatographic column, and aliphatic hydrocarbon in chromatographic column and aromatic hydrocarbon are eluted out and are collected with n-hexane and methylene chloride respectively;Enriching fat hydrocarbon and aromatic hydrocarbon collection liquid, the aliphatic hydrocarbon and aromatic hydrocarbon collection liquid of concentration respectively enter gas chromatographicanalyzer analysis, obtain the concentration of aliphatic hydrocarbon and aromatic hydrocarbon in total petroleum hydrocarbon.This method is easy to operate, realizes the separation determination of aliphatic hydrocarbon and aromatic component in total petroleum hydrocarbon, is conducive to avoid environmental pollution, it is ensured that human health to the judgement of the total petroleum hydrocarbon extent of injury in soil.

Description

The component method of separating and assaying of total petroleum hydrocarbon in soil
Technical field
The present invention relates to a kind of component separation determination sides of total petroleum hydrocarbon in analysis and testing technology field more particularly to soil Method.
Background technique
Petroleum hydrocarbon is one of the organic pollutant being widely present in current environment, including gasoline, kerosene, diesel oil, lubrication Oil, paraffin and pitch etc., are a variety of hydro carbons (normal alkane, branched paraffin, cycloalkane, aromatic hydrocarbons) and other organic matters on a small quantity, Such as sulfide, nitride, naphthenic mixture.With the development of economy, demand of the mankind to the energy constantly expands, Petroleum has become one of most important energy of the mankind.During the exploitation of petroleum, processing and utilization, more and more petroleum Soil environment and ocean may be entered so as to cause the pollution of soil environment and ocean water quality and destroy the excessive total petroleum of Hydrocarbon, which once enters soil, would become hard to be excluded, and will cause serious harm to society, economy and the mankind.And excessive oil hydrocarbon Into ocean, it can assemble in marine organism, as food chain enters human body, endanger human health.
It is mainly at present to measure total stone according to 2007 gas chromatography of EPA 8015C to the detection of total petroleum hydrocarbon in soil The total amount of petroleum hydrocarbon, but this method can not judge the constituent of total petroleum hydrocarbon, and aliphatic hydrocarbon and fragrance in the composition of total petroleum hydrocarbon The toxicity and the extent of injury of hydrocarbon have apparent difference, therefore for the separation determination of aliphatic hydrocarbon in total petroleum hydrocarbon and aromatic component It is of great significance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of component method of separating and assaying of total petroleum hydrocarbon in soil, originally Method is easy to operate, realizes the separation determination of aliphatic hydrocarbon and aromatic component in total petroleum hydrocarbon, is conducive to petroleum total in soil The judgement of the hydrocarbon extent of injury, avoids environmental pollution, it is ensured that human health.
In order to solve the above technical problems, the component method of separating and assaying of total petroleum hydrocarbon includes following step in soil of the present invention It is rapid:
Step 1: pedotheque is extracted into organic solvent with accelerated solvent extraction mode, extract liquor is concentrated after the completion of extraction To 1ml;
Step 2: inserting aluminium oxide in chromatographic column, extract liquor is flowed through into chromatographic column, uses n-hexane and methylene chloride by layer respectively Aliphatic hydrocarbon and aromatic hydrocarbon are eluted out and collect in analysis column;
Step 3: enriching fat hydrocarbon and aromatic hydrocarbon collection liquid are to 1ml, the aliphatic hydrocarbon and aromatic hydrocarbon collection liquid of concentration respectively enter gas The analysis of analysis of hplc instrument, obtains the concentration of aliphatic hydrocarbon and aromatic hydrocarbon in total petroleum hydrocarbon.
Further, in step 1, a piece of cellulose filter membrane is added in extraction bottom of pond portion, successively add 2g florisil silica, Then cellulose filter membrane is placed in abstraction pool top by the pedotheque and 2g quartz sand that 20g and diatomite mix well, open and add Extract liquor is concentrated into 1ml by nitrogen evaporator using after anhydrous sodium sulfate filtering means dehydration after the completion by the extraction of quick-dissolving agent abstraction instrument.
Further, in step 2,20ml n-hexane is added in 1ml concentrated extract, is concentrated into 1ml, mistake through nitrogen evaporator Alumina column, alumina column are that 10g aluminium oxide is added in chromatographic column, and tapping dress column, chromatographic column upper layer adds 1cm anhydrous slufuric acid Sodium;With 50 ml normal hexane prewashing chromatographic columns, eluate is discarded, 1ml concentration extraction is shifted before anhydrous sodium sulfate is exposed to air Liquid separately completes the transfer of concentrated extract to chromatographic column upper end with the rinse of 1ml normal hexane;Keep chromatographic column upper layer anhydrous sodium sulfate In solvent, with total amount 15ml normal hexane elution chromatography column, eluate is collected with 250ml flask, marks it for aliphatic hydrocarbon;Adjustment Flow velocity is 2mL/min, collects eluate with 100ml dichloromethane eluent chromatographic column, and with 250ml flask, and it is fragrant for marking it Hydrocarbon.
Further, in step 3, the analysis condition of gas chromatographicanalyzer be using DB-5 chromatographic column, 1.5 mL/min's Constant current mode, injector temperature 300oC, Splitless injecting samples, column temperature are 50oC in the initial stage and are kept for 2 minutes, the first stage 200 oC are warming up to the rate of 30 oC/minute, second stage is warming up to 325 oC with the rate of 15oC/minute and protects It holds 5 minutes.
Since the component method of separating and assaying of total petroleum hydrocarbon in soil of the present invention uses above-mentioned technical proposal, i.e. this method will be native Earth sample is extracted into organic solvent with accelerated solvent extraction mode, and extract liquor is concentrated after the completion of extraction;It is inserted in chromatographic column The extract liquor of concentration is flowed through chromatographic column by aluminium oxide, uses n-hexane and methylene chloride by aliphatic hydrocarbon in chromatographic column and fragrance respectively Hydrocarbon is eluted out and collects;Enriching fat hydrocarbon and aromatic hydrocarbon collection liquid, the aliphatic hydrocarbon and aromatic hydrocarbon collection liquid of concentration respectively enter Gas chromatographicanalyzer analysis, obtains the concentration of aliphatic hydrocarbon and aromatic hydrocarbon in total petroleum hydrocarbon.This method is easy to operate, realizes total stone The separation determination of aliphatic hydrocarbon and aromatic component in petroleum hydrocarbon is conducive to avoid the judgement of the total petroleum hydrocarbon extent of injury in soil Environmental pollution, it is ensured that human health.
Specific embodiment
Embodiment 1: pedotheque is extracted into organic solvent using accelerated solvent extraction mode by this method, after the completion of extraction Extract liquor is concentrated to 1ml;Insert aluminium oxide in chromatographic column, concentrated extract flowed through into chromatographic column, respectively with n-hexane and Aliphatic hydrocarbon in chromatographic column and aromatic hydrocarbon are eluted out and are collected by methylene chloride;Enriching fat hydrocarbon and aromatic hydrocarbon collection liquid are to 1ml And it respectively enters gas chromatographicanalyzer to be analyzed, obtains the concentration of aliphatic hydrocarbon and aromatic hydrocarbon in total petroleum hydrocarbon.
On the basis of embodiment 1, sample preparation is that a piece of cellulose filter membrane is added in extraction bottom of pond portion, successively adds 2g The pedotheque and 2g quartz sand that florisil silica, 20g and diatomite mix well, are then placed in extraction for cellulose filter membrane Accelerated solvent extraction extraction is opened on pond top, after the completion blows extract liquor by nitrogen using after anhydrous sodium sulfate filtering means dehydration Instrument is concentrated into 1ml.
On the basis of embodiment 1, aliphatic hydrocarbon and being separated into for aromatic hydrocarbon add in 1ml concentrated extract in total petroleum hydrocarbon Entering 20ml n-hexane, is concentrated into 1ml, peroxidating aluminium column through nitrogen evaporator, alumina column is that 10g aluminium oxide is added in chromatographic column, Tapping dress column, chromatographic column upper layer adds 1cm anhydrous sodium sulfate;With 50 ml normal hexane prewashing chromatographic columns, eluate is discarded, anhydrous Transfer 1ml concentrated extract separately completes concentration extraction with the rinse of 1ml normal hexane to chromatographic column upper end before sodium sulphate is exposed to air The transfer of liquid;It keeps chromatographic column upper layer anhydrous sodium sulfate in solvent, with total amount 15ml normal hexane elution chromatography column, uses 250ml Flask collects eluate, marks it for aliphatic hydrocarbon;Adjustment flow velocity is 2mL/min, with 100ml dichloromethane eluent chromatographic column, and Eluate is collected with 250ml flask, marks it for aromatic hydrocarbon.
The analysis condition of gas chromatographicanalyzer is using DB-5 chromatographic column, the constant current mould of 1.5 mL/min in this method Formula, injector temperature 300oC, Splitless injecting samples, column temperature are 50oC in the initial stage and are kept for 2 minutes that the first stage is with 30 o The rate of C/minute is warming up to 200 oC, and second stage is warming up to 325 oC with the rate of 15oC/minute and is kept for 5 points Clock.
The principle of this method is that adsorption capacity according to substance on stationary phase (aluminium oxide) is different and separate each component;One As in the case of the biggish substance of polarity be easily fixed phase (aluminium oxide) absorption, the weaker substance of polarity is not easy to be fixed phase (oxidation Aluminium) absorption.When using solvent elution, occur a series of absorption → desorption → process adsorbed → desorbed again again, adsorption capacity compared with The mobile distance of strong component is small, afterwards column out;The adsorption capacity distance mobile compared with weak component is big, first column out.The polarity of aliphatic hydrocarbon It is weaker, eluted first by solvent, and the polarity of aromatic hydrocarbon is stronger, after be eluted, to achieve the purpose that component separates.After separation Group be distributed into gas chromatographicanalyzer analysis, obtain the concentration of component.
This method can still use the gas chromatographicanalyzer (fid detector) conventionally used for analyzing total petroleum hydrocarbon to carry out Analysis saves cost without increasing equipment investment.Aliphatic hydrocarbon and fragrance are completely segregated into through total petroleum hydrocarbon in this method soil Hydrocarbon and respectively examinations are conducive to the specific aim selection of the judgement and subsequent improvement to soil pollutant source.

Claims (4)

1. the component method of separating and assaying of total petroleum hydrocarbon in a kind of soil, it is characterised in that this method includes the following steps:
Step 1: pedotheque is extracted into organic solvent with accelerated solvent extraction mode, extract liquor is concentrated after the completion of extraction To 1ml;
Step 2: inserting aluminium oxide in chromatographic column, extract liquor is flowed through into chromatographic column, uses n-hexane and methylene chloride by layer respectively Aliphatic hydrocarbon and aromatic hydrocarbon are eluted out and collect in analysis column;
Step 3: enriching fat hydrocarbon and aromatic hydrocarbon collection liquid are to 1ml, the aliphatic hydrocarbon and aromatic hydrocarbon collection liquid of concentration respectively enter gas The analysis of analysis of hplc instrument, obtains the concentration of aliphatic hydrocarbon and aromatic hydrocarbon in total petroleum hydrocarbon.
2. the component method of separating and assaying of total petroleum hydrocarbon in soil according to claim 1, it is characterised in that: step 1 In, a piece of cellulose filter membrane is added in extraction bottom of pond portion, successively adds what 2g florisil silica, 20g and diatomite mixed well Then cellulose filter membrane is placed in abstraction pool top by pedotheque and 2g quartz sand, open accelerated solvent extraction extraction, complete Extract liquor is concentrated into 1ml by nitrogen evaporator using after anhydrous sodium sulfate filtering means dehydration afterwards.
3. the component method of separating and assaying of total petroleum hydrocarbon in soil according to claim 1, it is characterised in that: step 2 In, 20ml n-hexane is added in 1ml concentrated extract, is concentrated into 1ml through nitrogen evaporator, peroxidating aluminium column, alumina column be 10g aluminium oxide is added in chromatographic column, tapping dress column, chromatographic column upper layer adds 1cm anhydrous sodium sulfate;With 50 ml normal hexane prewashing Chromatographic column discards eluate, and 1ml concentrated extract is shifted before anhydrous sodium sulfate is exposed to air to chromatographic column upper end, another use The transfer of 1ml normal hexane rinse completion concentrated extract;Keep chromatographic column upper layer anhydrous sodium sulfate in solvent, with total amount 15ml Normal hexane elution chromatography column collects eluate with 250ml flask, marks it for aliphatic hydrocarbon;Adjustment flow velocity is 2mL/min, is used 100ml dichloromethane eluent chromatographic column, and eluate is collected with 250ml flask, mark it for aromatic hydrocarbon.
4. the component method of separating and assaying of total petroleum hydrocarbon in soil according to claim 1, it is characterised in that: step 3 In, the analysis condition of gas chromatographicanalyzer is using DB-5 chromatographic column, the constant current mode of 1.5 mL/min, injector temperature 300oC, Splitless injecting samples, column temperature are 50oC in the initial stage and are kept for 2 minutes that the first stage is with the rate of 30 oC/minute 200 oC are warming up to, second stage is warming up to 325 oC with the rate of 15oC/minute and is kept for 5 minutes.
CN201910566015.7A 2019-06-27 2019-06-27 The component method of separating and assaying of total petroleum hydrocarbon in soil Pending CN110361465A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910566015.7A CN110361465A (en) 2019-06-27 2019-06-27 The component method of separating and assaying of total petroleum hydrocarbon in soil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910566015.7A CN110361465A (en) 2019-06-27 2019-06-27 The component method of separating and assaying of total petroleum hydrocarbon in soil

Publications (1)

Publication Number Publication Date
CN110361465A true CN110361465A (en) 2019-10-22

Family

ID=68217172

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910566015.7A Pending CN110361465A (en) 2019-06-27 2019-06-27 The component method of separating and assaying of total petroleum hydrocarbon in soil

Country Status (1)

Country Link
CN (1) CN110361465A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111521715A (en) * 2020-06-10 2020-08-11 浙江省地质矿产研究所 Method for detecting total petroleum hydrocarbon C in soil and sediment10~C40Method (2)
CN114216981A (en) * 2021-12-15 2022-03-22 广西壮族自治区海洋环境监测中心站 Method for detecting petroleum hydrocarbon in marine sediment
CN114487253A (en) * 2022-02-14 2022-05-13 中国石油化工股份有限公司 Method for determining petroleum hydrocarbon composition in petrochemical pollution site environment sample
CN114486415A (en) * 2021-12-23 2022-05-13 广东贝源检测技术股份有限公司 Method for extracting petroleum hydrocarbon in soil
CN115078577A (en) * 2022-06-14 2022-09-20 国网河北省电力有限公司电力科学研究院 Method for detecting petroleum hydrocarbon in soil

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0067372A1 (en) * 1981-06-15 1982-12-22 Asahi Kasei Kogyo Kabushiki Kaisha Liquid chromatography process
CN108318606A (en) * 2018-01-16 2018-07-24 中国海洋石油集团有限公司 Improve Full-automatic solid phase extraction instrument and its application in single fragrant gonane automation separation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0067372A1 (en) * 1981-06-15 1982-12-22 Asahi Kasei Kogyo Kabushiki Kaisha Liquid chromatography process
CN108318606A (en) * 2018-01-16 2018-07-24 中国海洋石油集团有限公司 Improve Full-automatic solid phase extraction instrument and its application in single fragrant gonane automation separation

Non-Patent Citations (8)

* Cited by examiner, † Cited by third party
Title
凌冰等: "加速溶剂萃取-气相色谱/质谱法测定土壤中多环芳烃", 《第十届中国钢铁年会暨第六届宝钢学术年会论文集》, pages 1 *
凌冰等: "加速溶剂萃取-气相色谱/质谱法测定土壤中有机氯", 《山东化工》, vol. 44, no. 12, pages 1 *
姜岩等: "土壤中石油烃预处理及含量分析方法研究进展①", 《土壤》 *
姜岩等: "土壤中石油烃预处理及含量分析方法研究进展①", 《土壤》, vol. 47, no. 3, 31 December 2015 (2015-12-31), pages 461 - 464 *
李建勇等: "利用快速溶剂萃取仪测定土壤中总石油烃", 《分析测试学报》, vol. 31 *
杨慧娟等: "气相色谱-质谱法分段测定土壤中的可提取总石油烃①", 《土壤》 *
杨慧娟等: "气相色谱-质谱法分段测定土壤中的可提取总石油烃①", 《土壤》, vol. 46, no. 1, 31 December 2014 (2014-12-31), pages 461 - 464 *
郑南荣: "气相色谱法测定土壤中有机氯农药残留", 《科技与创新》, no. 3, pages 1 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111521715A (en) * 2020-06-10 2020-08-11 浙江省地质矿产研究所 Method for detecting total petroleum hydrocarbon C in soil and sediment10~C40Method (2)
CN111521715B (en) * 2020-06-10 2022-07-19 浙江省地质矿产研究所 Method for detecting total petroleum hydrocarbon C in soil and sediment10~C40Method (2)
CN114216981A (en) * 2021-12-15 2022-03-22 广西壮族自治区海洋环境监测中心站 Method for detecting petroleum hydrocarbon in marine sediment
CN114486415A (en) * 2021-12-23 2022-05-13 广东贝源检测技术股份有限公司 Method for extracting petroleum hydrocarbon in soil
CN114486415B (en) * 2021-12-23 2024-06-07 广东贝源检测技术股份有限公司 Method for extracting petroleum hydrocarbon from soil
CN114487253A (en) * 2022-02-14 2022-05-13 中国石油化工股份有限公司 Method for determining petroleum hydrocarbon composition in petrochemical pollution site environment sample
CN115078577A (en) * 2022-06-14 2022-09-20 国网河北省电力有限公司电力科学研究院 Method for detecting petroleum hydrocarbon in soil

Similar Documents

Publication Publication Date Title
CN110361465A (en) The component method of separating and assaying of total petroleum hydrocarbon in soil
CN102393429B (en) Method for detecting trace phosphine gas in water sample by gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method
CN102520101A (en) Pre-treatment and analysis methods of organochlorine pesticides in soil
CN104749287B (en) The assay method of Xiu Dai bioxin in environmental sample
CN105510505A (en) Method for measuring content of dioxins in tea and rice
CN103776924A (en) Method for detecting polycyclic aromatic hydrocarbon in fried food
CN108572231A (en) The method of hydrophobicity eutectic solvent vortex aid dispersion liquid-liquid micro-extraction-high performance liquid chromatography detection Sudan red 1
CN101706484B (en) Method for synchronously purifying and separating organic extract of environmental medium step by step
CN102590411B (en) Method for detecting divalent cadmium ion in aquatic product by using HPLC-ICP-MS coupling technique
CN101241112A (en) Chinese herbal medicine residual organochlorine insecticide detection method
CN107192596A (en) Method for preparing purified for the THC standard substance of forensic science illicit drugs inspection
CN104407079A (en) Method for extracting polycyclic aromatic hydrocarbons from industrial wastewater
Jentoft et al. Analysis of polynuclear aromatic hydrocarbons in automobile exhaust by supercritical fluid chromatography
CN106053635A (en) Method of measuring polycyclic aromatic hydrocarbon in plant leaves
CN104391063B (en) Microneedle capturing device novelty teabag
CN107102074A (en) The GC MS analysis methods of polycyclic aromatic hydrocarbon in a kind of quantitative analysis aquatic products
Kang et al. Speciation of selenium in soil
CN201399261Y (en) Full-automatic extraction apparatus
JP2008008622A (en) Oil component measuring method
CN111085006A (en) Process for extracting organic pollutants in environment
CN109557223A (en) QuEChERs pillar and its application
CN110031585A (en) A method of measurement alkyl phenol Determination of oil-water partition coefficient
CN209696354U (en) A kind of organic matter auxiliary separating device
Ternon et al. Comprehensive analytical methodology to determine hydrocarbons in marine waters using extraction disks coupled to glass fiber filters and compound-specific isotope analyses
CN106542974B (en) A kind of method of sulfide in enrichment methyl tertiary-butyl ether

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20191022

RJ01 Rejection of invention patent application after publication