CN107817304A - The detection method of total petroleum hydrocarbon in a kind of soil - Google Patents
The detection method of total petroleum hydrocarbon in a kind of soil Download PDFInfo
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- CN107817304A CN107817304A CN201711003200.2A CN201711003200A CN107817304A CN 107817304 A CN107817304 A CN 107817304A CN 201711003200 A CN201711003200 A CN 201711003200A CN 107817304 A CN107817304 A CN 107817304A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of detection method of total petroleum hydrocarbon in soil, comprise the following steps：A, the concussion extraction of soils and sediments sample, obtains soil liquid to be tested；B, gas chromatographic analysis is handled, and the soil liquid obtained by step A is analyzed and processed；C, calibration process.Determined by correction factor, linear gauging and retention time measure carry out calibration process to soil fluid sample；D, calibration process is verified；E, result is calculated and represented.The detection method of total petroleum hydrocarbon has the characteristics of high sensitivity, precision height and reliability is high in the soil of the present invention.
Description
Technical field
The present invention relates to soil monitoring technical field, the detection method of total petroleum hydrocarbon in particularly a kind of soil.
Background technology
China's soil environment situation totally allows of no optimist, and some areas soil pollution is heavier, and arable soil environmental quality may
Sorrow, industry and mining discarded ground soil environment outstanding problem.In next step, should be from improving Soil Pollution Control policies and regulations standard etc.
Further strengthen Soil Pollution Control work.
It should be revised as early as possible in terms of accelerating to improve Soil Pollution Control policies and regulations standard《Standard of soil environment quality》Deng
Relevant criterion, the standards such as major pollutants analysis test method, soil changes are worked out, protected with constantly improve soil environment
Standards system is protected, meets the needs of soil environment supervision.
Total petroleum hydrocarbon in soil is the important indicator of Soil K+adsorption, and country also analyzes without the unified monitoring of formulation at present
Method, the international and domestic total petroleum hydrocarbon in soil particularly soil mid-boiling point are higher（170℃-430℃）, carbon number is in C10-
The standard method of C35 petroleum hydrocarbon and document are based on infrared spectrophotometer, and domestic temporary method uses national environmental protection
General bureau's establishment《National Soil Pollution Investigation sample analysis measuring technology regulation》In infrared spectrophotometric determination.This
Kind method sensitivity is low；Organic solvent usage amount is big, and error is easily produced during analysis, influences the accuracy of determination data.
How to make measurement is accurately and accurately to need to solve the problems, such as in petroleum hydrocarbon total amount measure.
The content of the invention
The main purpose of the present invention is the provision of a kind of detection method of total petroleum hydrocarbon in soil, has sensitivity
The characteristics of height, high precision height and reliability.
The present invention can be achieved through the following technical solutions：
The invention discloses a kind of detection method of total petroleum hydrocarbon in soil, comprise the following steps：
A, the concussion extraction of soils and sediments sample, obtains soil liquid to be tested；
B, gas chromatographic analysis is handled, and the soil liquid obtained by step A is analyzed and processed；
C, calibration process.Determined by correction factor, linear gauging and retention time measure are calibrated to soil fluid sample
Processing；
D, calibration process is verified；
E, result is calculated and represented:
TPH content meters formula is in pedotheque：
In formula：C0--- the concentration of determinand in the test solution that instrument is read, μ g/mL；
V0--- test solution constant volume, ml；
W --- soil sample amount, g；
N --- extension rate.
Further, the concrete operations of step A comprise the following steps：
A1, removal of impurities processing, remove tree root, leaf and stone impurity, weigh well mixed 20 ± 0.05g of soil sample and enough powder
Last shape anhydrous sodium sulfate, is poured into 250ml volumetric flasks, must increase Na according to soil water content2SO4Amount；
A2, liquid feeding, 100ml 1+1 dichloromethane and the mixed liquor of acetone are pipetted into volumetric flask；
A3, shake up, be put into shaking table and shaken 2 hours or so with 200r/min.
A4, filtering, extract after vibration is filtered, filtering is filled into K-D bottles using anhydrous sodium sulfate, and is put into 4-5
For grain zeolite into K-D bottles, water-bath is concentrated into 5 ml, and bath temperature control is at 85 DEG C, and K-D bottles are with dichloromethane rinse, rinse
Time is 30-40 minutes；
A5, concentration, change K-D pillars and be concentrated into 1 ml, replacing construction one was controlled in 5-10 minutes, was cooled to room temperature；
A6, turn sequence preservation, concentrate is transferred in 2 ml brown sample injection bottles, treats that instrument is analyzed.
Further, in step B, its actual conditions is：Chromatographic column temperature：40 DEG C of holding 3min, then 15 DEG C/min heatings
To 290 DEG C of holding 10min, injector temperature:300 DEG C, detection temperature：300℃.
Further, the concrete operations of step C are：
C1, correction factor measure：C is used for external standard method10-C12, C12-C16, C16-C21And C21-C24, C21-C35The survey of mixture
Determine program, determine each actual sample respectively and chromatographic detector is entered by automatic sampler, determine that it responds peak area, calculate
Its calibration factor：
C2, linear gauging：If the relative standard deviation of calibration factor is less than 20% working range, pass through the linear of origin
To correct, average calibration factor can be used for calibration curve, otherwise must repaint new standard curve;
C3, retention time measure：With the method qualitative analysis each type compound based on retention time.
Further, step D concrete operations are：Verification is by measuring one or more marks containing target determinand
Quasi- sample, if the response of each part be during ± 25% initial calibration in the range of, then it is assumed that the calibration is effective
, it is continuing with the calibration factor CF from initial quantization.
Further, in step A, replacing K-D pillars, which are dried the water for concentrating pipe outer wall with paper, every time prevents the globule
It is dropped in extract, small K-D pipes are wanted to be put into water bath when shaking, and prevent bumping.
Further, in step A, the temperature of water bath is at 85 DEG C, and the bath temperature of K-D pillars is at 80 DEG C.
The detection method of total petroleum hydrocarbon has following beneficial technique effect in soil of the present invention：
Firstth, high sensitivity, total petroleum hydrocarbon is lower than infrared spectrophotometer detection limit in Soil by Gas Chromatography, reaction
It is sensitiveer；
Secondth, precision is high, and total petroleum hydrocarbon is higher than infrared spectrophotometer precision in Soil by Gas Chromatography；
3rd, reliability is high, and total petroleum hydrocarbon is higher than the infrared spectrophotometer degree of accuracy in Soil by Gas Chromatography, data
It is more reliable.
Embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, with reference to embodiment and to this
Invention product is described in further detail.
The invention discloses a kind of detection method of total petroleum hydrocarbon in soil, comprise the following steps：
A, the concussion extraction of soils and sediments sample, obtains soil liquid to be tested；Concrete operations comprise the following steps：
A1, removal of impurities processing, remove tree root, leaf and stone impurity, weigh well mixed 20 ± 0.05g of soil sample and enough powder
Last shape anhydrous sodium sulfate, is poured into 250ml volumetric flasks, must increase Na according to soil water content2SO4Amount；
A2, liquid feeding, 100ml 1+1 dichloromethane and the mixed liquor of acetone are pipetted into volumetric flask；
A3, shake up, be put into shaking table and shaken 2 hours or so with 200r/min.
A4, filtering, extract after vibration is filtered, filtering is filled into K-D bottles using anhydrous sodium sulfate, and is put into 4-5
For grain zeolite into K-D bottles, water-bath is concentrated into 5 ml, and bath temperature control is at 85 DEG C, and K-D bottles are with dichloromethane rinse, rinse
Time is 30-40 minutes；
A5, concentration, change K-D pillars and be concentrated into 1 ml, replacing construction one was controlled in 5-10 minutes, was cooled to room temperature；
A6, turn sequence preservation, concentrate is transferred in 2 ml brown sample injection bottles, treats that instrument is analyzed.
In step A, replacing K-D pillars, which are dried the water for concentrating pipe outer wall with paper, every time prevents the globule to be dropped in extraction
In liquid, small K-D pipes are wanted to be put into water bath when shaking, and prevent bumping.In step A, for the temperature of water bath at 85 DEG C, K-D is small
The bath temperature of post is at 80 DEG C
B, gas chromatographic analysis is handled, and the soil liquid obtained by step A is analyzed and processed；Its actual conditions is：Chromatographic column
Temperature：40 DEG C keep 3min, and then 15 DEG C/min is warming up to 290 DEG C of holding 10min, injector temperature:300 DEG C, detection temperature：300
℃。
C, calibration process.Determined by correction factor, linear gauging and retention time measure are carried out to soil fluid sample
Calibration process；Concrete operations are：
C1, correction factor measure：C is used for external standard method10-C12, C12-C16, C16-C21And C21-C24, C21-C35The survey of mixture
Determine program, determine each actual sample respectively and chromatographic detector is entered by automatic sampler, determine that it responds peak area, calculate
Its calibration factor：
C2, linear gauging：If the relative standard deviation of calibration factor is less than 20% working range, pass through the linear of origin
To correct, average calibration factor can be used for calibration curve, otherwise must repaint new standard curve;
C3, retention time measure：With the method qualitative analysis each type compound based on retention time.
D, calibration process is verified；Concrete operations are：Verification is by measuring one or more marks containing target determinand
Quasi- sample, if the response of each part be during ± 25% initial calibration in the range of, then it is assumed that the calibration is effective
, it is continuing with the calibration factor CF from initial quantization.
E, result is calculated and represented:
TPH content meters formula is in pedotheque：
In formula：C0--- the concentration of determinand in the test solution that instrument is read, μ g/mL；
V0--- test solution constant volume, ml；
W --- soil sample amount, g；
N --- extension rate.
The present invention cardinal principle be：Pass through the total petroleum hydrocarbon in liquid-solid extraction or liquid-liquid extraction soil（TPH）, with 1:1
Dichloromethane/acetone mixture concussion extraction, after anhydrous sodium sulfate is dehydrated, K-D concentrations, finally with dichloromethane constant volume, enters
Gas chromatograph GC-FID carries out quantitative analysis.Using n-alkane C10-C35 mixtures as standard sample, to identical chromatostrip
Chromatographic peak under part in sample between C10-C35 is integrated, so as to obtain quantitative result
In order to further assess the technique effect of the present invention, the following index of this method of testing is assessed respectively, assesses knot
Fruit is as follows：
1st, detection limit
Method detection limit is according to the following formula：
MDL=S×t（N-1,0.99）
The standard deviation of S- parallel determinations,
The sample number of n- replicate analysis,
0.99- confidence levels.
Sample size is 10, sample volume 20g, and when being concentrated into 1.0mL sample introductions, this method detection is limited to 0.2mg/
kg。
2nd, the degree of accuracy
900ug C are added in 10 blank pedotheque 20g that laboratory is prepared5-C35Mix standard liquid（With【CDGG-
113592-02】C5-C35Mixed standard solution,【CDCT-C17894800】C33Standard items,【CDCT-C17430500】C34Standard
Product,【CDCT-C15981700】C35It is prepared by standard items）, rate of recovery experiment is done, is analyzed with gas chromatograph A90, as a result table
Bright petroleum hydrocarbon recovery of standard addition is in 82.5%-97.5%.
3rd, precision
Each continuously measurement 10 times under similarity condition to same 3 pedotheques, examine the precision of this repeated measuring results.As a result
Show petroleum hydrocarbon measured value relative standard deviation in 0.8%-2.5%.
The foregoing is only a preferred embodiment of the present invention, not makees any formal limitation to the present invention；It is all
The those of ordinary skill of the industry can be shown in by specification and described above and swimmingly implement the present invention；It is but all familiar
Professional and technical personnel without departing from the scope of the present invention, makes using disclosed above technology contents
A little variation, modification and evolution equivalent variations, be the present invention equivalent embodiment；Meanwhile all realities according to the present invention
Variation, modification and evolution of any equivalent variations that matter technology is made to above example etc., still fall within the technology of the present invention
Within the protection domain of scheme.
Claims (7)
1. the detection method of total petroleum hydrocarbon in a kind of soil, it is characterised in that comprise the following steps：
A, the concussion extraction of soils and sediments sample, obtains soil liquid to be tested；
B, gas chromatographic analysis is handled, and the soil liquid obtained by step A is analyzed and processed；
C, calibration process, determined by correction factor, linear gauging and retention time measure are calibrated to soil fluid sample
Processing；
D, calibration process is verified；
E, result is calculated and represented:
TPH content meters formula is in pedotheque：
In formula：C0--- the concentration of determinand in the test solution that instrument is read, μ g/mL；
V0--- test solution constant volume, ml；
W --- soil sample amount, g；
N --- extension rate.
2. the detection method of total petroleum hydrocarbon in soil according to claim 1, it is characterised in that：The concrete operations of step A
Comprise the following steps：
A1, removal of impurities processing, remove tree root, leaf and stone impurity, weigh well mixed 20 ± 0.05g of soil sample and enough powder
Last shape anhydrous sodium sulfate, is poured into 250ml volumetric flasks, must increase Na according to soil water content2SO4Amount；
A2, liquid feeding, 100ml 1+1 dichloromethane and the mixed liquor of acetone are pipetted into volumetric flask；
A3, shake up, be put into shaking table and shaken 2 hours or so with 200r/min；
A4, filtering, extract after vibration is filtered, filtering is filled into K-D bottles using anhydrous sodium sulfate, and is put into the boiling of 4-5 grains
For stone into K-D bottles, water-bath is concentrated into 5 ml, and bath temperature control is at 85 DEG C, and K-D bottles are with dichloromethane rinse, rinse time
For 30-40 minutes；
A5, concentration, change K-D pillars and be concentrated into 1 ml, replacing construction one was controlled in 5-10 minutes, was cooled to room temperature；
A6, turn sequence preservation, concentrate is transferred in 2 ml brown sample injection bottles, treats that instrument is analyzed.
3. the detection method of total petroleum hydrocarbon in soil according to claim 1 or 2, it is characterised in that：In step B, it has
Concrete conditions in the establishment of a specific crime is：Chromatographic column temperature：40 DEG C keep 3min, and then 15 DEG C/min is warming up to 290 DEG C of holding 10min, injector temperature:300
DEG C, detection temperature：300℃.
4. the detection method of total petroleum hydrocarbon in soil according to claim 3, it is characterised in that：The concrete operations of step C
For：
C1, correction factor measure：C is used for external standard method10-C12, C12-C16, C16-C21And C21-C24, C21-C35The measure of mixture
Program, each actual sample is determined respectively chromatographic detector is entered by automatic sampler, determine that it responds peak area, calculate it
Calibration factor：
C2, linear gauging：If the relative standard deviation of calibration factor is less than 20% working range, pass through the linear of origin
To correct, average calibration factor can be used for calibration curve, otherwise must repaint new standard curve;
C3, retention time measure：With the method qualitative analysis each type compound based on retention time.
5. the detection method of total petroleum hydrocarbon in soil according to claim 4, it is characterised in that：Step D concrete operations
For：Verification is by measuring one or more standard samples containing target determinand, if the response of each part is
In the range of during ± 25% initial calibration, then it is assumed that the calibration is effective, is continuing with the calibration factor from initial quantization
CF。
6. the detection method of total petroleum hydrocarbon in soil according to claim 5, it is characterised in that：In step A, every time more
Change K-D pillars with paper to dry and prevent the globule to be dropped in extract the water for concentrating pipe outer wall, small K-D pipes are wanted to be put into when shaking
In water bath, bumping is prevented.
7. the detection method of total petroleum hydrocarbon in soil according to claim 6, it is characterised in that：In step A, water bath
Temperature at 85 DEG C, the bath temperature of K-D pillars is at 80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711003200.2A CN107817304A (en) | 2017-10-24 | 2017-10-24 | The detection method of total petroleum hydrocarbon in a kind of soil |
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| CN201711003200.2A CN107817304A (en) | 2017-10-24 | 2017-10-24 | The detection method of total petroleum hydrocarbon in a kind of soil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021232786A1 (en) * | 2020-05-21 | 2021-11-25 | 江苏中之盛环境科技有限公司 | Method for detecting petroleum hydrocarbon components in water |
| CN113916997A (en) * | 2020-07-10 | 2022-01-11 | 上海金艺检测技术有限公司 | Method for measuring volatile petroleum hydrocarbon in soil |
| CN114002340A (en) * | 2021-09-07 | 2022-02-01 | 江苏天宇检测技术有限公司 | Method for detecting petroleum hydrocarbon in polluted 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 |
-
2017
- 2017-10-24 CN CN201711003200.2A patent/CN107817304A/en active Pending
Non-Patent Citations (5)
| Title |
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| A.P.S C H W A B ET AL.: "Extraction of Petroleum Hydrocarbons from Soil by Mechanical Shaking", 《ENVIRON. SCI. TECHNOL.》 * |
| SAMAN C.BUDDAADASA ET AL.: "A comparison between extractant solvents in the quantitative analysis of total petroleum hydrocarbons in soil samples", 《JOURNAL OF THE JAPAN PETROLEUM INSTITUTE》 * |
| 张欢燕 等: "环境中总石油烃的气相色谱分析测定", 《环境监控与预警》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021232786A1 (en) * | 2020-05-21 | 2021-11-25 | 江苏中之盛环境科技有限公司 | Method for detecting petroleum hydrocarbon components in water |
| CN113916997A (en) * | 2020-07-10 | 2022-01-11 | 上海金艺检测技术有限公司 | Method for measuring volatile petroleum hydrocarbon in soil |
| CN113916997B (en) * | 2020-07-10 | 2024-04-05 | 上海金艺检测技术有限公司 | Method for measuring volatile petroleum hydrocarbon in soil |
| CN114002340A (en) * | 2021-09-07 | 2022-02-01 | 江苏天宇检测技术有限公司 | Method for detecting petroleum hydrocarbon in polluted 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 |
| CN114487253B (en) * | 2022-02-14 | 2024-06-21 | 中国石油化工股份有限公司 | Method for determining petroleum hydrocarbon composition in petrochemical polluted site sample |
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