CN107607484A - The method of thimet content in quick measure soil - Google Patents
The method of thimet content in quick measure soil Download PDFInfo
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- CN107607484A CN107607484A CN201711006264.8A CN201711006264A CN107607484A CN 107607484 A CN107607484 A CN 107607484A CN 201711006264 A CN201711006264 A CN 201711006264A CN 107607484 A CN107607484 A CN 107607484A
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Abstract
The invention belongs to field of environment engineering, and in particular to a kind of method of thimet content in quick measure soil, include following step：1) processing of pedotheque；2) preparation of standard curve：2a) configuration standard liquid：The clean soil sample after one group of processing is taken in conical flask, one of them is as blank sample, and remaining is separately added into the thimet of certain mass, and it is in finite concentration gradient to make the thimet in pedotheque, according to liquid-solid ratio 4 after fully mixing:1 adds absolute ethyl alcohol in above-mentioned all pedotheques, shakes up extraction 1h；2b) draw regression curve, fit standard curvilinear equation；3) preparation and extraction of pedotheque to be measured；4) measure of soil sample leaching liquor absorbance to be measured and result calculate；The inventive method makes full use of the ethanol solution of thimet to have characteristic peak at 201nm and 220nm, and detection every time can obtain two results simultaneously, reduce further detection error.
Description
Technical field
The invention belongs to field of environment engineering, and in particular to a kind of method of thimet content in quick measure soil.
Background technology
Thimet is commonly called as 3911, chemical name o, o- diethyl sulfide-Ethylsulfanylmethyl phosphorodithioate (o, o-
Diethyl S- [(ethylsulfanyl) methyl] phosphorodithioate), it is that a kind of efficient, wide spectrum, absorbability are killed
Worm acaricide, belongs to extremely toxic substance, and China completely forbade in 2002 and used.But some once produced the enterprise of thimet
With a large amount of regions for using thimet, its soil all receives the pollution of thimet, resulting Environmental Health in various degree
Risk also more highlights.Therefore, quickly understand soil in thimet content, grasp soil by thimet pollution level very
It is necessary.
Existing market laboratory is using the thimet in gas chromatography detection soil, the method sensitivity and accuracy
It is higher.But gas chromatograph is expensive, use condition requires high, strict to use environment and operating condition requirement, uses
Personnel will pass through special training, cumbersome；The extractant toxicity that detection process is related to is larger, dangerous high；Especially examine
The survey cycle is longer, and the market-oriented test in laboratory cycle is generally up to 3-7 working day, and is generally required in associated restoration engineering fast
Speed judges the pollution level of thimet in soil, has been had a strong impact on using chromatography detection technique and has been repaiied by the environment of thimet pollution
The actual demand for journey of returning to work.
In addition, it is published can be used in detect thimet content method also have luminescence method (CN101706431A) and
Inhibiting AChE (CN1366065A).Both approaches operating process is complicated, respectively including the larger experimentation of workload and more
The preparation process of kind reagent；And be mainly used in water, the detection of the thimet trace residue such as fruits and vegetables, food, do not point out soil
The detection of middle thimet content and the preparation process of pedotheque.
And in thimet contaminated soil remediation engineering field, not yet disclose be exclusively used in thimet in quick detection soil at present
Content, effectively grasp soil in thimet pollution level method.
The content of the invention
It is an object of the invention to overcome the cycle of thimet in prior art detection soil longer, operating environment is harsh,
Expensive equipment, the flow present situation for being difficult to meet engineering site needs such as cumbersome, there is provided thimet contains in a kind of quick measure soil
The method of amount.
The present invention to achieve the above object, using following technical scheme：
A kind of method of thimet content in quick measure soil, it is characterised in that include following step：
1) processing of pedotheque：After soil sample impurities removing, crush and cross 100 mesh sieves after rolling pressure；
2) preparation of standard curve：2a) configuration standard liquid：It is utilized respectively thimet and absolute ethyl alcohol prepares different thimets
The pedotheque and its leaching liquor of pollution concentration；The clean soil sample after one group of processing is taken in conical flask, it is one of as empty
White sample, remaining is separately added into the thimet of certain mass, and it is in finite concentration gradient to make the thimet in pedotheque, fully mixes
Afterwards according to liquid-solid ratio 4:1 adds absolute ethyl alcohol in above-mentioned all pedotheques, shakes up extraction 1h；Regression curve 2b) is drawn, is intended
Standardization curvilinear equation:Using step 2a) in blank sample as control, measure step respectively using visible-ultraviolet specrophotometer
The absorbance of the pedotheque leaching liquor for the different thimet pollution concentrations prepared in 2a), wavelength is 201nm and 220nm, often
Individual leaching liquor is repeated 2 times at different wave length and takes average, then using thimet concentration in soil as abscissa, at different wave length
Absorbance draw two standard curves as ordinate, and try to achieve two regression equation (y respectively1=a1x1+b1, y2=
a2x2+b2), regression equation Linear Quasi is right to be satisfied by R2≥0.9；
3) preparation and extraction of pedotheque to be measured；Pedotheque to be measured takes the soil sample after processing to be placed in cone after processing
In shape bottle, according to liquid-solid ratio 4:1 adds absolute ethyl alcohol, shakes up extraction 1h, while do 1 Duplicate Samples；
4) measure of soil sample leaching liquor absorbance to be measured and result calculate；Using step 2a) in blank sample be used as control, profit
The soil sample leaching liquor to be measured absorbance at 201nm and 220nm respectively, different ripples are determined with visible-ultraviolet specrophotometer
The absorbance of strong point takes average respectively, then substitutes into two corresponding regression equations, two results being calculated respectively respectively
Average is taken again, produces the thimet concentration in pedotheque to be measured；
Appropriate soil sample is taken according to " quartering " in step 1), if soil sample humidity to be measured is larger, crushing can add when rolling pressure
Anhydrous sodium sulfate.
If the concentration of thimet is larger in step 3), appropriate leaching liquor supernatant can be taken and diluted with absolute ethyl alcohol and determined
Hold standby into volumetric flask；Simultaneously corresponding extension rate need to be multiplied by step 4) during result of calculation.
Step 2a) in concretely comprise the following steps：The clean soil sample after one group of not less than 6 sample treatment is taken in 150mL conical flasks
In, each soil sample 10g.
Compared with prior art, the beneficial effects of the invention are as follows：
The inventive method makes full use of the ethanol solution of thimet to have characteristic peak at 201nm and 220nm, every time detection
Two results can be obtained simultaneously, reduce further detection error.
The inventive method equally has higher sensitivity and preferably repeatability compared with existing gas chromatography；
And operating environment requires low, the chemicals larger without the instrument and toxicity of costliness；Particularly detection time is shorter (about 3h),
Be particularly suitable for use in engineering site, realizes the thimet content in quick measure soil, accurate to grasp thimet pollution journey in soil
The purpose of degree.
Brief description of the drawings
Fig. 1 is the stable spy that the ethanol solution of various concentrations thimet of the present invention shows at 201nm and 220nm
Levy peak schematic diagram.
Embodiment
In order that those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and most
The present invention is described in further detail for good embodiment.Fig. 1 shows the ethanol solution of various concentrations thimet of the present invention
The invariant feature peak figure showed at 201nm and 220nm.
Case study on implementation 1:The detection of thimet in Tianjin insecticide factory thimet workshop contaminated soil
1) after pedotheque, is rejected into the debris such as stone, branch, appropriate soil sample is taken according to " quartering ", then through broken
100 mesh sieves are crossed after rolling pressure.(the pedotheque processing being related to below is carried out by this step)
2a), taking the clean soil sample after 6 processing, each soil sample 10g, one of them is as blank in 150mL conical flasks
Sample, remaining is separately added into 0.1mg, 0.2mg, 0.4mg, 0.6mg, 0.8mg thimet, according to liquid-solid ratio 4 after fully mixing:1
Absolute ethyl alcohol is added in above-mentioned all pedotheques, shakes up extraction 1h；
2b), using step 2a) in blank sample as control, measure step 1 respectively using visible-ultraviolet specrophotometer and match somebody with somebody
The absorbance of the pedotheque leaching liquor of the different thimet pollution concentrations of system, wavelength are 201nm and 220nm, each extraction
Liquid is repeated 2 times at different wave length and takes average, then using thimet concentration in soil as abscissa (unit 103mg/kg),
Absorbance at different wave length draws two standard curves as ordinate, and tries to achieve two regression equation (y respectively1=
0.793x1, R1 2=0.96, y2=0.537x2, R2 2=0.93)；
3), after processing, soil sample is placed in the 150mL conical flasks of cleaning pedotheque to be measured after taking 10g sieves, is consolidated according to liquid
Than 4:1 adds absolute ethyl alcohol, shakes up extraction 1h, while do 1 Duplicate Samples；
4), using step 2a) in blank sample as control, utilize visible-ultraviolet specrophotometer to determine soil sample to be measured extraction
The liquid absorbance at 201nm and 220nm respectively, the absorbance at different wave length take respectively average (A201nm=0.158,
A220nm=0.104), two corresponding regression equations are then substituted into respectively, two results being calculated respectively take average again,
The thimet concentration produced in pedotheque to be measured is about 196.5mg/kg.
The detection of thimet in the neighbouring contaminated soil of the Tianjin insecticide factory sewage treatment facility of case study on implementation 2
1) after pedotheque, is rejected into the debris such as stone, branch, appropriate soil sample is taken according to " quartering ", is then added suitable
The anhydrous sodium sulfate of amount, 100 mesh sieves are crossed after crushing and rolling pressure.(the pedotheque processing being related to below is carried out by this step)
2a), taking the clean soil sample after 6 processing, each soil sample 10g, one of them is as blank in 150mL conical flasks
Sample, remaining is separately added into 1mg, 2mg, 4mg, 6mg, 8mg thimet, according to liquid-solid ratio 4 after fully mixing:1 above-mentioned all
Absolute ethyl alcohol is added in pedotheque, shakes up extraction 1h；
2b), using step 2a) in blank sample as control, measure step 1 respectively using visible-ultraviolet specrophotometer and match somebody with somebody
The absorbance of the pedotheque leaching liquor of the different thimet pollution concentrations of system, wavelength are 201nm and 220nm, each extraction
Liquid is repeated 2 times at different wave length and takes average, then using thimet concentration in soil as abscissa (unit 102mg/kg),
Absorbance at different wave length draws two standard curves as ordinate, and tries to achieve two regression equation (y respectively1=
8.634x1, R1 2=0.95, y2=5.921x2, R2 2=0.97)；
3), after processing, soil sample is placed in the 150mL conical flasks of cleaning pedotheque to be measured after taking 10g sieves, is consolidated according to liquid
Than 4:1 adds absolute ethyl alcohol, shakes up extraction 1h, while does 1 Duplicate Samples, takes 0.1mL leaching liquors supernatant and uses absolute ethyl alcohol
It is settled to standby in 50mL volumetric flasks；
4), using step 2a) in blank sample as control, utilize visible-ultraviolet specrophotometer to determine soil sample to be measured extraction
The liquid absorbance at 201nm and 220nm respectively, the absorbance at different wave length take respectively average (A201nm=0.327,
A220nm=0.213), two corresponding regression equations are then substituted into respectively, two results being calculated respectively take average again,
For result of calculation multiplied by with 500 (extension rates), the thimet concentration produced in pedotheque to be measured is about 1850mg/kg.
The detection of thimet in the Wuhan insecticide factory contaminated soil of case study on implementation 3
1) after pedotheque, is rejected into the debris such as stone, branch, appropriate soil sample is taken according to " quartering ", then through broken
100 mesh sieves are crossed after rolling pressure.(the pedotheque processing being related to below is carried out by this step)
2a), taking the clean soil sample after 6 processing, each soil sample 10g, one of them is as blank in 150mL conical flasks
Sample, remaining is separately added into 1mg, 2mg, 4mg, 6mg, 8mg thimet, according to liquid-solid ratio 4 after fully mixing:1 above-mentioned all
Absolute ethyl alcohol is added in pedotheque, shakes up extraction 1h；
2b), using step 2a) in blank sample as control, measure step 1 respectively using visible-ultraviolet specrophotometer and match somebody with somebody
The absorbance of the pedotheque leaching liquor of the different thimet pollution concentrations of system, wavelength are 201nm and 220nm, each extraction
Liquid is repeated 2 times at different wave length and takes average, then using thimet concentration in soil as abscissa (unit 102mg/kg),
Absorbance at different wave length draws two standard curves as ordinate, and tries to achieve two regression equation (y respectively1=
8.594x1, R1 2=0.91, y2=6.221x2, R2 2=0.91)；
3), after processing, soil sample is placed in the 150mL conical flasks of cleaning pedotheque to be measured after taking 10g sieves, is consolidated according to liquid
Than 4:1 adds absolute ethyl alcohol, shakes up extraction 1h, while do 1 Duplicate Samples；
4), using step 2a) in blank sample as control, utilize visible-ultraviolet specrophotometer to determine soil sample to be measured extraction
The liquid absorbance at 201nm and 220nm respectively, the absorbance at different wave length take respectively average (A201nm=0.893,
A220nm=0.684), two corresponding regression equations are then substituted into respectively, two results being calculated respectively take average again,
The thimet concentration produced in pedotheque to be measured is about 10.7mg/kg.
The measure of the method standard rate of recovery in specific embodiment of the invention 1-3：Add 1mg's in thimet pollutes soil sample
Thimet standard items, are then detected with this method, are repeated twice, and as a result calculate its sample TIANZHU XINGNAO Capsul up to 90%
More than, while compareed with gas chromatography test result, coincidence rate is up to more than 80%.
The repeatability and stability of the inventive method：It is respectively 10mg/kg and 100mg/kg thimet with self-control content
Pollution soil sample is detection object, the thimet pollution soil sample of two kinds of different contents is divided into two groups, every group of sample number is 7, profit
Two groups of pedotheques are determined with this method, every group of each survey 1, continuous to survey one week daily, obtains variation within batch coefficient and batch anaplasia
Different coefficient is respectively 3.88% and 4.79%, the repeatability of method and is had good stability.
The inventive method requires that the pedotheque of different measurement batches needs to do standard curve again, to ensure measurement result
Accuracy, when there is obvious concentration difference especially between different batches.
The inventive method makes full use of the ethanol solution of thimet to have characteristic peak at 201nm and 220nm, every time detection
Two results can be obtained simultaneously, reduce further detection error.
The inventive method equally has higher sensitivity and preferably repeatability compared with existing gas chromatography；
And operating environment requires low, the chemicals larger without the instrument and toxicity of costliness；Particularly detection time is shorter (about 3h),
Be particularly suitable for use in engineering site, realizes the thimet content in quick measure soil, accurate to grasp thimet pollution journey in soil
The purpose of degree.
Claims (4)
1. a kind of method of thimet content in quick measure soil, it is characterised in that include following step：
1) processing of pedotheque：After soil sample impurities removing, crush and cross 100 mesh sieves after rolling pressure；
2) preparation of standard curve：2a) configuration standard liquid：It is utilized respectively thimet and absolute ethyl alcohol prepares different thimet pollutions
The pedotheque and its leaching liquor of concentration；The clean soil sample after one group of processing is taken in conical flask, one of them as blank sample,
Remaining is separately added into the thimet of certain mass, and it is in finite concentration gradient to make the thimet in pedotheque, is pressed after fully mixing
According to liquid-solid ratio 4:1 adds absolute ethyl alcohol in above-mentioned all pedotheques, shakes up extraction 1h；2b) draw regression curve, fitting mark
Directrix curve equation:Using step 2a) in blank sample as control, measure step 2a respectively using visible-ultraviolet specrophotometer) in
The absorbance of the pedotheque leaching liquor of the different thimet pollution concentrations of preparation, wavelength are 201nm and 220nm, each leaching
Extract is repeated 2 times at different wave length and takes average, then using thimet concentration in soil as abscissa, the suction at different wave length
Shading value draws two standard curves as ordinate, and tries to achieve two regression equation (y respectively1=a1x1+b1, y2=a2x2+
b2), regression equation Linear Quasi is right to be satisfied by R2≥0.9；
3) preparation and extraction of pedotheque to be measured；Pedotheque to be measured takes the soil sample after processing to be placed in conical flask after processing
In, according to liquid-solid ratio 4:1 adds absolute ethyl alcohol, shakes up extraction 1h, while do 1 Duplicate Samples；
4) measure of soil sample leaching liquor absorbance to be measured and result calculate；Using step 2a) in blank sample as control, using can
See-ultraviolet specrophotometer determines the soil sample leaching liquor to be measured absorbance at 201nm and 220nm respectively, at different wave length
Absorbance take average respectively, then substitute into two corresponding regression equations respectively, two results being calculated respectively take again
Average, produce the thimet concentration in pedotheque to be measured.
2. the method for thimet content in quick measure soil according to claim 1, it is characterised in that in step 1)
Appropriate soil sample is taken according to " quartering ", if soil sample humidity to be measured is larger, anhydrous sodium sulfate can be added when rolling pressure by crushing.
3. the method for thimet content in quick measure soil according to claim 1, it is characterised in that in step 3) such as
The concentration of fruit thimet is larger, can take appropriate leaching liquor supernatant and is settled to absolute ethyl alcohol dilution standby in volumetric flask；
Simultaneously corresponding extension rate need to be multiplied by step 4) during result of calculation.
4. the method for thimet content in quick measure soil according to claim 1, it is characterised in that step 2a) in
Concretely comprise the following steps：The clean soil sample after one group of not less than 6 sample treatment is taken in 150mL conical flasks, each soil sample 10g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632448A (en) * | 2018-11-27 | 2019-04-16 | 浙江大学 | A kind of concentration and separation method of colloid phosphorus in soil |
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