CN106248708A - A kind of X fluorescence spectrum method rapid assay methods to heavy metals in soil lead - Google Patents
A kind of X fluorescence spectrum method rapid assay methods to heavy metals in soil lead Download PDFInfo
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- CN106248708A CN106248708A CN201610776494.1A CN201610776494A CN106248708A CN 106248708 A CN106248708 A CN 106248708A CN 201610776494 A CN201610776494 A CN 201610776494A CN 106248708 A CN106248708 A CN 106248708A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a kind of X fluorescence spectrum method rapid assay methods to heavy metals in soil lead, including: 1) take a certain amount of soil powder；2) described soil powder loaded specimen cup and is compacted with Manual tablet pressing machine, forming testing sample；3) being put into by testing sample in sample test box, this testing cassete includes: shell, and described shell upper end has hole, is provided with shell fragment in hole；Sample stage, described sample stage is arranged on the bottom of described enclosure；Hand-held set, there is N number of groove described hand-held set front end, and described hand-held set is coupled with described sample test box by the cooperation of groove and described shell fragment；4) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of testing sample；And 5) X-fluorescence intensity based on described testing sample, the lead element content being calculated in this soil；The method of the invention uses Portable X fluorescent spectrometry that pedotheque can directly carry out lead element quantitative analysis, test rate of accuracy reached is to more than 96%, method of testing is simple to operate, pollution-free, no material consumption, simultaneously, the assay method of embodiments of the invention has the further advantage that volume is little, portable, facilitate field work, field assay.
Description
Technical field
The present invention relates to environment measuring, it particularly relates to the assay method of a kind of Lead In Soil element.
Background technology
In recent years, heavy metal pollution Frequent Accidents, as Fengxiang, Shaanxi children blood lead exceed standard, the arsenic contamination accident of Linyi, Shandong,
Liuyang hunan lead contamination event, Zijin Mining contamination accident, Longjiang, Guangxi lead contamination event etc..These heavy metal pollution events are not
But bring great economic loss to society and also threaten the healthy living of people, also cause the height of relevant environmental administration of country
Degree is paid attention to, and simultaneously Heavy Metal Pollution, in-depth heavy metal monitoring is put in more urgent, more importantly position
On；, GB chemical detection method is substantially belonged to for the detection of heavy metals in soil lead, sample need to be carried out acid treatment,
Processing method typically uses Microwave Digestion, Wet method etc., complex operation, uses strong acid simultaneously, has a large amount of acid gas to produce,
Whole sample processing time is long, at least 2 hours, wastes time and energy；The method can only sampling and testing simultaneously, it is impossible to meet on-the-spot quickly
The requirement of test.
In order to meet the requirement of on-the-spot quickly test, we study use Portable X fluorescent spectrometry to the lead in soil
Detection, it is only necessary to soil is carried out field investigation and sampling, quickly prepares, precisely test, early stage preparation method is simple, and uses X-fluorescence light
Spectrometry can carry out a keyization operation, it is not necessary to professional training can complete, simple to operate.
Summary of the invention
In view of this, need to overcome at least one in drawbacks described above of the prior art.
The invention provides a kind of X fluorescence spectrum method rapid assay methods to heavy metals in soil lead, including: 1)
Take a certain amount of soil powder；
2) described soil powder loaded specimen cup and is compacted with Manual tablet pressing machine, forming testing sample；
3) being put into by testing sample in sample test box, this testing cassete includes:
Shell, described shell upper end has hole, is provided with shell fragment in hole；
Sample stage, described sample stage is arranged on the bottom of described enclosure；
Hand-held set, there is N number of groove described hand-held set front end, and described hand-held set is by groove and the cooperation of described shell fragment and described sample
Product testing cassete couples；
4) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of testing sample；And
5) X-fluorescence intensity based on described testing sample, the lead element content being calculated in this soil.
Use is dried, grinds, is crossed a series of pre-treatments such as mesh sieve, and these pre-treatments one can make powder sample granule to be measured
Evenly, two can make the powder sample of certain granules size be left out, and generally, are that size is specific more than certain
The powder particle of size forecloses, to ensure regularity and the repeatability of the lead element test in powder sample, it practice,
Large effect is there is in the size of granule to test result accuracy；After crossing mesh sieve, powder is sufficiently mixed, it is ensured that
Sample homogeneity；Ensure the granularity of sample simultaneously, reduce grain dispersion and the impact of mineral effect of X-fluorescence test.
Meanwhile, the assay method of embodiments of the invention has the further advantage that sample treatment is simple, only uses letter
Either simplex tool carries out early stage to sample to be prepared, and sample pre-treatments only needs 2min；Instrument test is simple, and a key operates
With, and without any waste consumable, instrument possesses sample test box, it is ensured that test safe and reliable.
It addition, according to the X fluorescence spectrum method disclosed by the invention rapid assay methods to heavy metals in soil lead, also
There is following additional technical feature:
According to some embodiments of the present invention, in described step 4), it is calculated the lead in this soil by following formula (1)
Constituent content,
C=bI+a (1)
Lead element weight/mass percentage composition during wherein C represents soil, I represents the X-fluorescence intensity of testing sample, b and a is fixing ginseng
Number.
Utilizing the test philosophy of X fluorescence spectrometer, the content of lead is directly proportional to the X-fluorescence intensity obtained after the lead excited,
Thus, according to obtained X-fluorescence intensity, can be in the hope of the lead content in this soil.
According to some embodiments of the present invention, described preset parameter b and a is to obtain by the following method:
4-1) by the soil powder of known for a series of difference lead content, obtain the standard sample of different known lead content, by it
Load specimen cup and be compacted with Manual tablet pressing machine；
4-2) measure the X-fluorescence intensity of the standard sample of different known lead content respectively, and be based respectively on each lead content and its phase
Corresponding X-fluorescence intensity demarcates standard curve；
4-3) by following equation of linear regression, obtain preset parameter b and a,
Wherein, with represent the average quality percentage composition of standard sample of the most known lead content and average X-fluorescence intensity respectively.
It should be noted that the value of b and a is referred to the preset parameter of instrument, it is also possible to by the soil of standard lead content
Earth is by asking for standard curve, and is tried to achieve by equation of linear regression.
According to some embodiments of the present invention, in step 2) in described soil powder in preferred described loading specimen cup
Weight accounts for less than the 1/10 of the weight of the soil powder obtained by step 1).
Prepare a large amount of powder and take wherein certain proportion part and detect, the repeatable of test can be better ensured that
Property and precision.
According to some embodiments of the present invention, the weight of soil powder obtained in described step 1) is 100 grams.
According to some embodiments of the present invention, step 4-1) in, the quantity of described standard sample is more than or equal to 4.
According to some embodiments of the present invention, described hand-held set also includes: X-fluorescence emitter, the internal peace of described hand-held set
Equipped with described X-fluorescence emitter.
According to some embodiments of the present invention, described sample detection box also includes: handle plate, and described handle plate is arranged on institute
State the side of sample detection box, and be connected with described shell fragment by elastomeric element.
During detection sample, the front end of described hand-held set is put into the hole of described detection box upper end, pulls described handle plate, institute
State in the groove that shell fragment inserts described hand-held set, make described hand-held set and described sample detection box compact siro spinning technology, prevent radiation from letting out
Leakage；
After sample detection completes, pulling described handle plate, described shell fragment ejects the groove of described hand-held set, takes out described hand-held set
?.
According to some embodiments of the present invention, pressure during described Manual tablet pressing machine tabletting: between 20MPa-22 MPa.
According to some embodiments of the present invention, the number of recesses on described hand-held set is: N is more than or equal to 2, and relatively sets
Put.
Being provided with Pressure gauge on Manual tablet pressing machine, it is possible to grasp the size of pressure accurately, test sample is treated in the compacting of the present invention
The pressure of product is: between 20MPa-22 MPa, and the sample homogeneity that this pressure limit suppresses out is good, suitably eliminates granule
Degree effect and the impact of mineral effect, assist tabletting with boric acid during compacting sample simultaneously.
Use described Manual tablet pressing machine and described portable example testing cassete can carry out the most at the scene sample making and
Sample detection, substantially increases efficiency and the precision of sample detection；Described portable example detection box is directly pacified by shell fragment
It is contained on sample room, sample can be placed before sample room, wherein also have the thickest stereotype, be possible to prevent radiation leakage, this company
The convenient plug of the mode that connects, gap is little, and simple in construction is easy to operate, high safety.
Aspect and advantage that the present invention adds will part be given in the following description, and part will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage will become from the following description of the accompanying drawings of embodiments
Substantially with easy to understand, wherein:
The flow chart of Fig. 1 present invention；
Fig. 2 is the schematic diagram of the portable example detection box of the present invention；
In figure, 1 is hand-held set, and 2 is handle plate, and 3 is shell.
Detailed description of the invention
The embodiments described below is exemplary, is only used for explaining the present invention, and can not be construed to the limit to the present invention
System.
The X fluorescence spectrum method quick mensuration to heavy metals in soil lead of the present invention is described below with reference to accompanying drawings
Method, wherein Fig. 1 is the flow chart of the present invention.
According to embodiments of the invention, as it is shown in figure 1, the invention provides a kind of X fluorescence spectrum method to a huge sum of money in soil
Belong to the rapid assay methods of Element Lead, including:
1) a certain amount of soil powder is taken；
2) described soil powder loaded specimen cup and is compacted with Manual tablet pressing machine, forming testing sample；
3) being put into by testing sample in sample test box, this testing cassete includes:
Shell 3, described shell 3 upper end has hole, is provided with shell fragment in hole；
Sample stage, described sample stage is arranged on the bottom within described shell 3；
Hand-held set 1, there is N number of groove described hand-held set 1 front end, and described hand-held set 1 is by groove and the cooperation of described shell fragment and institute
State sample test box to couple；
4) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of testing sample；And
5) X-fluorescence intensity based on described testing sample, the lead element content being calculated in this soil.
When fetching earth earth powder, soil is carried out drying, grind, cross a series of pre-treatments such as mesh sieve, choose as far as possible
Grain sample little, uniform, it is ensured that sample homogeneity；Ensure the granularity of sample simultaneously, reduce the grain dispersion of X-fluorescence test
And the impact of mineral effect, it is also possible to ensure the high precision of test.
Using drying, grind, cross the pre-treatments one such as mesh sieve and can make powder sample granule to be measured evenly, two can make one
The powder sample determining granular size is left out, and generally, is size to be arranged more than the powder particle of certain specific dimensions
Except outside, to ensure regularity and the repeatability of the lead element test in powder sample, it practice, the size of granule is to test
There is large effect in result accuracy；After crossing mesh sieve, powder is sufficiently mixed, it is ensured that sample homogeneity；Simultaneously
Ensure the granularity of sample, reduce grain dispersion and the impact of mineral effect of X-fluorescence test.
Meanwhile, the assay method of embodiments of the invention has the further advantage that sample treatment is simple, only uses letter
Either simplex tool carries out early stage to sample to be prepared, and sample pre-treatments only needs 2min；Instrument test is simple, and a key operates
With, and without any waste consumable, instrument possesses sample test box, it is ensured that test safe and reliable.
According in embodiments of the invention, step one, measuring formula is:
C=bI+a；
Wherein C represents testing sample content, and I represents the X-fluorescence intensity of testing sample；
Wherein equation of linear regression is:
According to embodiments of the invention, described preset parameter b and a is to obtain by the following method:
4-1) by the soil powder of known for a series of difference lead content, obtain the standard sample of different known lead content, by it
Load specimen cup and be compacted with Manual tablet pressing machine；
4-2) measure the X-fluorescence intensity of the standard sample of different known lead content respectively, and be based respectively on each lead content and its phase
Corresponding X-fluorescence intensity demarcates standard curve；
4-3) by following equation of linear regression, obtain preset parameter b and a,
Wherein, with represent the average quality percentage composition of standard sample of the most known lead content and average X-fluorescence intensity respectively.
It should be noted that the value of b and a is referred to the preset parameter of instrument, it is also possible to by the soil of standard lead content
Earth is by asking for standard curve, and is tried to achieve by equation of linear regression.
Preferably, in step 4-1) in sample adds a certain proportion of nickel element, that removes between adjacent element is dry
Disturb, the double and interference at peak and the interference etc. of escape peak, go out to affect the influence value of element, at test process by coefficient calculations
In this influence value is subtracted out.
According to some embodiments of the present invention, in step 2, the powder dose in described loading specimen cup with described quantitatively
The ratio of soil is 1/10.
Alternatively, described quantitative soil is 100 grams.
Alternatively, the powder dose in described loading specimen cup is 10 grams.
According in some embodiments of the present invention, step one, the quantity of described standard sample is more than or equal to 4.
Also include according to hand-held set described in some embodiments of the present invention 1: X-fluorescence emitter, the internal peace of described hand-held set 1
Equipped with described X-fluorescence emitter.
According to some embodiments of the present invention, described sample detection box also includes: handle plate 2, and described handle plate 2 is arranged on
The side of described sample detection box, and be connected with described shell fragment by elastomeric element.
During detection sample, the front end of described hand-held set 1 is put into the hole of described detection box upper end, pulls described handle plate 2,
Described shell fragment inserts in the groove of described hand-held set 1, makes described hand-held set 1 and described sample detection box compact siro spinning technology, prevents spoke
Penetrate leakage；
After sample detection completes, pulling described handle plate 2, described shell fragment ejects the groove of described hand-held set 1, takes out described hand-held
Machine 1.
According to some embodiments of the present invention, pressure during described Manual tablet pressing machine tabletting: between 20MPa-22 MPa.
According to some embodiments of the present invention, the number of recesses on described hand-held set 1 is: N is more than or equal to 2, and relatively sets
Put.
Being provided with Pressure gauge on Manual tablet pressing machine, it is possible to grasp the size of pressure accurately, test sample is treated in the compacting of the present invention
The pressure of product is: between 20MPa-22 MPa, and the sample homogeneity that this pressure limit suppresses out is good, suitably eliminates granule
Degree effect and the impact of mineral effect, assist tabletting with boric acid during compacting sample simultaneously.
Use described Manual tablet pressing machine and described portable example testing cassete can carry out the most at the scene sample making and
Sample detection, substantially increases efficiency and the precision of sample detection；Described portable example detection box is directly pacified by shell fragment
Being contained on sample room, the convenient plug of this connected mode, gap is little, in case radiation leakage, simple in construction, easy to operate, safety
Property is strong.
According to some embodiments of the present invention, the test shooting condition of curve is: excite pipe pressure 20-50KV (kilovolt), swashs
Send out pipe flow 50-100 μ A(microampere), optical filter: molybdenum titanium superimposed sheets (molybdenum sheet thickness 0.05-0.15 millimeter, titanium sheet thickness 0.1-0.5
Millimeter), lead element detected energy level: 10-15 KeV.
Preferably, the test shooting condition of curve is: excites pipe pressure 30-40KV (kilovolt), excites pipe flow 70-90 μ A(micro-
Peace), optical filter: molybdenum titanium superimposed sheets (molybdenum sheet thickness 0.08-0.12 millimeter, titanium sheet thickness 0.2-0.4 millimeter), lead element detection energy
Level: 11-13 KeV.
Below, reference example, describe the method for testing of the present invention in detail.
According to one embodiment of present invention, in the case of full background, weigh the soil powder of a series of known lead content
End sample (crossing 40 mesh sieves) about 10g, loads specimen cup, and uses Manual tablet pressing machine to be compacted by pedotheque, to get standard samples；
Measure the X fluorescence spectrum of above-mentioned standard sample, obtain the X-fluorescence intensity of known content standard sample, and according to concentration and its
Corresponding X-fluorescence intensity makes standard curve；
According to standard curve, by following equation of linear regression, obtain preset parameter b and a,
Wherein, with represent the average quality percentage composition of standard sample of the most known lead content and average X-fluorescence intensity respectively.
Take 100g pedotheque, dry, grind, cross mesh sieve；
Weighing 10g soil powder sample, load specimen cup, and use Manual tablet pressing machine to be compacted by sample, it is glimmering that preparation becomes applicable X
The powder sample to be measured of optical tests；
Testing sample is put into portable example testing cassete detect；
Measure the X fluorescence spectrum of powder sample to be measured, obtain its X-fluorescence intensity, and be calculated this soil by following formula (1)
Lead element content in earth,
C=bI+a (1)
Lead element weight/mass percentage composition during wherein C represents soil, I represents the X-fluorescence intensity of testing sample, b and a is fixing ginseng
Number.
Although the multiple illustrative examples with reference to the present invention have carried out detailed retouching to the detailed description of the invention of the present invention
State, it must be understood that those skilled in the art can be designed that multiple other improvement and embodiment, these improve and implement
Example will fall within spirit and scope.Specifically, in the scope of aforementioned disclosure, accompanying drawing and claim
Within, rational modification and improvement can be made in terms of the layout of parts and/or sub-combination layout, without departing from
The spirit of the present invention.Except the modification in terms of parts and/or layout and improvement, its scope is by claims and equivalent thereof
Thing limits.
Claims (10)
1. the X fluorescence spectrum method rapid assay methods to heavy metals in soil lead, it is characterised in that including:
1) a certain amount of soil powder is taken；
2) described soil powder loaded specimen cup and is compacted with Manual tablet pressing machine, forming testing sample；
3) being put into by testing sample in sample test box, this testing cassete includes:
Shell, described shell upper end has hole, is provided with shell fragment in hole；
Sample stage, described sample stage is arranged on the bottom of described enclosure；
Hand-held set, there is N number of groove described hand-held set front end, and described hand-held set is by groove and the cooperation of described shell fragment and described sample
Product testing cassete couples；
4) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of testing sample；And
5) X-fluorescence intensity based on described testing sample, the lead element content being calculated in this soil.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, its feature
It is, in described step 5), the lead element content being calculated in this soil by following formula (1),
C=bI+a (1)
Lead element weight/mass percentage composition during wherein C represents soil, I represents the X-fluorescence intensity of testing sample, b and a is fixing ginseng
Number.
The X fluorescence spectrum method the most according to claim 2 rapid assay methods to heavy metals in soil lead, its feature
Being, described preset parameter b and a is to obtain by the following method:
4-1) by the soil powder of known for a series of difference lead content, obtain the standard sample of different known lead content, by it
Load specimen cup and be compacted with Manual tablet pressing machine；
4-2) measure the X-fluorescence intensity of the standard sample of different known lead content respectively, and be based respectively on each lead content and its phase
Corresponding X-fluorescence intensity demarcates standard curve；
4-3) by following equation of linear regression, obtain preset parameter b and a,
Wherein, with represent the average quality percentage composition of standard sample of the most known lead content and average X-fluorescence intensity respectively.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, its feature
Be, in step 2) described in load the weight of the described soil powder in specimen cup and account for the soil powder obtained by step 1)
Weight less than 1/10.
The X fluorescence spectrum method the most according to claim 4 rapid assay methods to heavy metals in soil lead, its feature
Being, the weight of soil powder obtained in described step 1) is 100 grams.
The X fluorescence spectrum method the most according to claim 3 rapid assay methods to heavy metals in soil lead, its feature
It is, step 4-1) in, the quantity of described standard sample is more than or equal to 4.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, it is special
Levying and be, described hand-held set also includes:
X-fluorescence emitter, described hand-held set is internally installed described X-fluorescence emitter.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, it is special
Levying and be, described sample detection box also includes:
Handle plate, described handle plate is arranged on the side of described sample detection box, and is connected with described shell fragment by elastomeric element.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, it is special
Levy and be, pressure during described Manual tablet pressing machine tabletting: between 20MPa-22 MPa.
The X fluorescence spectrum method the most according to claim 1 rapid assay methods to heavy metals in soil lead, it is special
Levying and be, the number of recesses on described hand-held set is: N is more than or equal to 2, and is oppositely arranged.
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| CN111272465A (en) * | 2020-04-20 | 2020-06-12 | 河海大学 | Portable normal position soil map collection equipment |
| CN112730493A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | On-site detection method for soil metal substances |
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| CN112730493A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | On-site detection method for soil metal substances |
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