CN101776622B - Soil measuring method - Google Patents
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- CN101776622B CN101776622B CN2009101566330A CN200910156633A CN101776622B CN 101776622 B CN101776622 B CN 101776622B CN 2009101566330 A CN2009101566330 A CN 2009101566330A CN 200910156633 A CN200910156633 A CN 200910156633A CN 101776622 B CN101776622 B CN 101776622B
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- 239000002689 soil Substances 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004876 x-ray fluorescence Methods 0.000 claims abstract description 18
- 230000003595 spectral effect Effects 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000000691 measurement method Methods 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 8
- 238000013528 artificial neural network Methods 0.000 claims description 7
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 238000013507 mapping Methods 0.000 claims description 4
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 8
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- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000011005 laboratory method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
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Abstract
The invention relates to a soil measuring method, comprising the following steps that: a. an XRF soil analyzer is utilized to measure a soil standard sample and establish and store the following relation, i.e. the relation of the concentration C of the element to be measured and characteristic curve fluorescence intensity IFe of Fe element, and characteristic curve fluorescence intensity I of the element to be measured; b. an X ray emitted by a light source irradiates on the soil to be measured; c. a detector receives the X-ray fluorescence emitted by the soil to be measured, and obtaining spectral data of the soil to be measured; and d. a processing unit analyzes the characteristic curve fluorescence intensity IFe of the Fe element, and characteristic curve fluorescence intensity I of the element to be measured in the spectral data, and utilizing the relation to obtain the concentration C of the element to be measured with elimination of the influence of soil moisture. The soil measuring method has the advantages of simple and fast operation, high measuring accuracy, wide application range and the like.
Description
Technical Field
The invention relates to soil detection, in particular to a method for measuring elements in soil.
Background
In recent years, due to the rapid increase of population and the rapid development of industry, solid wastes are continuously stacked and dumped on the surface of soil, harmful wastewater continuously permeates into the soil, and harmful gas and floating dust in the atmosphere continuously fall into the soil along with rainwater, so that the heavy metal pollution of the soil is caused seriously. The heavy metal pollution of the soil directly affects the structure and the function of a soil ecosystem, and finally poses threats to ecological safety and the health of people. In recent years, due to increasing heavy metal pollution events caused by industrial development, the production and life of local residents are greatly influenced, and thus the evaluation and detection of some key areas are urgently needed.
The X-ray fluorescence (XRF) technology is used as a nondestructive multi-element analysis technology, is simple and quick to operate, and is widely applied to measurement of soil elements.
However, when the soil element is measured by using an X-ray fluorescence instrument, the humidity has a remarkable influence on the measurement, and the influence on the characteristic X-ray and scattering of the target element is larger when the humidity is larger. For example, the concentration of Pb in a dry soil sample is 600ppm, and when the soil sample is wetted and the humidity is 30%, the concentration of Pb measured by an X-ray fluorescence instrument is 400ppm, and the relative error exceeds 33%.
If the measurement error is to be reduced, the humidity of the measured concentration of the element to be measured needs to be corrected when the soil element is measured.
At present, the common method is to carry out drying pretreatment on a soil sample, and specifically comprises the following steps: baking a soil sample to be detected to be in a dry state at a constant temperature of 100-105 ℃, and then measuring the concentration of elements in the sample to be detected by using an X-ray fluorescence instrument. The existing method has some defects:
1. baking the soil to a dry state requires equipment such as an oven, which complicates the soil measuring device and increases the cost. This approach is not feasible for portable soil analyzers.
2. The drying process is time-consuming and inefficient.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the soil measuring method which is high in measuring accuracy and easy to operate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a soil measuring method comprising the steps of:
a. soil standards are measured by an XRF soil analyzer, and the following relations are established and stored:
the concentration C of the element to be detected and the characteristic line fluorescence intensity I of the Fe elementFeCharacteristic line of element to be measuredRelationship of fluorescence intensity I:
b. irradiating the soil to be detected by X rays emitted by the light source;
c. the detector receives X-ray fluorescence emitted by soil to be detected to obtain spectral data of the soil to be detected;
d. the processing unit analyzes the characteristic line fluorescence intensity I of the Fe element in the spectrum dataFeAnd the fluorescence intensity I of the characteristic line of the element to be detected, and using the relationship
Thereby obtaining the concentration C of the element to be measured without the influence of soil humidity.
Preferably, in the step a, the relationship is obtained in the following manner
：
Obtaining the scattering intensity I of the dry soilComCharacteristic line fluorescence intensity I of Fe elementFeThe relationship between: i isCom＝F(IFe)；
Obtaining the concentration C of the element to be detected and the fluorescence intensity I and the scattering intensity I of the characteristic line of the element to be detectedComThe relationship between: c ═ f (I, I)com)；
Storing the relationship: c ═ F (I, F (I)Fe))。
Preferably, in the step a, the characteristic line fluorescence intensity I of the C, Fe element concentration of the element to be detected of each group of dry soil standard samples is measuredFeObtaining the concentration C of the element to be detected in the soil and the characteristic line fluorescence intensity I of the Fe element by utilizing an artificial neural network algorithmFeAnd the mapping relation of the characteristic line fluorescence intensity I of the element to be detected is as follows:
further, the relationship
The method specifically comprises the following steps:
wherein M, N is a constant associated with the element to be tested, and A, B is a constant.
Further, the relation ICom＝F(IFe) Is ICom＝A+B·IFeWherein A, B is a constant.
Further, the relationship C ═ f (I, I)Com) Is composed of
Where M, N is a constant associated with the element to be measured.
The basic principle of the invention is as follows: when the XRF technology is used for detecting soil, X-rays generate strong scattering on the soil, and the scattering magnitude is related to a primary spectrum and a scattering matrix. Under the same primary spectrum, the more light elements are contained in the sample, the stronger the scattering. When the soil sample contains more moisture, the content of light elements in the sample is increased, and therefore, the more moisture of the soil is, the stronger the scattering is, as shown in fig. 3.
Theoretically, scattering is related to the light element content, and scattering is the additive effect of all light elements. Since the content of the Fe element in the soil is the highest, the Fe element is approximately considered to be removed, and the other elements are all light elements. The Fe element content can thus be approximated as a complement to the light element content. It follows that the content of Fe in the soil is related to the scattering intensity.
FIG. 1 is a graph of the relationship between Fe content and scattering intensity, which is established according to soil standards 07401-07408, and it can be known that there is a good linear correlation between Fe content and scattering intensity. FIG. 2 is a graph showing the relationship between the fluorescence intensity and the scattering intensity of the characteristic line of Fe element, and it is understood from this graph that the fluorescence intensity and the scattering intensity of the characteristic line of Fe element are also approximately linearly related. Therefore, by establishing the relationship between the characteristic line fluorescence intensity of the Fe element in the soil and the scattering intensity, it is feasible to obtain the scattering intensity by using the characteristic line fluorescence intensity of the Fe element in the soil.
Theoretically, the fluorescence intensity of the characteristic line of the elements in the soil should be influenced by humidity, and the influence is mainly reflected in the effects of enhancement of scattering background and dilution effect of moisture. For the characteristic line fluorescence intensity of Fe element, the influence of scattering can be reduced by adding primary filter. In addition, the dilution effect of the moisture can reduce the absorption of the characteristic line of the Fe element, but the influence is limited and can be ignored. Therefore, the characteristic line fluorescence intensity of Fe element is relatively less affected by humidity, as shown in fig. 4.
In summary, the characteristic line fluorescence intensity of the Fe element is obtained from the spectrum data of the soil to be measured, and is used as the characteristic line fluorescence intensity of the Fe element excluding the influence of the soil humidity, and the concentration of the element to be measured excluding the influence of the soil humidity is calculated according to the relationship between the concentration of the element to be measured and the characteristic line fluorescence intensity of the Fe element.
Compared with the prior art, the invention has the following beneficial effects:
1. simple and quick operation
According to the invention, an operator is not required to carry out drying pretreatment on the soil sample to be measured, devices such as a humidity sensor and the like are not required to be equipped during measurement, the concentration of the element to be measured for removing the soil humidity information can be directly given under the condition that the soil humidity is unknown, and the operation is simple, convenient and rapid. Can be widely applied to portable soil analyzers.
2. Improve the measurement accuracy
The invention eliminates the influence of humidity when measuring the concentration of soil elements. A large number of experimental results show that the method greatly improves the accuracy of the measurement of the soil elements.
3. Wide application range
The measurement method can be applied to the measurement of all types of soil elements, including contaminated or severely contaminated soil.
Drawings
FIG. 1 is a graph showing the relationship between Fe content and scattering intensity;
FIG. 2 is a graph showing the relationship between the fluorescence intensity and the scattering intensity of a characteristic line of Fe element;
FIG. 3 is a graph of humidity in soil versus scattering intensity;
FIG. 4 is a graph of characteristic line fluorescence intensity of Fe element in relation to humidity;
FIG. 5 is a schematic flow chart of the measurement method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In the following examples, the fluorescence intensity was obtained by the area method.
Example 1:
a method for measuring Sr element in soil, as shown in fig. 5, comprising the steps of:
a. measuring soil standard samples 07401-07408 by using an XRF soil analyzer, and establishing the characteristic line fluorescence intensity I of Fe element in dry soilFe(the selection interval is 6.20-6.61KeV) and the scattering intensity Icom(selection interval 20.00-21.50 KeV):
Icom＝F(IFe)＝A+B·IFe
wherein, A is 514.72, B is-0.12;
establishing the concentration C of the element SrSrCharacteristic line fluorescence intensity I with element SrSr(selected interval is 13.95-14.38KeV), the scattering intensity IcomThe relationship between:
wherein M isSr＝-12.78，NSr＝1056.82；
Storing the relationship into an XRF soil analyzer;
b. the X-ray emitted by the light source irradiates on a soil sample to be measured (for comparison, the real content of Sr element is 240ppm through a laboratory method);
c. the detector receives X-ray fluorescence emitted by a soil sample to be detected to obtain spectral data of the soil to be detected;
d. the processing unit obtains the following data according to the spectrum data of the soil to be detected: the characteristic line fluorescence intensity of Fe element is 893.0CPS (selection interval is 6.20-6.61KeV), and the characteristic line fluorescence intensity I of Sr elementSr89.9CPS (selection interval of 13.95-14.38KeV), and the characteristic line fluorescence intensity of the Fe element measured is taken as the characteristic line fluorescence intensity I of the Fe element excluding the influence of soil humidityFe＝893.0CPS；
The characteristic line fluorescence intensity I of the Fe elementFeSubstitution of 893.0CPS into a prestored relationship Icom＝A+B·IFeObtaining scattering intensity I excluding the influence of soil humiditycom＝407.6CPS；
Measuring the scattering intensity IcomCharacteristic line fluorescence intensity I of 407.6CPS and Sr elementsSrSubstituting 89.9CPS into a prestored relationshipObtaining the element Sr with the concentration of C in the soil excluding the influence of humiditySrSee table 1 for relevant data measured at 220.3 ppm;
when the Sr element content in other soil is measured, the steps b, c and d are repeated.
Table 1: comparison of this example with the prior art
As can be seen from the comparison in table 1, the accuracy of the present measurement method is greatly improved compared to the prior art.
Example 2:
a method for measuring Zr element in soil comprises the following steps:
a. measuring soil standard samples 07401-07408 by using an XRF soil analyzer to obtain the concentration C of the element Zr of each group of dry soil standard samplesZrCharacteristic line fluorescence intensity I of element ZrZr(the selection interval is 15.53-15.98KeV), characteristic line fluorescence intensity I of Fe elementFe(the selection interval is 6.20-6.61KeV), and the concentration C of the element Zr in the soil is obtained by utilizing an artificial neural network algorithmZrCharacteristic line fluorescence intensity I of Fe elementFeCharacteristic line fluorescence intensity I of element ZrZrThe specific way of the mapping relationship is as follows:
taking the three-layer forwarding network based on the error back-propagation algorithm as an example, the network is divided into three layers, namely an input layer IN (including I and I)Fe) Hidden layer y (containing J elements), and output layer O (i.e., concentration C); input IN by connecting weights wijAnd hidden layer unit yjAre connected, yj＝f(∑wijINi+w0) Then passes the weight mjIs connected with an output unit O, O ═ f (sigma m)jyj+m0) Thus, the mapping relationship between the input layer and the output layer is reconstructed by the connection weights, and the function f generally takes the following form: (u) ═ 1+ e-u)-1。
Characteristic line fluorescence intensity I of element Zr of dry soil standard sampleZrCharacteristic line fluorescence intensity of Fe element IFeAs input, the concentration C of the element ZrZrAs output, artificial neural network training is performed, and finally the system establishes CZrAnd IZr、IFeThe artificial neural network model of (1).
Storing the relationship into an XRF soil analyzer;
b. irradiating the soil sample to be detected with X-rays emitted by a light source (for comparison, the real content of Zr element in the soil sample is 300ppm by using a laboratory method);
c. the detector receives X-ray fluorescence emitted by a soil sample to be detected to obtain spectral data of the soil to be detected;
d. the processing unit obtains the following data according to the spectrum data of the soil to be detected: the characteristic line fluorescence intensity of Fe element is 1690.0CPS (selection interval is 6.20-6.61KeV), and the characteristic line fluorescence intensity I of Zr elementZr112.1CPS (selected interval 15.53-15.98KeV), and the characteristic line fluorescence intensity of Fe element measured was taken as the characteristic line fluorescence intensity I of Fe element excluding the influence of soil moistureFe＝1690.0CPS；
Will IZr＝112.1CPS、IFe1690.0CPS as input to neural network systemThe content C of Zr which is an element for eliminating humidity interference can be directly obtained by the artificial neural network model which is stored firstlyZr＝278.8ppm。
And when measuring the content of the Zr element in other soil, repeating the steps b, c and d.
Table 2: comparison of this example with the prior art
As can be seen from the comparison in table 2, the accuracy of the present measurement method is greatly improved compared to the prior art.
Example 3:
a method for measuring Pb element in soil, as shown in fig. 5, comprising the steps of:
a. measuring soil standard samples 07401-07408 by using an XRF soil analyzer, and establishing the characteristic line fluorescence intensity I of Fe element in dry soilFe(the selection interval is 6.20-6.61KeV) and the scattering intensity Icom(selection interval 20.00-21.50 KeV):
Icom＝F(IFe)＝A+B·IFe
wherein, A is 514.72, B is-0.12;
establishing the concentration C of the element Pb to be detectedPbCharacteristic line fluorescence intensity I with element PbPb(the selection interval is 12.42-12.81KeV), the scattering intensity IcomThe relationship between:
wherein,
storing the relationship into an XRF soil analyzer;
b. irradiating the soil sample to be detected with X-rays emitted by a light source (for comparison, the real content of Pb element measured by a laboratory method is 20 ppm);
c. the detector receives X-ray fluorescence emitted by a soil sample to be detected to obtain spectral data of the soil to be detected;
d. the processing unit obtains the following data according to the spectrum data of the soil to be detected: the characteristic line fluorescence intensity of Fe element is 1571.0CPS (selection interval is 6.20-6.61KeV), and the characteristic line fluorescence intensity of Pb element
(the selection interval is 12.42-12.81KeV), and the measured fluorescence intensity of the characteristic line of the Fe element is taken as the fluorescence intensity I of the characteristic line of the Fe element excluding the influence of soil humidityFe＝1571.0CPS；
The characteristic line fluorescence intensity I of the Fe elementFeSubstitution of 1571.0CPS into a prestored relationship Icom＝A+B·IFeObtaining scattering intensity I excluding the influence of soil humiditycom＝326.2CPS；
Measuring the scattering intensity Icom326.2CPS, characteristic line fluorescence intensity of element PbSubstituting into pre-stored relationshipsObtaining the element Pb with the concentration C which excludes the influence of humidity in the soilPnSee table 3 for data measured at 17.3 ppm;
when the content of Pb element in other soil is measured, repeating the steps b, c and d.
Table 3: comparison of this example with the prior art
As can be seen from the comparison in table 3, the accuracy of the present measurement method is greatly improved compared to the prior art.
The above embodiments should not be construed as limiting the scope of the invention. The key points of the invention are as follows: the influence of the moisture in the soil on the fluorescence intensity of the characteristic line of the Fe element is small and can be ignored, and on the basis, the relationship between the concentration of the element to be detected and the fluorescence intensity of the characteristic line of the Fe element is established in advance; in the soil measurement process, the obtained characteristic line fluorescence intensity of the element to be measured, the characteristic line fluorescence intensity of the Fe element and the relation are utilized, so that the concentration of the element to be measured, which is not influenced by soil humidity, is obtained. Any changes made to the invention without departing from the spirit thereof should fall within the scope of the invention.
Claims (6)
1. A soil measuring method comprising the steps of:
a. soil standards are measured by an XRF soil analyzer, and the following relations are established and stored:
the concentration C of the element to be detected and the characteristic line fluorescence intensity I of the Fe elementFeAnd the relation of the characteristic line fluorescence intensity I of the element to be detected:
b. irradiating the soil to be detected by X rays emitted by the light source;
c. the detector receives X-ray fluorescence emitted by soil to be detected to obtain spectral data of the soil to be detected;
d. the processing unit analyzes the characteristic line fluorescence intensity I of the Fe element in the spectrum dataFeAnd the fluorescence intensity I of the characteristic line of the element to be detected, and using the relationship Thereby obtaining the concentration C of the element to be measured without the influence of soil humidity.
2. The measurement method according to claim 1, characterized in that: in step a, the relationship is obtained in the following manner
Obtaining the scattering intensity I of the dry soilComCharacteristic line fluorescence intensity I of Fe elementFeThe relationship between: i isCom＝F(IFe)；
Obtaining the concentration C of the element to be detected and the fluorescence intensity I and the scattering intensity I of the characteristic line of the element to be detectedComThe relationship between: c ═ f (I, I)com)；
Storing the relationship: c ═ F (I, F (I)Fe))。
3. The measurement method according to claim 1, characterized in that: in the step a, the characteristic line fluorescence intensity I of the C, Fe element of the concentration of the element to be detected of each group of dry soil standard samples is measuredFeObtaining the concentration C of the element to be detected in the soil and the characteristic line fluorescence intensity I of the Fe element by utilizing an artificial neural network algorithmFeAnd the mapping relation of the characteristic line fluorescence intensity I of the element to be detected is as follows:
4. the measurement method according to claim 1, characterized in that: said relation The method specifically comprises the following steps: <math>
<mrow>
<mi>C</mi>
<mo>=</mo>
<mi>M</mi>
<mo>+</mo>
<mi>N</mi>
<mo>·</mo>
<mfrac>
<mi>I</mi>
<mrow>
<mi>A</mi>
<mo>+</mo>
<mi>B</mi>
<mo>·</mo>
<msub>
<mi>I</mi>
<mi>Fe</mi>
</msub>
</mrow>
</mfrac>
<mo>,</mo>
</mrow>
</math> wherein M, N is a constant associated with the element to be tested, and A, B is a constant.
5. The measurement method according to claim 2, characterized in that: said relation ICom＝F(IFe) Is ICom＝A+B·IFeWhereinAnd A, B is a constant.
6. The measurement method according to claim 2, characterized in that: the relationship C ═ f (I, I)Com) Is composed of <math>
<mrow>
<mi>C</mi>
<mo>=</mo>
<mi>M</mi>
<mo>+</mo>
<mi>N</mi>
<mo>·</mo>
<mfrac>
<mi>I</mi>
<msub>
<mi>I</mi>
<mi>Com</mi>
</msub>
</mfrac>
<mo>,</mo>
</mrow>
</math> Where M, N is a constant associated with the element to be measured.
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| CN104089968A (en) * | 2014-07-18 | 2014-10-08 | 上海化工研究院 | Device for detecting heavy metal in soil on site by rotary bucket type XRF (X-Ray Fluorescence) method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1601261A (en) * | 2003-09-28 | 2005-03-30 | 中国石油化工股份有限公司 | X-Ray Fluorescence Method for Analyzing Various Metal Components in Catalytic Cracking Catalyst |
| CN1947003A (en) * | 2004-04-28 | 2007-04-11 | 松下电器产业株式会社 | Fluorescent X-ray analysis method and fluorescent X-ray analysis device |
| WO2009134924A1 (en) * | 2008-04-30 | 2009-11-05 | Thermo Niton Analyzers Llc | In vivo measurement of trace elements in bone by x-ray fluorescence |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1601261A (en) * | 2003-09-28 | 2005-03-30 | 中国石油化工股份有限公司 | X-Ray Fluorescence Method for Analyzing Various Metal Components in Catalytic Cracking Catalyst |
| CN1947003A (en) * | 2004-04-28 | 2007-04-11 | 松下电器产业株式会社 | Fluorescent X-ray analysis method and fluorescent X-ray analysis device |
| WO2009134924A1 (en) * | 2008-04-30 | 2009-11-05 | Thermo Niton Analyzers Llc | In vivo measurement of trace elements in bone by x-ray fluorescence |
Non-Patent Citations (1)
| Title |
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| 越智宽友等.使用散射X射线的理论强度进行土壤\岩石中的微量元素的X射线荧光分析.<冶金标准化与质量>.2004,第42卷(第5期),第18-19页. * |
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