CN104655664A - Method and device for in-situ detection of multiple elements and contents in water body - Google Patents
Method and device for in-situ detection of multiple elements and contents in water body Download PDFInfo
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- CN104655664A CN104655664A CN201510041417.7A CN201510041417A CN104655664A CN 104655664 A CN104655664 A CN 104655664A CN 201510041417 A CN201510041417 A CN 201510041417A CN 104655664 A CN104655664 A CN 104655664A
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Abstract
The invention discloses a method for in-situ detection of multiple elements and contents in water body. The method comprises the following steps: exciting a to-be-detected water body in a sample box by virtue of an exciting source in the center of a polyethylene coating; meanwhile, respectively collecting gamma ray and X fluorescence signal by virtue of a gamma ray detector and an X fluorescence detector; and amplifying the collected signal by virtue of a signal amplifier, then converting into an energy spectrum for analysis through multiple analyzers, and processing data by virtue of a computer so as to obtain the multiple elements and the contents in the water body. The invention also discloses a measuring device. According to the device and the method disclosed by the invention, two detectors can be respectively used for detecting instantaneous characteristic gamma ray and characteristic X fluorescence to detect the multiple elements, including low atomic number and high atomic number, in a water solution in a combined mode; and the device and the method are wide in detection range, high in detection precision and low in detection limit.
Description
Technical field
The present invention relates to Element detection analysis field in water body, be specifically related to the method and apparatus of a kind of in situ detection water body multielement composition and content.
Background technology
Water pollution is concerning people, and more so, its in situ detection is the problem that need solve in harm.Conventional detection method comprises X fluorescence spectrum, anodic stripping voltammetry, the determination method such as immunodetection and function DNA detection method of atomic absorption spectrography (AAS), atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry and Recent study.These methods need the operative technique personnel of sampling, sample preparation, strict Laboratory room and specialty, testing cost is relatively high, and be difficult to carry out real-time continuous detection, can not meet at burst mode tra nsmitter investigation and the needs in ecological risk investigation, therefore people are still continue to find can be faster, more accurately and carry out the detection means of field condition.
Send out gamma neutron active ray wink and analyze (Prompt Gamma Neutron Activation Analysis, PGNAA) technology have non-destructive, high sensitivity, not by sample shape and surrounding environment impact, can carry out to the environmental sample in large volume the feature that multielement original position detects in real time, be widely used in oil well logging, mineral prospecting, the detection of explosive composition, biology, the field such as archaeology and the analysis of environmental sample multielement definite value.The detection of PGNAA technology in position in water body is in recent years a focus, but due to the restriction of radioactive source activity in situ detection, effect is unsatisfactory.Though someone in conjunction with the X-fluorescence information of the internal conversion produced in PGNAA technology to improve the detectability of single heavy metal in water body, but its composition is not single during water body in-situ detects, and X-fluorescence technology is difficult to detect low-Z elements such as hydrogen, oxygen, nitrogen, how realizing in site measurement while multielement in water body is a large difficult point.Therefore, necessary the deficiency solving prior art is improved to prior art.
Summary of the invention
The object of the invention is to provide the method and apparatus of a kind of in situ detection water body multielement composition and content, to solve the deficiencies in the prior art.
The present invention is by the following technical solutions:
A method in situ detection water body multielement composition and content, comprises the steps:
The water body to be detected that step one, utilization are fixed in the excitaton source excited sample box at tygon integument center; Wherein, described excitaton source is isotope neutron source or neutron generator;
Step 2, utilize gamma ray detectors and X-fluorescence detector to collect gamma rays and the X-fluorescence signal of water body multielement respectively simultaneously;
Step 3, utilize signal amplifier to amplify the signal that gamma ray detectors and X-fluorescence detector are collected, be converted into the power spectrum that can be used for analysis afterwards through multichannel analyzer, then carry out data processing by computing machine, obtain water body multielement composition and content; Wherein, computing machine carries out the acquisition that data processing method comprises elemental characteristic peak and background count, and the power spectrum counting provided by multichannel analyzer by following formula is converted into each constituent content:
C
i＝AI
γi+D (1)
C
j＝BI
Xj+E (2)
Wherein, C
ifor element i concentration, wt%, element i are the element of atomic number≤20; C
jfor element j concentration, wt%, element j are the element of atomic number >20; I
γ i, I
xjthe relative intensity of element i feature gamma rays and element j feature X-fluorescence respectively; A, B, D, E are undetermined coefficient, demarcated obtain by device element.
Tygon integument described in step one is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm; The thickness of described sample box is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm; Described tygon integument is positioned at 1-5cm immediately below sample box.
The neutron flux of isotope neutron source described in step one and neutron generator is 1 × 10
6n/cm
2above; Described isotope neutron source comprises 252Cf; Described neutron generator comprises DD neutron generator or DT neutron generator.
Gamma ray detectors described in step 2 comprises crystal counter or semiconductor detector, described crystal counter comprises Nal detector, bismuth germanate detector or cesium iodide detector, and described semiconductor detector comprises P type high purity germanium detector, N-type high purity germanium detector or tellurium-zinc-cadmium detector; Low pressure and the high pressure of described gamma ray detectors provide by power supply, and low pressure is 12-24V, and high pressure is 500-2000V.
Described in step 2, X-fluorescence detector comprises crystal counter, semiconductor detector or gas detector, described crystal counter comprises the Nal detector of band beryllium window, described semiconductor detector comprises silicon PIN detector, silicon drifting detector or Cd Te probe, and described gas detector comprises proportional counter tube; Low pressure and the high pressure of described X-fluorescence detector provide by power supply, and low pressure is 12-24V, and high pressure is 500-3000V.
Gamma ray detectors described in step 2 and X-fluorescence detector lay respectively at directly over sample box, carry out collection signal.
The device of a kind of in situ detection water body multielement composition and content, comprise excitaton source, tygon integument, sample box, gamma ray detectors, X-fluorescence detector, power supply one, power supply two, signal amplifier, multichannel analyzer, described excitaton source is isotope neutron source or neutron generator, is fixed on the center of tygon integument; Described tygon integument is positioned at certain distance immediately below sample box; Place gamma ray detectors and X-fluorescence detector directly over described sample box respectively, power supply one and power supply two are connected gamma ray detectors and X-fluorescence detector respectively; The output terminal of gamma ray detectors is connected with the input end of signal amplifier respectively with the output terminal of X-fluorescence detector, and the output terminal of signal amplifier is connected with the input end of multichannel analyzer, and the output terminal of multichannel analyzer is connected with outer source machine.
Described tygon integument is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm; The thickness of described sample box is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm; Described tygon integument is positioned at 1-5cm immediately below sample box.
The neutron flux of described isotope neutron source and neutron generator is 1 × 10
6n/cm
2above; Described isotope neutron source comprises 252Cf; Described neutron generator comprises DD neutron generator or DT neutron generator.
Described gamma ray detectors comprises crystal counter or semiconductor detector, described crystal counter comprises Nal detector, bismuth germanate detector or cesium iodide detector, and described semiconductor detector comprises P type high purity germanium detector, N-type high purity germanium detector or tellurium-zinc-cadmium detector; Described X-fluorescence detector comprises crystal counter, semiconductor detector or gas detector, described crystal counter comprises the Nal detector of band beryllium window, described semiconductor detector comprises silicon PIN detector, silicon drifting detector or Cd Te probe, and described gas detector comprises proportional counter tube.
The principle of the invention: the feature gamma that the present invention utilizes the element such as neutron and O, C generation inelastic scattering and the element such as neutron and H generation capture reaction to produce, these feature gammas are collected by gamma ray detectors, through multichannel analyzer, signal is converted into the power spectrum that can be used for analyzing again, finally carries out by computing machine elemental composition and the content that data processing obtains the low atomic numbers (≤20) such as water body O, C, H; Next internal conversion X-fluorescence utilizing neutron and element reaction to produce and secondary gamma rays excite the X-fluorescence information of high atomic number in water body (>20) element, the X-fluorescence information of water body high atomic number element is collected by X-fluorescence detector, through multichannel analyzer, signal is converted into the power spectrum that can be used for analyzing again, finally carries out by computing machine composition and the content that data processing obtains water body high atomic number (>20) element.
Beneficial effect of the present invention:
1, the inventive method utilizes simultaneously and sends out gamma rays INAA (PGNAA) and x-ray fluorescence analysis technology (XRF) wink, use double detector to detect respectively and send out Characteristic γ ray and feature X-fluorescence wink, multielement in joint-detection aqueous solution, comprise the element of low atomic number and high atomic number, sensing range is wide, accuracy of detection is high, and detectability is low.And simple to operate, without chemical contamination, Measuring Time is short, safe and reliable, composition and the content detection of multielement in water body can be realized, there is wide application prospect.
2, the inventive method utilizes the gamma-rays produced in PGNAA to excite the feature X-fluorescence information of element, replaces traditional excitaton source (X-ray tube, high energy electron or radioactive source etc.), simple and fast and reducing costs.
3, sample itself directly degraded neutron in the inventive method, improves neutron utilization factor.
Accompanying drawing explanation
Figure l is apparatus of the present invention schematic diagram.
Fig. 2 is gamma-ray spectrometry figure in embodiment 1.
Fig. 3 is X-fluorescence energy spectrogram in embodiment 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
A method in situ detection water body multielement composition and content, comprises the steps:
Step one, utilize the water body to be detected that is fixed in the excitaton source excited sample box at tygon integument center, neutron reacts with element in water body and releases gamma (γ) ray, while gamma-rays can inspire the X-fluorescence information of element.Tygon integument is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm.Excitaton source is isotope neutron source or neutron generator, and neutron flux is 1 × 10
6n/cm
2above; Isotope neutron source comprises 252Cf; Neutron generator comprises DD neutron generator or DT neutron generator.The thickness of sample box is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm.Tygon integument is positioned at 1-5cm immediately below sample box.
The gamma ray detectors that step 2, simultaneously utilization are positioned at directly over sample box and X-fluorescence detector collect gamma rays and the X-fluorescence signal of water body multielement respectively, and these signals are referred to as " core fingerprint ", can carry out qualitative or quantitative test.Gamma ray detectors comprises crystal counter or semiconductor detector, crystal counter comprises Nal detector, bismuth germanate detector or cesium iodide detector, and semiconductor detector comprises P type high purity germanium detector, N-type high purity germanium detector or tellurium-zinc-cadmium detector.Low pressure and the high pressure of gamma ray detectors provide by power supply, and low pressure is 12-24V, and high pressure is 500-2000V.X-fluorescence detector comprises crystal counter, semiconductor detector or gas detector, described crystal counter comprises the Nal detector of band beryllium window, described semiconductor detector comprises silicon PIN detector, silicon drifting detector or Cd Te probe, and described gas detector comprises proportional counter tube.Low pressure and the high pressure of described X-fluorescence detector provide by power supply, and low pressure is 12-24V, and high pressure is 500-3000V.
Step 3, utilize signal amplifier to amplify the signal that gamma ray detectors and X-fluorescence detector are collected, be converted into the power spectrum that can be used for analysis afterwards through multichannel analyzer, then carry out data processing by computing machine, obtain water body multielement composition and content; Wherein, computing machine carries out the acquisition that data processing method comprises elemental characteristic peak and background count, and the power spectrum counting provided by multichannel analyzer by following formula is converted into each constituent content:
C
i＝AI
γi+D (1)
C
j＝BI
Xj+E (2)
Wherein, C
ifor element i concentration, wt%, element i are the element of atomic number≤20; C
jfor element j concentration, wt%, element j are the element of atomic number >20; I
γ i, I
xjthe relative intensity of element i feature gamma rays and element j feature X-fluorescence respectively; A, B, D, E are undetermined coefficient, demarcated obtain by device element.
The device of a kind of in situ detection water body multielement composition and content, as shown in Figure 1, excitaton source 1, tygon integument 2, sample box 8, gamma ray detectors 3, X-fluorescence detector 2, power supply 1, power supply 2 10, signal amplifier 5, multichannel analyzer 6 is comprised.Tygon integument 2 is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm.Excitaton source 1 is isotope neutron source or neutron generator, is fixed on the center of tygon integument 2.The thickness of sample box 8 is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm.Tygon integument 2 is positioned at 1-5cm immediately below sample box 8.Place gamma ray detectors 3 and X-fluorescence detector 2 directly over sample box 8 respectively, power supply 1 and power supply 2 10 are connected gamma ray detectors 3 and X-fluorescence detector 2 respectively.The output terminal of gamma ray detectors 3 is connected with the input end of signal amplifier 5 respectively with the output terminal of X-fluorescence detector 2, and the output terminal of signal amplifier 5 is connected with the input end of multichannel analyzer 6, and the output terminal of multichannel analyzer 6 is connected with outer source machine 7.
The lasing light emitter that following examples relate to is 252Cf neutron source, is fixed on tygon integument center; Tygon integument thickness is 1cm, diameter 11cm, long 50cm; The thick 0.8cm of sample box, long 50cm, wide 50cm, height 50cm; Tygon integument is positioned at 1cm immediately below sample box.Described gamma ray detectors is 4 × 4 inches of bismuth germanium oxide (BGO) detectors that Saint Gobain company produces, low pressure 24V, high pressure 700V; Described X-fluorescence detector is the Nal detector of band beryllium window, low pressure 24V, high pressure 750V; Described multichannel analyzer is the DigiBase multichannel analyzer of ORTEC company.
Embodiment 1
1, utilize the mercuric acetate solution sample be fixed in the excitaton source excited sample box at tygon integument center, mercury element concentration is the mercuric acetate solution of 0wt%, 0.1wt%, 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%.
2, utilize gamma ray detectors and X-fluorescence detector to collect gamma rays and the X-fluorescence signal of water body multielement respectively, often kind of sample measures 3600s respectively simultaneously.
3, signal amplifier is utilized to amplify the signal that gamma ray detectors and X-fluorescence detector are collected, the power spectrum that can be used for analyzing is converted into afterwards through multichannel analyzer, obtain gamma-ray spectrometry figure (Fig. 2) and X-fluorescence energy spectrogram (Fig. 3) respectively, carry out data processing by computing machine again, obtain water body multielement composition and content.Computing machine carries out the acquisition that data processing method comprises elemental characteristic peak and background count, and the power spectrum counting provided by multichannel analyzer by following formula is converted into each constituent content:
C
i＝AI
γi+D (1)
C
j＝BI
Xj+E (2)
Wherein, C
ifor element i concentration, wt%, element i are the element of atomic number≤20; C
jfor element j concentration, wt%, element j are the element of atomic number >20; I
γ i, I
xjthe relative intensity of element i feature gamma rays and element j feature X-fluorescence respectively; A, B, D, E are undetermined coefficient, and demarcated by device element and obtain, each undetermined coefficient of the present embodiment is as shown in the table:
From R
2(linearly dependent coefficient) all closely 1, illustrates that correlativity is fine.
Claims (10)
1. a method in situ detection water body multielement composition and content, is characterized in that, comprises the steps:
The water body to be detected that step one, utilization are fixed in the excitaton source excited sample box at tygon integument center; Wherein, described excitaton source is isotope neutron source or neutron generator;
Step 2, utilize gamma ray detectors and X-fluorescence detector to collect gamma rays and the X-fluorescence signal of water body multielement respectively simultaneously;
Step 3, utilize signal amplifier to amplify the signal that gamma ray detectors and X-fluorescence detector are collected, be converted into the power spectrum that can be used for analysis afterwards through multichannel analyzer, then carry out data processing by computing machine, obtain water body multielement composition and content; Wherein, computing machine carries out the acquisition that data processing method comprises elemental characteristic peak and background count, and the power spectrum counting provided by multichannel analyzer by following formula is converted into each constituent content:
C
i＝AI
γi+D (1)
C
j＝BI
Xj+E (2)
Wherein, C
ifor element i concentration, wt%, element i are the element of atomic number≤20; C
jfor element j concentration, wt%, element j are the element of atomic number >20; I
γ i, I
xjthe relative intensity of element i feature gamma rays and element j feature X-fluorescence respectively; A, B, D, E are undetermined coefficient, demarcated obtain by device element.
2. the method for in situ detection water body multielement composition according to claim 1 and content, is characterized in that, tygon integument described in step one is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm; The thickness of described sample box is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm; Described tygon integument is positioned at 1-5cm immediately below sample box.
3. the method for in situ detection water body multielement composition according to claim 1 and content, it is characterized in that, the neutron flux of isotope neutron source described in step one and neutron generator is 1 × 10
6n/cm
2above; Described isotope neutron source comprises 252Cf; Described neutron generator comprises DD neutron generator or DT neutron generator.
4. the method for in situ detection water body multielement composition according to claim 1 and content, it is characterized in that, gamma ray detectors described in step 2 comprises crystal counter or semiconductor detector, described crystal counter comprises Nal detector, bismuth germanate detector or cesium iodide detector, and described semiconductor detector comprises P type high purity germanium detector, N-type high purity germanium detector or tellurium-zinc-cadmium detector; Low pressure and the high pressure of described gamma ray detectors provide by power supply, and low pressure is 12-24V, and high pressure is 500-2000V.
5. the method for in situ detection water body multielement composition according to claim 1 and content, it is characterized in that, described in step 2, X-fluorescence detector comprises crystal counter, semiconductor detector or gas detector, described crystal counter comprises the Nal detector of band beryllium window, described semiconductor detector comprises silicon PIN detector, silicon drifting detector or Cd Te probe, and described gas detector comprises proportional counter tube; Low pressure and the high pressure of described X-fluorescence detector provide by power supply, and low pressure is 12-24V, and high pressure is 500-3000V.
6. the method for in situ detection water body multielement composition according to claim 1 and content, is characterized in that, gamma ray detectors described in step 2 and X-fluorescence detector lay respectively at directly over sample box, carry out collection signal.
7. the device of an in situ detection water body multielement composition and content, it is characterized in that, comprise excitaton source, tygon integument, sample box, gamma ray detectors, X-fluorescence detector, power supply one, power supply two, signal amplifier, multichannel analyzer, described excitaton source is isotope neutron source or neutron generator, is fixed on the center of tygon integument; Described tygon integument is positioned at certain distance immediately below sample box; Place gamma ray detectors and X-fluorescence detector directly over described sample box respectively, power supply one and power supply two are connected gamma ray detectors and X-fluorescence detector respectively; The output terminal of gamma ray detectors is connected with the input end of signal amplifier respectively with the output terminal of X-fluorescence detector, and the output terminal of signal amplifier is connected with the input end of multichannel analyzer, and the output terminal of multichannel analyzer is connected with outer source machine.
8. the device of in situ detection water body multielement composition according to claim 7 and content, is characterized in that, described tygon integument is cylinder barrel, and thickness is 1-2cm, and diameter is 10-14cm; The thickness of described sample box is 0.8-1.2cm, and long is 50-60cm, and wide is 50-60cm, and height is 45-55cm; Described tygon integument is positioned at 1-5cm immediately below sample box.
9. the device of in situ detection water body multielement composition according to claim 7 and content, it is characterized in that, the neutron flux of described isotope neutron source and neutron generator is 1 × 10
6n/cm
2above; Described isotope neutron source comprises 252Cf; Described neutron generator comprises DD neutron generator or DT neutron generator.
10. the device of in situ detection water body multielement composition according to claim 7 and content, it is characterized in that, described gamma ray detectors comprises crystal counter or semiconductor detector, described crystal counter comprises Nal detector, bismuth germanate detector or cesium iodide detector, and described semiconductor detector comprises P type high purity germanium detector, N-type high purity germanium detector or tellurium-zinc-cadmium detector; Described X-fluorescence detector comprises crystal counter, semiconductor detector or gas detector, described crystal counter comprises the Nal detector of band beryllium window, described semiconductor detector comprises silicon PIN detector, silicon drifting detector or Cd Te probe, and described gas detector comprises proportional counter tube.
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| CN110389145A (en) * | 2018-04-23 | 2019-10-29 | 中国科学院大连化学物理研究所 | A kind of method of inorganic cyanide content in detection solution |
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| CN107490591A (en) * | 2017-04-19 | 2017-12-19 | 安徽华脉科技发展有限公司 | A kind of heavy metal in soil content detection device |
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| CN112444532A (en) * | 2019-08-10 | 2021-03-05 | 丹东东方测控技术股份有限公司 | Method for measuring total iron content in sintered material on line |
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| CN111337990A (en) * | 2020-03-13 | 2020-06-26 | 兰州大学 | Metal mineral logging device and method based on pulse neutron source |
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Application publication date: 20150527 |