CN107589083B - Atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains and detection method - Google Patents
Atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains and detection method Download PDFInfo
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- CN107589083B CN107589083B CN201710691555.9A CN201710691555A CN107589083B CN 107589083 B CN107589083 B CN 107589083B CN 201710691555 A CN201710691555 A CN 201710691555A CN 107589083 B CN107589083 B CN 107589083B
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Abstract
An atomic absorption spectrometer and a detection method for simultaneously detecting lead and cadmium elements in grains. The spectrometer adopts a lead-cadmium composite hollow cathode lamp, a power supply and a control module, and is configured in a lead element high-performance lamp working state, a cadmium element common lamp working state and a copper element near wavelength background-deducting working state, so that the lead-cadmium element background-deducting measurement is realized at the same time; meanwhile, a double-atomization-region atomizer, a power supply and a control module are used, the double-atomization-region atomizer is configured in a sub-region time-sharing atomization mode, and calculation and selection of optimal sensitivity of the lead and cadmium single elements are realized by setting whether different regions are injected or not and adjusting the injection amount of the different regions; the method comprises a pretreatment method for simultaneously extracting lead and cadmium elements in grains and a sample introduction and data processing method for simultaneous measurement. The lead-cadmium composite hollow cathode lamp is different from a common multi-element lamp, improves light energy, widens linear range, improves sensitivity and detection limit, and is suitable for rapid large-flux simultaneous detection of lead and cadmium elements in grains.
Description
Technical Field
The invention relates to an atomic absorption spectrometer and a detection method for simultaneously detecting lead and cadmium elements in grains, and belongs to the technical field of atomic absorption spectroscopy.
Background
The world health organization determines lead and cadmium elements as grain pollutants to control. It is necessary to strengthen the detection of lead and cadmium in grains and prevent lead and cadmium poisoning. The existing grain determination method is mainly based on GB 5009.12-2010 determination of lead in national food safety standards and GB 5009.15-2014 determination of cadmium in national food safety standards. The existing atomic absorption spectrometer can detect the contents of lead and cadmium elements, but the limit value of lead and cadmium in a grain sample cannot be matched with the linear range of the existing atomic absorption spectrometer, so that the lead and cadmium in the grain are difficult to be simultaneously pretreated and simultaneously measured.
The X-ray fluorescence spectrometer of steel Minakg can test cadmium element in grain samples, but is only limited to the measurement of the cadmium element, and can not measure the lead element.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and further provides an atomic absorption spectrometer and a detection method for simultaneously detecting lead and cadmium elements in grains.
The purpose of the invention is realized by the following technical scheme:
an atomic absorption spectrometer for simultaneously measuring lead and cadmium elements in grains comprises: the high-performance lead-cadmium composite hollow cathode lamp, the atomizer, the light splitting and detecting system, the control system and the data processing system are respectively connected with the high-performance lead-cadmium composite hollow cathode lamp, the atomizer, the light splitting and detecting system and the data processing system, and the high-performance lead-cadmium composite hollow cathode lamp and the light splitting and detecting system are respectively connected with the atomizer.
The atomizer comprises a graphite tube, two heating electrodes, a second power supply and a second control module, wherein the two ends of the graphite tube are respectively connected with one heating electrode, the second power supply is electrically connected with the two heating electrodes respectively, and the second control module is connected with the second power supply. Two atomization regions, namely an atomization region I and an atomization region II, are arranged in the graphite tube.
A detection method of an atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains,
a pretreatment method for simultaneously extracting lead and cadmium elements in grains comprises the steps of ① smashing representative grain samples, sieving the smashed representative grain samples to obtain 60-mesh corn and other grains not smaller than 40-mesh, ② accurately transferring 3.0mL of 5% nitric acid solution into a 10mL centrifuge tube to serve as extracting solution, ③ accurately weighing 0.20g +/-0.01 g of sample into the 10mL centrifuge tube added with the extracting solution, ④ placing the 10mL centrifuge tube added with the sample on a vortex type oscillator, setting oscillation frequency to be 2000rpm, starting the oscillator, oscillating and mixing for 5 minutes, closing the oscillator, ⑤ supplementing 2.0mL of deionized water, starting the oscillator, oscillating and mixing for 30 seconds, closing the oscillator, ⑥ transferring the centrifuge tube into a centrifuge, setting rotation speed to be 5000r/min, starting the centrifuge for 1 minute, stopping the centrifuge automatically, ⑦ taking out the centrifuge tube, and sucking 1.0mL of supernatant into a sample bottle to obtain a standard sample.
① setting corresponding temperature rise degree, ② transferring standard sample to graphite tube by manual or automatic feeding to measure lead and cadmium element standard curve, ③ transferring measured sample to graphite tube by manual or automatic feeding to measure, and calculating to obtain final sample measured data after collecting atom spectrogram and data by data processing system.
The high-performance lead-cadmium composite hollow cathode lamp is configured in a lead element high-performance lamp working state, a cadmium element common lamp working state and a copper element near wavelength background-buckling working state, so that the lead-cadmium element background-buckling measurement is realized at the same time; meanwhile, a double-atomization-region atomizer and a corresponding power supply and control module are used, the double-atomization-region atomizer is configured in a regional and time-sharing atomization mode, and the calculation and selection of the optimal sensitivity of the lead and cadmium single elements are realized by setting whether to sample in different regions and adjusting the sample amount in different regions; the light splitting and detecting system adopts a concave grating and a photomultiplier, the concave grating is arranged on a reflection light path of a concave mirror, and the unique corresponding position of the photomultiplier is determined by the wavelength of different elements; the control system controls the time-sharing sequence work of the high-performance lead-cadmium composite hollow cathode lamp, controls the atomizer to heat according to a set temperature-rising program, and controls the light splitting and detection system to collect atomization data; and the data processing system performs operation processing on the acquired data to obtain a measurement result.
The high-performance lead-cadmium composite hollow cathode lamp adopted by the invention is different from a common multi-element lamp, the light energy is improved, the linear range is widened, the sensitivity and the detection limit are improved, the application range of the sample content is expanded due to the adoption of the double-atomization-zone atomizer, the detection method is simple, and the high-performance lead-cadmium composite hollow cathode lamp is suitable for rapid large-flux simultaneous detection of lead and cadmium elements in grains.
Drawings
FIG. 1 is a system diagram of an atomic absorption spectrometer for simultaneously measuring lead and cadmium elements in grains.
FIG. 2 is a diagram of an atomizer system.
FIG. 3 is a diagram of a high performance lead-cadmium composite hollow cathode lamp system.
In the figure, reference numerals, 1 is a high-performance lead-cadmium composite hollow cathode lamp, 2 is an atomizer, 3 is a light splitting and detecting system, 4 is a control system, 5 is a data processing system, 11 is a power supply I, 12 is a control module I, 13 is an anode, 14 is a lead-cadmium composite main cathode, 15 is a copper single main cathode, 16 is an auxiliary cathode, 21 is a graphite tube, 22 is an atomization zone I, 23 is an atomization zone II, 24 is a heating electrode, 25 is a power supply II, and 26 is a control module II.
Detailed Description
The invention will be described in further detail below with reference to the accompanying drawings: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation is given, but the scope of the present invention is not limited to the following embodiments.
As shown in fig. 1, the atomic absorption spectrometer for simultaneously measuring lead and cadmium elements in grain according to the present embodiment includes: the high-performance lead-cadmium composite hollow cathode lamp comprises a high-performance lead-cadmium composite hollow cathode lamp 1, an atomizer 2, a light splitting and detecting system 3, a control system 4 and a data processing system 5, wherein the control system 4 is respectively connected with the high-performance lead-cadmium composite hollow cathode lamp 1, the atomizer 2, the light splitting and detecting system 3 and the data processing system 5, and the high-performance lead-cadmium composite hollow cathode lamp 1 and the light splitting and detecting system 3 are respectively connected with the atomizer 2.
The high-performance lead-cadmium composite hollow cathode lamp 1 is configured in a lead element high-performance lamp working state, a cadmium element common lamp working state and a copper element near wavelength background-deducting working state, so that lead and cadmium elements are simultaneously subjected to background-deducting measurement; then the control system 4 controls the atomizer 2 to atomize the sample, the light splitting and detecting system 3 splits and detects the sample through the concave grating and the photomultiplier, and finally the data processing system 5 collects and calculates the measured data to obtain the lead and cadmium content test result.
As shown in fig. 3, the high-performance lead-cadmium composite hollow cathode lamp 1 includes: the high-performance lead-cadmium composite hollow cathode lamp comprises a power supply I11, a control module I12, an anode 13, a lead-cadmium composite main cathode 14, a copper single main cathode 15 and an auxiliary cathode 16, wherein the anode 13 of the power supply I11 is connected with the anode 13 of the high-performance lead-cadmium composite hollow cathode lamp 1, the cathode of the power supply I11 is respectively connected with the lead-cadmium composite main cathode 14, the copper single main cathode 15 and the auxiliary cathode 16 of the high-performance lead-cadmium composite hollow cathode lamp 1, and the control module I12 is respectively connected with the lead-cadmium composite main cathode 14, the copper single main cathode 15 and the auxiliary cathode 16 of the high-performance lead-cadmium composite hollow cathode lamp 1.
The working time sequence of the auxiliary cathode 16 is controlled by a control module I to configure the background-buckled working state of the high-performance lead-cadmium composite hollow cathode lamp 1 in the working state of a lead element high-performance lamp, the working state of a cadmium element common lamp and the working state of a copper element near wavelength, so that the lead-cadmium element and the copper element are simultaneously buckled and subjected to background measurement; the atomic absorption spectrometer widens the linear range of lead element and widens the measurement range by using the state change of the lead high-performance lamp.
As shown in fig. 2, the atomizer 2 includes a graphite tube 21, two heating electrodes 24, a second power supply 25 and a second control module 26, wherein two ends of the graphite tube 21 are respectively connected with one heating electrode 24, the second power supply 25 is respectively electrically connected with the two heating electrodes 24, and the second control module 26 is connected with the second power supply 25.
Two atomization regions, namely an atomization region I22 and an atomization region II 23, are arranged in the graphite tube 21.
The second power supply 25 supplies electric power to the graphite tube 21 electrode through the two heating electrodes 4, then the graphite tube converts the electric power into heat energy to dry, ash and atomize the sample, and the second control module 26 sets the temperature rise program of the atomizer.
The copper element of the copper single main cathode 15 is used as a near wavelength buckle background of lead and cadmium elements.
The embodiment relates to a detection method of an atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains,
a pretreatment method for simultaneously extracting lead and cadmium elements in grains comprises the steps of ① smashing representative grain samples, sieving the smashed representative grain samples to obtain 60-mesh corn and other grains not smaller than 40-mesh, ② accurately transferring 3.0mL of 5% nitric acid solution into a 10mL centrifuge tube to serve as extracting solution, ③ accurately weighing 0.20g +/-0.01 g of sample into the 10mL centrifuge tube added with the extracting solution, ④ placing the 10mL centrifuge tube added with the sample on a vortex type oscillator, setting oscillation frequency to be 2000rpm, starting the oscillator, oscillating and mixing for 5 minutes, closing the oscillator, ⑤ supplementing 2.0mL of deionized water, starting the oscillator, oscillating and mixing for 30 seconds, closing the oscillator, ⑥ transferring the centrifuge tube into a centrifuge, setting rotation speed to be 5000r/min, starting the centrifuge for 1 minute, stopping the centrifuge automatically, ⑦ taking out the centrifuge tube, and sucking 1.0mL of supernatant into a sample bottle to obtain a standard sample.
① setting corresponding temperature rise degree, ② transferring standard sample to graphite tube by manual or automatic feeding to measure lead and cadmium element standard curve, ③ transferring measured sample to graphite tube by manual or automatic feeding to measure, and calculating to obtain final sample measured data after collecting atom spectrogram and data by data processing system.
The above description is only a preferred embodiment of the present invention, and these embodiments are based on different implementations of the present invention, and the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. An atomic absorption spectrometer for simultaneously measuring lead and cadmium elements in grains comprises: the device comprises a high-performance lead-cadmium composite hollow cathode lamp (1), an atomizer (2), a light splitting and detecting system (3), a control system (4) and a data processing system (5), and is characterized in that the control system (4) is respectively connected with the high-performance lead-cadmium composite hollow cathode lamp (1), the atomizer (2), the light splitting and detecting system (3) and the data processing system (5), and the high-performance lead-cadmium composite hollow cathode lamp (1) and the light splitting and detecting system (3) are respectively connected with the atomizer (2);
the high-performance lead-cadmium composite hollow cathode lamp (1) comprises: the high-performance lead-cadmium composite hollow cathode lamp comprises a power supply I (11), a control module I (12), an anode (13), a lead-cadmium composite main cathode (14), a copper single main cathode (15) and an auxiliary cathode (16), wherein the anode of the power supply I (11) is connected with the anode (13) of the high-performance lead-cadmium composite hollow cathode lamp (1), the cathode of the power supply I (11) is respectively connected with the lead-cadmium composite main cathode (14), the copper single main cathode (15) and the auxiliary cathode (16) of the high-performance lead-cadmium composite hollow cathode lamp (1), and the control module I (12) is respectively connected with the lead-cadmium composite main cathode (14), the copper single main cathode (15) and the auxiliary cathode (16) of the high-performance lead-cadmium composite hollow cathode lamp (1);
the atomizer (2) comprises a graphite pipe (21), two heating electrodes (24), a second power supply (25) and a second control module (26), wherein the two ends of the graphite pipe (21) are respectively connected with one heating electrode (24), the second power supply (25) is electrically connected with the two heating electrodes (24), and the second control module (26) is connected with the second power supply (25).
2. The atomic absorption spectrometer for simultaneous measurement of lead and cadmium elements in grains according to claim 1, wherein two atomization zones, namely an atomization zone one (22) and an atomization zone two (23), are arranged in the graphite tube (21).
3. The atomic absorption spectrometer for simultaneous measurement of lead and cadmium elements in grains according to claim 2, wherein the copper element of the copper single main cathode (15) is used as a background for the adjacent wavelength of the lead and cadmium elements.
4. A method for detecting the lead and cadmium elements in the grains by using the atomic absorption spectrometer for simultaneous detection of the lead and cadmium elements in the grains as claimed in claim 1, 2 or 3,
firstly, a pretreatment method for simultaneously extracting lead and cadmium elements in grains comprises the steps of ①, crushing and sieving representative grain samples, namely 60 meshes of corn and not less than 40 meshes of other grains, ② accurately transferring 3.0mL of 5% nitric acid solution into a 10mL centrifuge tube to serve as extracting solution, ③ accurately weighing 0.20g +/-0.01 g of sample into the 10mL centrifuge tube added with the extracting solution, ④ placing the 10mL centrifuge tube added with the sample on a vortex type oscillator, setting the oscillation frequency to be 2000rpm, starting the oscillator, oscillating and mixing for 5 minutes, closing the oscillator, ⑤ supplementing 2.0mL of deionized water, starting the oscillator, oscillating and mixing for 30 seconds, closing the oscillator, ⑥ transferring the centrifuge tube into the centrifuge, setting the rotation speed to be 5000r/min, starting the centrifuge for 1 minute, automatically stopping the centrifuge, ⑦ taking out the centrifuge tube, and sucking 1.0mL of supernatant into a sample bottle to serve as a standard sample;
secondly, the high-performance lead-cadmium composite hollow cathode lamp is configured in the working state of a lead element high-performance lamp, the working state of a cadmium element common lamp and the working state of a copper element near wavelength background, so that the lead-cadmium element background-deducting measurement is realized at the same time; then the control system controls the atomizer to carry out sample atomization, the light splitting and detecting system carries out light splitting and detection through the concave grating and the photomultiplier, and finally the data processing system carries out acquisition and operation of measured data to obtain a test result of the lead and cadmium content.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4833366A (en) * | 1987-02-12 | 1989-05-23 | Beijing General Research Institute For Non-Ferrous Metals | High performance hollow cathode lamp |
| CN2063631U (en) * | 1990-01-03 | 1990-10-10 | 北京有色金属研究总院 | Hollow cathode lamp for visible ultraviolet molecular absorption spectrum |
| CN201707292U (en) * | 2010-06-23 | 2011-01-12 | 北京朝阳华洋分析仪器有限公司 | Transversally heated graphite tube |
| CN102184834A (en) * | 2011-04-21 | 2011-09-14 | 齐齐哈尔医学院 | Hollow cathode lamp and atomic absorption spectrometer manufactured by hollow cathode lamp |
| CN204536189U (en) * | 2015-02-11 | 2015-08-05 | 赵凯 | The horizontal graphite-pipe of a kind of Atomic absorption |
| CN106290180A (en) * | 2015-05-18 | 2017-01-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of Pb in food, chromium, cadmium and the detection method of copper content |
-
2017
- 2017-08-14 CN CN201710691555.9A patent/CN107589083B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4833366A (en) * | 1987-02-12 | 1989-05-23 | Beijing General Research Institute For Non-Ferrous Metals | High performance hollow cathode lamp |
| CN2063631U (en) * | 1990-01-03 | 1990-10-10 | 北京有色金属研究总院 | Hollow cathode lamp for visible ultraviolet molecular absorption spectrum |
| CN201707292U (en) * | 2010-06-23 | 2011-01-12 | 北京朝阳华洋分析仪器有限公司 | Transversally heated graphite tube |
| CN102184834A (en) * | 2011-04-21 | 2011-09-14 | 齐齐哈尔医学院 | Hollow cathode lamp and atomic absorption spectrometer manufactured by hollow cathode lamp |
| CN204536189U (en) * | 2015-02-11 | 2015-08-05 | 赵凯 | The horizontal graphite-pipe of a kind of Atomic absorption |
| CN106290180A (en) * | 2015-05-18 | 2017-01-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of Pb in food, chromium, cadmium and the detection method of copper content |
Non-Patent Citations (2)
| Title |
|---|
| 侯晓燕等.微波消解-石墨炉原子吸收法测定食品污染物中铅镉的含量.《中国食品卫生杂志》.2010,第22卷(第5期), * |
| 微波消解-石墨炉原子吸收法测定食品污染物中铅镉的含量;侯晓燕等;《中国食品卫生杂志》;20101231;第22卷(第5期);第418-420页 * |
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