CN107589083A - Lead and cadmium elements are the same as the Atomic Absorption Spectrometer and detection method surveyed in a kind of grain - Google Patents
Lead and cadmium elements are the same as the Atomic Absorption Spectrometer and detection method surveyed in a kind of grain Download PDFInfo
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- CN107589083A CN107589083A CN201710691555.9A CN201710691555A CN107589083A CN 107589083 A CN107589083 A CN 107589083A CN 201710691555 A CN201710691555 A CN 201710691555A CN 107589083 A CN107589083 A CN 107589083A
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Abstract
Lead and cadmium elements are the same as the Atomic Absorption Spectrometer and detection method surveyed in a kind of grain.Spectrometer uses lead cadmium composite hollow cathode modulation and power supply and control module, configures and closes on wavelength buckle back scape working condition in lead element high performance lamps working condition, cadmium element ordinary lamps working condition and copper, realizes lead and cadmium elements buckle back scape measurement simultaneously；Use diatomic area atomizer and power supply and control module simultaneously, by the configuration of diatomic area atomizer in subregion timesharing atomization pattern, by setting different zones, whether sample introduction and adjustment different zones sample size realize the calculating and selection of lead, cadmium single element optimum sensitivity；Method includes the pre-treating method that lead and cadmium elements extract simultaneously in grain and the sample introduction and data processing method of measurement simultaneously.The lead cadmium composite hollow cathode modulation of the present invention is different from common multi-element lamp, improves light energy, has widened the range of linearity, improves sensitivity and detection limit, is adapted to the quick big flux of lead and cadmium elements in grain to detect simultaneously.
Description
Technical field
The present invention relates to lead and cadmium elements in a kind of grain with the Atomic Absorption Spectrometer and detection method surveyed, belong to atom suction
Receive spectral technique field.
Background technology
Lead, cadmium element are defined as grain contamination thing and are controlled by by the World Health Organization.Strengthen grain lead, cadmium detection,
Prevent that lead, cadmium poisoning are very necessary.Existing grain determination methodology Main Basiss GB 5009.12-2010《Food security country
The measure of lead in standard food》With GB 5009.15-2014《The measure of national food safety standard cadmium in foods》.Existing original
Sub- absorption spectrometer can detect the content of lead, cadmium element, but due in grain samples lead cadmium Limited Doses can not match it is existing
The range of linearity of Atomic Absorption Spectrometer, the lead cadmium in grain is caused to be difficult to while pre-treatment and measure simultaneously.
Steel grinds the cadmium element that the Xray fluorescence spectrometer of nanogram can be tested in grain samples, but is only limited to cadmium element
Measurement, it is impossible to carry out the measurement of lead element.
The content of the invention
The invention aims to solve the above-mentioned problems of the prior art, and then provide lead cadmium member in a kind of grain
Element is the same as the Atomic Absorption Spectrometer and detection method surveyed.
The purpose of the present invention is achieved through the following technical solutions：
The same Atomic Absorption Spectrometer surveyed of lead and cadmium elements in a kind of grain, including：High-performance lead cadmium composite hollow cathode modulation,
Atomizer, light splitting and detecting system, control system and data handling system, the control system are answered with high-performance lead cadmium respectively
Close hollow cathode lamp, atomizer, light splitting and detecting system with data handling system to be connected, the high-performance lead cadmium compound air
Heart cathode modulation and light splitting and detecting system are connected with atomizer respectively.
It is each that the atomizer includes graphite-pipe, two heating electrodes, power supply two and control module two, the both ends of graphite-pipe
A heating electrode is connected with, power supply two electrically connects with two heating electrodes respectively, and control module two is connected with power supply two.Institute
State in graphite-pipe and be provided with Liang Ge atomization area, i.e. atomization area one and atomization area two.
A kind of detection method using lead and cadmium elements in grain with the Atomic Absorption Spectrometer surveyed,
One while lead and cadmium elements pre-treating method in grain is extracted, 1. crushed representative grain samples, mistake
Sieve, the mesh of corn 60, other grains are not less than 40 mesh；2. accurately pipette the conduct into 10mL centrifuge tubes of the salpeter solutions of 3.0mL 5%
Extract solution；3. 0.20g ± 0.01g samples are accurately weighed in having added in the 10mL centrifuge tubes of extract solution；4. after sample-adding
10mL centrifuge tubes are placed on spiral vortex type oscillator, and setting frequency of oscillation is 2000rpm, start oscillator, and vibration mixes 5 minutes,
Close oscillator；5. adding 2.0mL deionized waters, start oscillator, vibration mixes 30 seconds, closes oscillator；6. centrifuge tube turns
Move in centrifuge, rotating speed 5000r/min is set, 1 minute time, starts centrifuge, is automatically stopped to centrifuge；7. take out from
Heart pipe, it is standard sample into sample bottle to draw supernatant liquor 1.0mL.
The 2nd, 1. corresponding measurement heating degree is set；2. the transfer criteria sample by way of either manually or automatically sample introduction
Measured into graphite-pipe, make the standard curve of lead and cadmium elements；3. survey is shifted by way of either manually or automatically sample introduction
Amount sample measures into graphite-pipe, is transported after carrying out the collection of atomization spectrogram and data by data handling system
Calculate, draw final sample measurement data.
The present invention uses high-performance lead cadmium composite hollow cathode modulation and corresponding power supply and control module, by this high-performance lead cadmium
The configuration of composite hollow cathode modulation closes on ripple in lead element high performance lamps working condition, cadmium element ordinary lamps working condition and copper
Long buckle back scape working condition, realize lead and cadmium elements buckle back scape measurement simultaneously；Simultaneously using diatomic area atomizer and accordingly
Power supply and control module, diatomic area atomizer is configured in subregion timesharing atomization pattern, by setting not same district
Whether sample introduction and adjustment different zones sample size realize the calculating and selection of lead, cadmium single element optimum sensitivity in domain；It is divided
Concave grating and photomultiplier are used with detecting system, concave grating is located on the reflected light path of concave mirror, passes through different members
The wavelength of element determines unique correspondence position of photomultiplier；Point of control system control high-performance lead cadmium composite hollow cathode modulation
Sequential working, control atomizer are according to the heating schedule heating, control light splitting and detecting system of setting to atomization data
Collection；Data handling system carries out calculation process to the data of collection and draws measurement result.
High-performance lead cadmium composite hollow cathode modulation of the present invention is different from common multi-element lamp, improves luminous energy
Amount, has widened the range of linearity, has improved sensitivity and detection limit, sample size has been expanded in the use of diatomic area atomizer
The scope of application, detection method is simple, is adapted to the quick big flux of lead and cadmium elements in grain to detect simultaneously.
Brief description of the drawings
Fig. 1 is the same Atomic Absorption Spectrometer system diagram surveyed of lead and cadmium elements in grain.
Fig. 2 is atomizer system diagram.
Fig. 3 is high-performance lead cadmium composite hollow cathode modulation system diagram.
Reference in figure, 1 is high-performance lead cadmium composite hollow cathode modulation, and 2 be atomizer, and 3 be light splitting and detection
System, 4 be control system, and 5 be data handling system, and 11 be power supply one, and 12 be control module one, and 13 be anode, and 14 be lead cadmium
Compound main cathode, 15 be copper list main cathode, and 16 be auxiliary cathode, and 21 be graphite-pipe, and 22 be atomization area one, and 23 be atomization area
Two, 24 be heating electrode, and 25 be power supply two, and 26 be control module two.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail：The present embodiment using technical solution of the present invention as
Under the premise of implemented, give detailed embodiment, but protection scope of the present invention is not limited to following embodiments.
As shown in figure 1, lead and cadmium elements are the same as the Atomic Absorption Spectrometer surveyed, bag in a kind of grain involved by the present embodiment
Include：High-performance lead cadmium composite hollow cathode modulation 1, atomizer 2, light splitting and detecting system 3, control system 4 and data processing system
System 5, the control system 4 respectively with high-performance lead cadmium composite hollow cathode modulation 1, atomizer 2, light splitting and detecting system 3 and
Data handling system 5 is connected, the high-performance lead cadmium composite hollow cathode modulation 1 and light splitting and detecting system 3 respectively with atom
Change device 2 to be connected.
High-performance lead cadmium composite hollow cathode modulation 1 is configured in lead element high performance lamps working condition, cadmium element ordinary lamps work
Make state and copper closes on wavelength buckle back scape working condition, realize lead and cadmium elements buckle back scape measurement simultaneously；Then by by controlling
System 4 processed controls atomizer 2 to carry out sample atoms, and light splitting and detecting system 3 are entered by concave grating and photomultiplier
Row light splitting and detection, final data processing system 5 measures the collection of data and computing obtains the test result of lead cadmium content.
As shown in figure 3, the high-performance lead cadmium composite hollow cathode modulation 1 includes：Power supply 1, control module 1, sun
Pole 13, the compound main cathode 14 of lead cadmium, copper list main cathode 15 and auxiliary cathode 16, positive pole and the high-performance lead cadmium of the power supply 1
The anode 13 of composite hollow cathode modulation 1 is connected, the negative pole of power supply 1 respectively with high-performance lead cadmium composite hollow cathode modulation 1
The compound main cathode 14 of lead cadmium, copper list main cathode 15 are connected with auxiliary cathode 16, control module 1 respectively with high-performance lead cadmium
The compound main cathode 14 of lead cadmium, the copper list main cathode 15 of composite hollow cathode modulation 1 are connected with auxiliary cathode 16.
High-performance lead cadmium composite hollow cathode modulation 1 is configured by the work schedule of the control auxiliary cathode 16 of control module one
Wavelength buckle back scape working condition is closed in lead element high performance lamps working condition, cadmium element ordinary lamps working condition and copper,
Realize lead and cadmium elements buckle back scape measurement simultaneously；This Atomic Absorption Spectrometer has widened lead element using lead high performance lamps state change
The range of linearity, widened measurement range.
As shown in Fig. 2 the atomizer 2 includes 21, two heating electrodes 24 of graphite-pipe, power supply 2 25 and control module
2 26, the both ends of graphite-pipe 21 are respectively connected with a heating electrode 24, and power supply 2 25 electrically connects with two heating electrodes 24 respectively,
Control module 2 26 is connected with power supply 2 25.
Liang Ge atomization area, i.e. atomization area 1 and atomization area 2 23 are provided with the graphite-pipe 21.
Power supply 2 25 provides electrical power by two heating electrodes 4 for the electrode of graphite-pipe 21, is then converted into by graphite-pipe
Thermal energy makes sample drying ashing and atomization, and control module 2 26 sets the heating schedule of atomizer.
The copper of the copper list main cathode 15 uses as the wavelength buckle back scape that closes on of lead and cadmium elements.
A kind of detection method using lead and cadmium elements in grain with the Atomic Absorption Spectrometer surveyed involved by the present embodiment,
One while lead and cadmium elements pre-treating method in grain is extracted, 1. crushed representative grain samples, mistake
Sieve, the mesh of corn 60, other grains are not less than 40 mesh；2. accurately pipette the conduct into 10mL centrifuge tubes of the salpeter solutions of 3.0mL 5%
Extract solution；3. 0.20g ± 0.01g samples are accurately weighed in having added in the 10mL centrifuge tubes of extract solution；4. after sample-adding
10mL centrifuge tubes are placed on spiral vortex type oscillator, and setting frequency of oscillation is 2000rpm, start oscillator, and vibration mixes 5 minutes,
Close oscillator；5. adding 2.0mL deionized waters, start oscillator, vibration mixes 30 seconds, closes oscillator；6. centrifuge tube turns
Move in centrifuge, rotating speed 5000r/min is set, 1 minute time, starts centrifuge, is automatically stopped to centrifuge；7. take out from
Heart pipe, it is standard sample into sample bottle to draw supernatant liquor 1.0mL.
The 2nd, 1. corresponding measurement heating degree is set；2. the transfer criteria sample by way of either manually or automatically sample introduction
Measured into graphite-pipe, make the standard curve of lead and cadmium elements；3. survey is shifted by way of either manually or automatically sample introduction
Amount sample measures into graphite-pipe, is transported after carrying out the collection of atomization spectrogram and data by data handling system
Calculate, draw final sample measurement data.
The foregoing is only a preferred embodiment of the present invention, these embodiments are all based on the present invention
Different implementations under general idea, and protection scope of the present invention is not limited thereto, it is any to be familiar with the art
Technical staff the invention discloses technical scope in, the change or replacement that can readily occur in, should all cover the present invention's
Within protection domain.Therefore, protection scope of the present invention should be defined by the protection domain of claims.
Claims (6)
1. the same Atomic Absorption Spectrometer surveyed of lead and cadmium elements in a kind of grain, including：High-performance lead cadmium composite hollow cathode modulation
(1), atomizer (2), light splitting and detecting system (3), control system (4) and data handling system (5), it is characterised in that institute
State control system (4) respectively with high-performance lead cadmium composite hollow cathode modulation (1), atomizer (2), light splitting and detecting system (3)
It is connected with data handling system (5), the high-performance lead cadmium composite hollow cathode modulation (1) and light splitting and detecting system (3) point
It is not connected with atomizer (2).
2. lead and cadmium elements are the same as the Atomic Absorption Spectrometer surveyed in grain according to claim 1, it is characterised in that the height
Performance lead cadmium composite hollow cathode modulation (1) includes：Power supply one (11), control module one (12), anode (13), the compound main the moon of lead cadmium
Pole (14), copper list main cathode (15) and auxiliary cathode (16), positive pole and the high-performance lead cadmium composite hollow of the power supply one (11)
The anode (13) of cathode modulation (1) is connected, the negative pole of power supply one (11) respectively with high-performance lead cadmium composite hollow cathode modulation (1)
The compound main cathode of lead cadmium (14), copper list main cathode (15) are connected with auxiliary cathode (16), control module one (12) respectively with height
The compound main cathode of lead cadmium (14), copper list main cathode (15) and auxiliary cathode (16) phase of performance lead cadmium composite hollow cathode modulation (1)
Connection.
3. lead and cadmium elements are the same as the Atomic Absorption Spectrometer surveyed in grain according to claim 2, it is characterised in that the original
Sonization device (2) includes graphite-pipe (21), two heating electrodes (24), power supply two (25) and control module two (26), graphite-pipe
(21) both ends are respectively connected with a heating electrode (24), and power supply two (25) is electrically connected with two heating electrodes (24), controlled respectively
Molding block two (26) is connected with power supply two (25).
4. lead and cadmium elements are the same as the Atomic Absorption Spectrometer surveyed in grain according to claim 3, it is characterised in that the stone
Liang Ge atomization area, i.e. atomization area one (22) and atomization area two (23) are provided with ink pipe (21).
5. lead and cadmium elements are the same as the Atomic Absorption Spectrometer surveyed in grain according to claim 4, it is characterised in that the copper
The copper of single main cathode (15) uses as the wavelength buckle back scape that closes on of lead and cadmium elements.
6. inspection of the lead and cadmium elements with the Atomic Absorption Spectrometer surveyed in the grain described in a kind of usage right requirement 1,2,3,4 or 5
Survey method, it is characterised in that
The first, corresponding measurement heating degree is set；
2nd, transfer criteria sample measures into graphite-pipe by way of either manually or automatically sample introduction, makes lead and cadmium elements
Standard curve；
3rd, measurement sample is shifted by way of either manually or automatically sample introduction to measure into graphite-pipe, passes through data processing
System carries out computing after carrying out the collection of atomization spectrogram and data, draws final sample measurement data.
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| CN201710691555.9A CN107589083B (en) | 2017-08-14 | 2017-08-14 | Atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains and detection method |
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| CN201710691555.9A CN107589083B (en) | 2017-08-14 | 2017-08-14 | Atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains and detection method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116593412A (en) * | 2023-05-18 | 2023-08-15 | 佛山市沃特测试技术服务有限公司 | Food detection instrument and method for microelement analysis |
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| CN116593412A (en) * | 2023-05-18 | 2023-08-15 | 佛山市沃特测试技术服务有限公司 | Food detection instrument and method for microelement analysis |
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