CN110441247A - A kind of Atomic absorption/emission spectrum in flame detection device simultaneously - Google Patents
A kind of Atomic absorption/emission spectrum in flame detection device simultaneously Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 51
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 48
- 238000000295 emission spectrum Methods 0.000 title claims abstract description 41
- 230000003595 spectral effect Effects 0.000 claims abstract description 22
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 7
- 230000001360 synchronised effect Effects 0.000 claims abstract description 6
- 238000000712 atomic emission detection Methods 0.000 claims abstract description 5
- 238000001228 spectrum Methods 0.000 claims description 11
- 238000005259 measurement Methods 0.000 abstract description 12
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000005070 sampling Methods 0.000 abstract description 4
- 230000000295 complement effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 11
- 239000011734 sodium Substances 0.000 description 11
- 230000005283 ground state Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000005284 excitation Effects 0.000 description 6
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001007 flame atomic emission spectroscopy Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- 238000001636 atomic emission spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000567 combustion gas Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical group [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000000559 atomic spectroscopy Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000013075 data extraction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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Abstract
The present invention discloses a kind of detection device simultaneously of Atomic absorption/emission spectrum in flame, the outgoing beam of light source successively by shutter, prefocusing lens, atomizer/excitaton source and after condenser lens reach detector；The switch that time-sequence control module triggers shutter carries out modulation of source, and synchronous detection trigger device carries out spectroscopic acquisition, so that it is carried out atomic absorption spectrum detection during shutter is opened, atomic emission detection is carried out during shutter close.The present invention is integrated with Atomic absorption and emission spectrum detection in same atomizer/excitaton source, can single injected sampling measure Atomic absorption and emission spectrum simultaneously, therefore sample consumption is reduced, and improves two kinds of spectral signals time of measurement result and Space Consistency simultaneously；Expand the concentration range that can analyze unknown sample by being complementary to one another for measurement result, and realizes that the mutual calibration of two kinds of measurement results improves precision of analysis.
Description
Technical field
The present invention relates to atomic spectroscopic analysis technical field, Atomic absorption/emission spectrum in specially a kind of flame is same
When detection device.
Background technique
Atomic spectrometry determination is one of the Element detection means being most widely used.By the development of many years, atom light
Spectral analysis technology has graduallyd mature, including principle, it is theoretical with instrument, using etc..Currently, the miniaturization of instrument, multifunction at
Meet more application scenarios demands for its important one of developing direction to obtain more analyte relevant informations.Tradition
Atomic Absorption Spectrometric Instruments be usually made of light source, atomizer and detection system, by measure by atomizing element base
The atomic absorption light spectral intensity of state atom is treated survey element and is quantified；Atomic Emission Spectrometer AES device is usually by excitaton source and detection
System is constituted, and the atomic emission spectrum intensity by measuring the element excited atom being excited quantifies element to be measured.
Traditional Atomic absorption and Atomic Emission Spectrometer AES device works in single-mode, even if the instrument of integrated two kinds of functions, also only
A kind of function use can be selected before detection；Can not single injected sampling obtain Atomic absorption and atomic emission spectrum signal, nothing simultaneously
Method combines the respective advantage of two kinds of measuring principles and extends the application range of atomic spectroscopic analysis instrument.Can not still at present
Realize the atom spectrum instrument that Atomic absorption and atomic emission spectrum measure simultaneously.
Flame atom absorption spectrophotography method (Flame Atomic Absorption Spectrometry, FAAS) is made
For a kind of practical atomic spectroscopic analysis technology, it is widely used to the fields such as scientific research and industrial production.It is by liquid-like
Product are brought into head-on collision atomizer by combustion-supporting gas, are formed subtle droplet and are formed flame with the uniform after-combustion of combustion gas mixing, make sample
Product solution removes solvent, is atomized into the ground state atom steam for element to be measured, and passes through extinction caused by measurement ground state atom
Degree signal determines the concentration of element to be measured in sample.FAAS is by selecting suitable flame to can satisfy the survey of most elements
Amount demand can directly measure most of metallic element, can also indirect determination part nonmetalloid even organic compound.So
And there is also some limitations by FAAS, and such as: poor for part easily dissociation, the elemental analysis sensitivity of easily ionizable, work is bent
The line range of linearity is relatively narrow, and multielement cannot be carried out while be measured etc., these bring many be stranded to practical application
It is difficult.
FAAS measurement part is easily dissociated, the problem that the elemental analysis sensitivity of easily ionizable is poor, the main reason is that
These elements easy ionization or excitation in flame, lead to the reduction of ground state free atom and excited atom increases, therefore final
Atomic absorption spectrum measurement sensitivity it is poor；And excited atom increases the effect that exactly atomic emission detection expectation obtains
Fruit helps to improve its sensitivity.In addition, it is also that Atomic Emission Spectral Analysis method is solid that the range of linearity is wide, multielement detects simultaneously
Some advantages.In fact, flame is both a kind of atomizer and a kind of excitaton source herein.Using the high temperature of flame by member to be measured
Element is energized into excitation state, and carrying out quantitative method to sample concentration according to its characteristic emission spectral line is NITRATE BY FLAME ATOMIC transmitting
Spectra methods (Flame Atomic Emission Spectrometry, FAES).It is in chemical industry, food, environment and geology
It has a wide range of applications in terms of the Element detection of equal ambits, especially to the lower alkali metal of excitation Capability Requirement and alkaline earth gold
Belonging to element such as sodium, calcium, magnesium etc. and the higher element of content has good measurement effect.Although the detection limit of existing FAES is also not
Enough ideals, but it is easy to operate, to sample morphology close friend, the range of linearity is wider, still plays and focuses in actual sample analysis
It acts on.
If FAES and FAAS can be integrated, and realize Atomic absorption and atomic emission spectrum while measuring, then
The advantage that the two can sufficiently be combined, forms novel atom spectrum instrument.And atomic absorption spectrography (AAS) and atomic emission spectrum
Method also has similar place in principle and apparatus structure, and maximum difference is only atomic absorption spectroscopy relative to original
One additional light source of sub- emission spectrometry method needs generates the characteristic spectral line of element to be measured, such as hollow cathode lamp；The two
Integrated there is potential feasibility.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of Atomic absorption and atomic emission spectrums of can be realized
It measures simultaneously, improves the comprehensive analysis performance of instrument, and extend the atom in the flame of atomic spectroscopic analysis instrument application range
Absorption/emission spectrum while detection device.Technical solution is as follows:
A kind of Atomic absorption/emission spectrum detection device, including light source, shutter, prefocusing lens, atomization simultaneously in flame
Device/excitaton source, rear condenser lens, detector and time-sequence control module；It is saturating that the outgoing beam of light source successively passes through shutter, prefocusing
Mirror, atomizer/excitaton source and rear condenser lens reach detector；The switch that time-sequence control module triggers shutter carries out light source tune
System, and synchronous detection trigger device carries out spectroscopic acquisition, it is made to carry out atomic absorption spectrum detection, During shutter is opened
Atomic emission detection is carried out during shutter close.
Further, detection trigger device carries out the timing that the period of the clock signal of spectroscopic acquisition is modulation of source
The half of signal period, and the two phase is kept fixed；Between the high period of the clock signal of modulation of source, shutter is opened,
The clock signal that detection trigger device carries out spectroscopic acquisition is also high level, and the spectral signal of detector acquisition is Atomic absorption
Spectral signal；Between the low period of the clock signal of modulation of source, shutter close, detection trigger device carries out spectroscopic acquisition
Clock signal be in high level again, the spectral signal of detector acquisition is atomic emission spectrum signal.
Further, time-sequence control module detection trigger device carries out the commencing signal of spectroscopic acquisition, faster than triggering
The signal delay certain time of door open-close, and the signal for stopping spectroscopic acquisition is more certain in advance than the signal of shutter off/on
Time.
The beneficial effects of the present invention are:
1) present invention can single injected sampling realize that the Atomic absorption of element to be measured and atomic emission spectrum detect simultaneously in flame, mention
The time and Space Consistency of high two kinds of spectral signals while measurement result；
2) present invention is measured simultaneously by Atomic absorption and atomic emission spectrum, and two kinds of measurement results are complementary to one another, and can be obtained
The broader working curve range of linearity expands the Atomic absorption of single-mode or the detection of content of element model of atomic emission spectrum
It encloses, the broader element sample to be measured of analytical concentration range；
3) atomization due to different elements to be measured in flame or launching efficiency are different, lead to its ground state and excited atom
Ratio is different, can be selected in two kinds of measurement results measurement effect more preferably atomic absorption spectrography (AAS) or atomic emission spectrometry into
Row analysis is mutually calibrated to obtain more accurate detection effect, or by two kinds of measurement results；
4) Atomic absorption and the Atomic Emission Spectral Analysis of identity element may be implemented in the present invention, can also be achieved the atom of multielement
Emission spectrum is analyzed simultaneously, and sample consumption can be effectively reduced；
5) result that the present invention combines Atomic absorption and atomic emission spectrum to measure simultaneously can be to original of the element to be measured in flame
Subbase state and excitation state are analyzed, and atom thermodynamical equilibrium situation can be investigated；Flame spreading atom spectrum instrument applies model
It encloses.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of Atomic absorption/emission spectrum in flame of the present invention while detection device.
Fig. 2 is the time diagram of time-sequence control module of the present invention output.
Fig. 3 is the spectrogram that the present invention uses Atomic absorption and Simultaneous Determination Na element.
Fig. 4 is the present invention using Atomic absorption and Simultaneous Determination Cu Elements Atom absorption spectrum and Na
The spectrogram of Elements Atom emission spectrum.
In figure: 1. light sources, 2. shutters, 3. prefocusing lens, 4. atomizers/excitaton source, condenser lens after 5., 6. detections
Device, 7. time-sequence control modules.
Specific embodiment
The present invention is described in further details in the following with reference to the drawings and specific embodiments.Present invention combination atomic absorption light
In place of spectrum and atomic emission spectrum principle and the similar and difference of apparatus structure, atomizer/excitaton source and detector are shared, is led to
The synchronous working between time-sequence control module coordination light source and detector is crossed, realizes that Atomic absorption and emission spectrum measure simultaneously.
Sample analytes are evaporated in flame atomizer/excitaton source, dissociate, be atomized into for the gaseous state ground state of element to be measured it is former
Son, a part of ground state atom absorb the characteristic wavelength radiation of light source, and the illuminant characterization wavelength signals weakened by detection are available
Atomic absorption light spectrum signal；In addition, part ground state atom further obtains energy in flame atomizer/excitaton source reaches sharp
State is sent out, low-lying level state is then returned to by excitation state and gives off the light of its characteristic wavelength simultaneously, and obtains atomic emission spectrum
Signal.
As shown in Figure 1, detection device includes light source 1, shutter to Atomic absorption/emission spectrum in flame of the invention simultaneously
2, prefocusing lens 3, atomizer/excitaton source 4, rear condenser lens 5, detector 6 and time-sequence control module 7；The outgoing of light source 1
Light beam successively by shutter 2, prefocusing lens 3, atomizer/excitaton source 4 and after condenser lens 5 reach detector 6；Timing control
The switch that molding block 7 triggers shutter 2 carries out modulation of source, and synchronous detection trigger device 6 carries out spectroscopic acquisition, makes it fast
Door 2 carries out atomic absorption spectrum detection during opening, and carries out atomic emission detection in 2 down periods of shutter.
As shown in Fig. 2, abscissa represents the time, unit: ms, ordinate represent clock signal level.Top is timing control
Molding block triggers the timing of shutter release, and high level represents shutter opening；Low level represents shutter close.Lower section is timing control
Module detection trigger device acquires the timing of spectral signal, and high level represents detector acquisition spectral signal；Low level represents detection
Device stops spectroscopic acquisition.
Time-sequence control module coordinates the synchronization work between shutter progress modulation of source and detector progress spectroscopic acquisition
Make, and realizes the time diagram of Atomic absorption and atomic emission spectrum while detection.
In the present embodiment, the period that detection trigger device carries out the clock signal of spectroscopic acquisition is the timing of modulation of source
The half of signal period, and the two phase is kept fixed；Between the high period of the clock signal of modulation of source, shutter is opened,
The clock signal that detection trigger device carries out spectroscopic acquisition is also high level, and the spectral signal of detector acquisition is Atomic absorption
Spectral signal；Between the low period of the clock signal of modulation of source, shutter close, detection trigger device carries out spectroscopic acquisition
Clock signal be in high level again, the spectral signal of detector acquisition is atomic emission spectrum signal.Wherein, timing control
Molding block detection trigger device carries out the commencing signal of spectroscopic acquisition, the signal delay certain time of door open-close faster than triggering,
And the signal for stopping spectroscopic acquisition shifting to an earlier date certain time than the signal of shutter off/on, and detector is avoided to detect shutter
The spectral signal of switching moments fluctuates, and improves the stability of signal acquisition.
It is specific as follows:
1. the clock signal of time-sequence control module output light source modulation, 100 ms of period, duty ratio 50%, high electricity in a cycle
Flat 50 ms of duration, 50 ms of the low level duration；Between the high period of clock signal, shutter is opened；Believe in timing
Number low period between, shutter close；
2. time-sequence control module exports the clock signal that detection trigger device carries out spectroscopic acquisition, 50 ms of period, duty ratio
60%, 30 ms of high level lasting time, 20 ms of the low level duration in a cycle；Phase is kept with 1. middle clock signal
It is fixed；Meanwhile first rising edge compares first 10 ms of rise edge delay of clock signal in 1., second rising edge compares in 1.
First failing edge of clock signal postpones 10 ms.Detector carries out spectroscopic acquisition, In between the high period of clock signal
Detector stops spectroscopic acquisition between the low period of clock signal；
3. between the 1. high period of middle clock signal, between the high period of corresponding 2. middle clock signal, the light of detector acquisition
Spectrum signal is atomic absorption light spectrum signal；Between the 1. low period of middle clock signal, the high level of corresponding 2. middle clock signal
Period, the spectral signal of detector acquisition are atomic emission spectrum signal.
Concrete operations process of the invention is as follows:
1) sample feeding pipe is inserted into sample solution, sample solution sucks atomizer, the subtle mist of generation by the negative pressure of combustion-supporting gas
Grain uniformly enters combustion head with combustion gas mixing afterwards；
2) sample analytes are evaporated in atomizer/excitaton source Air-acetylene Flame (or other type flames), solve
From the gaseous state ground state or excited atom that, atomization/excitation becomes element to be measured；
3) time-sequence control module coordinates the synchronous working between shutter progress modulation of source and detector progress spectroscopic acquisition,
To the ground state atom and excited atom progress Atomic absorption and atomic emission spectrum letter in step 2 in atomizer/excitaton source
Number detection, thus detection while realizing single injected sampling to Atomic absorption and atomic emission spectrum；
4) data extraction is carried out to the spectral signal collected simultaneously in step 3), obtains independent Atomic absorption and atom hair
Spectral signal is penetrated, the further data processing of subsequent needs is carried out.
Embodiment 1: in the Atomic absorption/emission spectrum while detection device in the present embodiment flame, contain Na element
Sample solution enters in the flame of the formation of atomizer/excitaton source 4, and Atomic absorption/emission spectrum through the invention is examined simultaneously
Survey technology, finally obtain Na element Atomic absorption and atomic emissions at the same detection spectrogram, as shown in figure 3, abscissa generation
Table wavelength, ordinate representation signal value.Dotted line represents the outgoing spectral signal of light source, and solid line represents the atomic absorption light of Na element
Spectrum signal；Chain-dotted line represents the atomic emission spectrum signal of Na element；Wherein, 589.00 nm and 589.59 nm are Na element
Characteristic wavelength.
Embodiment 2: in the Atomic absorption/emission spectrum while detection device in the present embodiment flame, contain Cu and Na member
The sample solution of element enters in the flame of the formation of atomizer/excitaton source 4, and Atomic absorption/emission spectrum through the invention is same
When detection technique, finally obtain the Atomic absorption of Cu element and the atomic emissions of Na element and meanwhile detection spectrogram, such as Fig. 4 institute
Show, abscissa represents wavelength, ordinate representation signal value.Dotted line represents the outgoing spectral signal of light source, in solid line representative sample
The atomic absorption light spectrum signal of Cu element；Chain-dotted line represents the atomic emission spectrum signal of Na element；Wherein, 324.75 nm and
327.40 nm are the characteristic wavelength of Cu element.
Claims (3)
1. Atomic absorption/emission spectrum while detection device in a kind of flame, which is characterized in that including light source (1), shutter
(2), prefocusing lens (3), atomizer/excitaton source (4), rear condenser lens (5), detector (6) and time-sequence control module
(7)；The outgoing beam of light source (1) successively by shutter (2), prefocusing lens (3), atomizer/excitaton source (4) and after focus
Lens (5) reach detector (6)；The switch that time-sequence control module (7) triggers shutter (2) carries out modulation of source, and synchronous triggering
Detector (6) carries out spectroscopic acquisition, so that it is carried out atomic absorption spectrum detection during shutter (2) are opened, in shutter (2)
Down periods carry out atomic emission detection.
2. Atomic absorption/emission spectrum while detection device in flame according to claim 1, which is characterized in that touching
The period of the clock signal of detector progress spectroscopic acquisition is sent out as the half in the clock signal period of modulation of source, and the two
Phase is kept fixed；Between the high period of the clock signal of modulation of source, shutter is opened, and detection trigger device carries out spectral signal
The clock signal of acquisition is also high level, and the spectral signal of detector acquisition is atomic absorption light spectrum signal；In modulation of source
Between the low period of clock signal, shutter close, the clock signal that detection trigger device carries out spectroscopic acquisition is in again
High level, the spectral signal of detector acquisition are atomic emission spectrum signal.
3. Atomic absorption/emission spectrum while detection device in flame according to claims 1 and 2, which is characterized in that
Time-sequence control module detection trigger device carries out the commencing signal of spectroscopic acquisition, than the signal delay one for triggering fast door open-close
It fixes time, and the signal for stopping spectroscopic acquisition shifting to an earlier date certain time than the signal of shutter off/on.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257256A (en) * | 2020-03-26 | 2020-06-09 | 四川大学 | Atomic absorption, fluorescence and emission spectrum simultaneous measurement analysis detection system and method |
| CN112903628A (en) * | 2021-01-25 | 2021-06-04 | 内蒙古光能科技有限公司 | Trace gas detection device in negative pressure state and detection method thereof |
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