CN105842221A - Atomic fluorescence spectrometer and background subtraction method thereof - Google Patents

Atomic fluorescence spectrometer and background subtraction method thereof Download PDF

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Publication number
CN105842221A
CN105842221A CN201610377937.XA CN201610377937A CN105842221A CN 105842221 A CN105842221 A CN 105842221A CN 201610377937 A CN201610377937 A CN 201610377937A CN 105842221 A CN105842221 A CN 105842221A
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fluorescence signal
light source
sample
object element
fluorescence
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CN105842221B (en
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高树林
李志华
李宏
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BEIJING JINSUKUN TECHNOLOGY DEVELOPMENT Co Ltd
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BEIJING JINSUKUN TECHNOLOGY DEVELOPMENT Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6402Atomic fluorescence; Laser induced fluorescence
    • G01N21/6404Atomic fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6402Atomic fluorescence; Laser induced fluorescence
    • G01N21/6404Atomic fluorescence
    • G01N2021/6406Atomic fluorescence multi-element
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N2021/6417Spectrofluorimetric devices

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  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a background subtraction method of an atomic fluorescence spectrometer. The method includes: testing a tested sample through a target element light source to obtain a first fluorescence signal, wherein the first fluorescence signal is a superposed signal of fluorescence signals generated by interference elements and a target element in the tested sample; testing the tested sample through a background subtraction light source to obtain a second fluorescence signal, wherein the second fluorescence signal is a fluorescence signal generated by the interference elements in the tested sample; subjecting the first fluorescence signal and the second fluorescence signal to margin calculation to obtain a fluorescence signal of the target element. By addition of the background subtraction light source, the fluorescence signal generated by the interference elements in the tested sample is obtained and then subtracted according to an algorithm, and accordingly testing accuracy is improved.

Description

Atomic fluorescence spectrometer background deduction method and atomic fluorescence spectrometer
Technical field
The present invention relates to spectrogrph spectral processing techniques field, particularly relate to a kind of atomic fluorescence spectrometer Background deduction method and atomic fluorescence spectrometer.
Background technology
At present, atomic fluorescence spectrometer to be widely used in food, environmental protection, medicine, disease control, geology Look for ore deposit, the mensuration of the elements such as the heavy metal arsenic hydrargyrum lead antimony bismuth in the field such as metallurgical, testing these heavy metals Often containing in the sample of element and be difficult to by atomizing element (aluminum calcium etc.), in test process, these are high Temperature element is difficult to by atomization, is easily generated the little granule of oxide, and the light of excitation source is produced refraction, Overlap with fluorescence signal produced by object element, detected by photomultiplier tube, just create serious Interference, above-mentioned interference causes the biggest error to test.
Atomic fluorescence spectrometer is to utilize short focus dispersionless light path system principle so that at the bottom of detection limit, Highly sensitive, cost is low, is used widely in China.But atomic fluorescence easily produces folding to light source again Rhizoma Belamcandae is disturbed, so limiting atomic fluorescence spectrometer can only preferably be applied to hydride generation method institute energy The element of test, it is to avoid high temperature element produces refraction interference to light source.Therefore Atomic Fluorescence Spectrometry is limited Try the probability of more multielement.
In prior art, the method taked is to utilize hydride generation method to make tested Element generation corresponding Hydride, the high temperature element sepatation with difficult atomization is easily generated metal-oxide, eliminate and object element is surveyed The interference of examination.But the element that can generate hydride after all is limited, the most greatly have impact on atom glimmering Light can the quantity of test elements.Affect atomic fluorescence spectrometer application in more areas.Exist at present Atomic fluorescence field does not the most utilize the method that the function of instrument itself carrys out background correction interference, Zhi Nengli Separate tested object element with hydride generation method, or separate when sample pre-treatments, come Reach the purpose of test target element.But element only ten several elements at present that thing separates can be hydrogenated, Affect atomic fluorescence spectrometer device actual application value in more areas.
Summary of the invention
It is an object of the invention to provide a kind of during atomic fluorescence spectrometer detection sample, logical Cross increase button background light source, obtain fluorescence signal produced by interference element in sample, and then use Fluorescence signal produced by algorithm deduction interference element, improves the accuracy rate of test.
In order to realize described goal of the invention, according to an aspect of the present invention, it is provided that a kind of atomic fluorescence light The background deduction method of spectrometer, including:
By object element light source, sample is tested, obtain the first fluorescence signal;Described first Fluorescence signal is the superposition letter of fluorescence signal produced by object element and interference element in described sample Number;
By button background light source, described sample is tested, obtain the second fluorescence signal;Described Two fluorescence signal values are fluorescence signal produced by interference element in described sample;
Carry out making difference operation by described first fluorescence signal and the second fluorescence signal, obtain described object element Fluorescence signal.
Further, described by object element light source, sample is tested, obtain the first fluorescence letter Number step include:
By atomizer, described sample is carried out atomization;
Atomization region by sample described in object element light source activation;
Described atomization region is detected, obtains described first fluorescence signal.
Further, described by button background light source described sample is tested, obtain the second fluorescence The step of signal includes:
Atomization region by sample described in buckle back scape light source activation;
Described atomization region is detected, obtains described second fluorescence signal.
Further, in the step in the described atomization region by sample described in object element light source activation After Zhou, including:
After first scheduled time, extinguish object element light source;
After second scheduled time that object element light source extinguishes, light described button background light source.
Further, by button background light source, sample is tested described, obtain the second fluorescence letter Number step after, also include:
By formula (1), described second fluorescence signal is converted, obtain scaling results;
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;
F is, by button background light source, sample is tested the second obtained fluorescence signal;
A1 is, by object element light source, interference solution is tested obtained fluorescence signal;
A2 is, by object element light source, blank solution is tested obtained fluorescence signal;
B1 is, by button background light source, interference solution is tested obtained fluorescence signal;
B2 is, by button background light source, blank solution is tested obtained fluorescence signal.
Further, described carry out making difference operation by described first fluorescence signal and the second fluorescence signal, obtain The step of the fluorescence signal of object element includes:
By formula (2), described scaling results and the first fluorescence signal are calculated, obtain described target The fluorescence signal of element;
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;
A is described first fluorescence signal;
F is described scaling results.
Further, the high intensity made by element that described button background light source does not contains in using sample Hollow cathode lamp.
In order to realize described goal of the invention, according to a further aspect in the invention, it is provided that a kind of atomic fluorescence Spectrogrph, including:
Atomizer, for carrying out atomization to sample;
Object element light source, for exciting the atomization region of described sample;
Button background light source, for exciting the atomization region of described sample;
Detector, for the atomization region when object element light source is lit, to described sample Detect, obtain the first fluorescence signal;It is additionally operable to when buckle back scape light source light source is lit, to described The atomization region of sample is detected, and obtains the second fluorescence signal;
Described first fluorescence signal is glimmering produced by the object element in described sample and interference element The superposed signal of optical signal;Described second fluorescence signal value is the glimmering of the interference element in described sample Optical signal;
Computing module, for described first fluorescence signal and the second fluorescence signal are made difference operation, Fluorescence signal to described object element.
Further, described a kind of atomic fluorescence spectrometer, also include control module, at object element light After first scheduled time that source point is lit, send to described object element light source and extinguish instruction, to put out Go out described object element light source;It is additionally operable to after second scheduled time that object element light source extinguishes, to Described button background light source sends enabled instruction, to light described button background light source.
Further, described a kind of atomic fluorescence spectrometer, described computing module includes: first calculates list Unit, for being converted described second fluorescence signal by formula (1), obtains scaling results;
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;
F is, by button background light source, sample is tested the second obtained fluorescence signal;
A1 is, by object element light source, interference solution is tested obtained fluorescence signal;
A2 is, by object element light source, blank solution is tested obtained fluorescence signal;
B1 is, by button background light source, interference solution is tested obtained fluorescence signal;
B2 is, by button background light source, blank solution is tested obtained fluorescence signal.
Further, described a kind of atomic fluorescence spectrometer, described computing module also includes: second calculates Unit, for being calculated described scaling results and the first fluorescence signal by formula (2), obtains institute State the fluorescence signal of object element;
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;
A is described first fluorescence signal;
F is described scaling results.
Above-mentioned instead of tradition for atomic fluorescence spectrometer background deduction method and utilize hydride generation method to make The process of the corresponding hydride of tested Element generation, can effectively eliminate in atomization process produced Anaclasis is disturbed, and has the good suitability.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of atomic fluorescence spectrometer background deduction method of the present invention;
Fig. 2 is that the signal strength values of the fluorescence signal according to the generation of the inventive method sample becomes in time Change schematic diagram.
Wherein, Fig. 2 a is the fluorescence letter produced under object element light source according to the inventive method sample Number signal strength values change over schematic diagram;
Fig. 2 b is the letter of the fluorescence signal produced under button background light source according to the inventive method sample Number intensity level changes over schematic diagram;
Fig. 3 is to illustrate the electric control signal of object element light source and button background light source according to the inventive method Figure;
Fig. 4 is the knot that the present invention uses the atomic fluorescence spectrometer of atomic fluorescence spectrometer background deduction method Structure schematic diagram.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention of greater clarity, below in conjunction with being embodied as Mode referring to the drawings, the present invention is described in more detail.It should be understood that these describe simply example Property, and it is not intended to limit the scope of the present invention.Additionally, in the following description, eliminate known knot Structure and the description of technology, to avoid unnecessarily obscuring idea of the invention.
The present invention can be used in flame method atomic fluorescence spectrometer, it is also possible to is used in hydrogenation atomic fluorescence spectrophotometry Instrument.
First embodiment
Fig. 1 is the schematic flow sheet of atomic fluorescence spectrometer background deduction method of the present invention.
As it is shown in figure 1, the background deduction method in atomic fluorescence spectrometer of the present invention comprises the following steps:
Step 102, is tested sample by object element light source, obtains the first fluorescence signal.
Object element light source uses the high-strength hollow cathode fluorescent lamp made by object element.According to test purpose Difference, object element light source changes the most accordingly.Such as, whether sample to be tested contains Certain element (i.e. the object element of this test), then use the high intensity hollow cathode made by this element Lamp is as object element light source.More specifically, whether sample to be tested contains arsenic element, then adopts With the high-strength hollow cathode fluorescent lamp made by arsenic as object element light source.
Element included in sample divides from the easiest atomizing angle, is divided into Easily by atomizing element and be difficult to by atomizing element, wherein, object element belongs to easily by atomization, It is difficult to be included interference element by atomizing element.In prior art, interference element includes aluminium element, calcium Element etc..
Described interference element is easily combined the short grained element generating oxide with oxygen, due to the oxidation produced The little granule of thing can produce refraction fluorescence signal, described refraction fluorescence signal and mesh to the light of object element light source Fluorescence signal produced by mark element overlaps, and is detected by photomultiplier tube, and then testing result is produced Raw error.
With a concrete example 1, this step is described below.
Choosing a sample C, the element comprised in this sample C includes: arsenic, lead, bismuth, Aluminum.
Test target is: test the content of arsenic element in described sample C.
From test target, the object element of this test is arsenic element, therefore selects made by arsenic High-strength hollow cathode fluorescent lamp is as object element light source.Owing to aluminium element is difficult to by atomization, therefore this The interference element of test is aluminium element.
In atomic fluorescence spectrometer, (high intensity made by arsenic is empty to light current object element light source Heart cathode modulation) the atomization region of sample C is tested, in sample C, arsenic element is subject to Current object element light source excited generation fluorescence signal, lead, bismuth these easily by atomizing element Will not be excited by current object element light source, although aluminium element also will not be by current object element light Source is excited, but, owing to aluminium element is difficult to atomization, can combine with oxygen and produce the little granule of oxide, The little granule of this oxide can produce refraction fluorescence signal, described refraction to the light of current object element light source Fluorescence signal produced by fluorescence signal and arsenic element overlaps, by the photomultiplier tube of atomic fluorescence spectrometer Being detected, the fluorescence signal (the i.e. first fluorescence signal) that therefore testing result obtains, for described sample The superposed signal of fluorescence signal produced by middle object element (arsenic element) and interference element (aluminium element).
Step 104, is tested described sample by button background light source, obtains the second fluorescence letter Number.
In this step, the sample that button background light source is tested is by object element light source in step 102 The same a sample tested.
Button background light source uses the high-strength hollow cathode fluorescent lamp made by element not contained in sample. One of ordinary skill in the art, when testing sample, estimate in sample according to the source of sample May not contain or element that content is the lowest, therefore use the high-strength hollow cathode fluorescent lamp that this element is made As button background light source.
In the fields such as the food of prior art, environmental protection, medicine, disease control, in sample with little or no Containing precious metal element, therefore, when testing the sample in the fields such as food, environmental protection, medicine, disease control, The general high-strength hollow cathode fluorescent lamp selecting precious metal element to make is as button background light source.Wherein, your gold Belong to and include the elements such as gold element, platinum element, palladium element.But in the samples such as mining industry field often Occur, in the field of precious metal element, selecting the high-strength hollow cathode fluorescent lamp that other elements are made as buckle back Scape light source.Such as, the gold element content in a sample of test, then use the high intensity that cobalt element is made Hollow cathode lamp is as buckleing background light source.
This step is illustrated below as a example by the example 1 of step 102.
In atomic fluorescence spectrometer, (high intensity made by gold is hollow to light current button background light source Cathode modulation) the atomization region of sample C is tested, owing to not containing gold in sample C Element, therefore, in sample C, only aluminium element and the oxygen combination generation little granule of oxide can be to currently Object element light source light produce refraction fluorescence signal, described refraction fluorescence signal is by atomic fluorescence spectrophotometry The photomultiplier tube of instrument is detected, and therefore, the fluorescence signal that the testing result of this step 102 obtains is (i.e. First fluorescence signal), fluorescence signal produced by interference element (aluminium element) in described sample.
Step 106, carries out making difference operation by described first fluorescence signal and the second fluorescence signal, obtains institute State the fluorescence signal of object element.
When the little granule of the oxide of interference element is being irradiated by the irradiation of object element light source and button background light source Time produced fluorescence signal intensity level consistent on the premise of, by the signal strength values of the first fluorescence signal Deduct the signal strength values of the second fluorescence signal, obtain the signal intensity of the fluorescence signal that object element produces Value.
Fig. 2 is that the signal strength values of the fluorescence signal according to the generation of the inventive method sample becomes in time Change schematic diagram.
Wherein, Fig. 2 a is the fluorescence letter produced under object element light source according to the inventive method sample Number signal strength values change over schematic diagram.
Fig. 2 b is the letter of the fluorescence signal produced under button background light source according to the inventive method sample Number intensity level changes over schematic diagram.
As shown in Figure 2 a, when object element light source igniting, the signal that photomultiplier tube is detected is first The fluorescence signal of fluorescence signal, i.e. object element and the superposed signal of the fluorescence signal of interference element.
As shown in Figure 2 b, when buckle back scape light source igniting, the signal that photomultiplier tube is detected is second glimmering The fluorescence signal of optical signal, i.e. interference element.
In the intensity level of fluorescence signal produced due to interference element in Fig. 2 a and Fig. 2 b, interference element produces The intensity level of fluorescence signal consistent, therefore, i.e..Therefore, by the signal of the first fluorescence signal in Fig. 2 a Intensity level deducts the signal strength values of the second fluorescence signal in Fig. 2 b, obtains the fluorescence letter that object element produces Number signal strength values.
Second embodiment
In the present embodiment, step 102 described in the first embodiment, by object element light Sample is tested by source, obtains the first fluorescence signal and includes:
Step 1021, carries out atomization by atomizer to described sample;
Step 1022, by the atomization region of sample described in object element light source activation;
Step 1023, detects described atomization region, obtains described first fluorescence signal.
Described step 104, is tested described sample by button background light source, obtains second glimmering Optical signal includes:
Step 1041, by the atomization region of sample described in buckle back scape light source activation;
Step 1042, detects described atomization region, obtains described second fluorescence signal.
In described step 1021, by the atomization region of sample described in object element light source activation After step, including:
After first scheduled time, extinguish object element light source;
After second scheduled time that object element light source extinguishes, light described button background light source.
Fig. 3 is to illustrate the electric control signal of object element light source and button background light source according to the inventive method Figure.
As it is shown on figure 3, in the whole test process to sample, object element light source and buckle back scape Light source intersection is lit, and object element light source is lit in the period tl, in time period T2 Button background light source is lit, and in time period T3, object element light source is lit, and detains in time period T4 Background light source is lit.
Illustrate that atomic fluorescence spectrometer background deduction method of the present invention is to detected sample with an instantiation below The test process of product.
After user is by the input equipment hit testing of computer, the control module of computer is to object element Light source sends enabled instruction, and object element light source is lit, and excites the atomization region of sample, and 100 After delicate, the fluorescence signal that computer starts photomultiplier tube to be detected is sampled, and obtains first Fluorescence signal.After sampling time sheet arrives, the control module of computer sends to object element light source and closes Instruction, object element light source extinguishes.Until object element light source extinguish after 100 delicate time, the control of computer Molding block sends enabled instruction to button background light source, and button background light source is lit, and excites the former of sample The region of sonization, after 100 is delicate, the fluorescence signal that computer starts photomultiplier tube to be detected enters Row sampling, obtained second fluorescence signal, the control module of computer is according to the formula (1) preset and public affairs First fluorescence signal and the second fluorescence signal are calculated by formula (2), obtain testing result.
3rd embodiment
Further, on the basis of the first embodiment, the present invention studies discovery, the oxygen of interference element The little granule of compound is produced fluorescence signal when being irradiated by object element light source and button background light source irradiates Intensity level be unanimously the most accidental situation, in most cases, the little granule of oxide of interference element exists When being irradiated by object element light source and detain background light source irradiation, the intensity level of produced fluorescence signal is not It is consistent, therefore before described first fluorescence signal and the second fluorescence signal are made difference operation, Need by formula (1), the signal strength values of the second fluorescence signal to be converted.
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;
F is, by button background light source, sample is tested the second obtained fluorescence signal;
A1 is, by object element light source, interference solution is tested obtained fluorescence signal;
A2 is, by object element light source, blank solution is tested obtained fluorescence signal;
B1 is, by button background light source, interference solution is tested obtained fluorescence signal;
B2 is, by button background light source, blank solution is tested obtained fluorescence signal.
After the scaling results F being obtained the second fluorescence signal by formula (1), right by formula (2) Described scaling results F and the first fluorescence signal A calculates, and obtains the fluorescence signal of described object element;
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;
A is described first fluorescence signal;
F is described scaling results.
It should be noted that use computer programming language that formula (1) and formula (2) are programmed into control In molding block, after photomultiplier tube detects the first fluorescence signal and the second fluorescence signal, by described First fluorescence signal and the second fluorescence signal are sent to computer, and it is glimmering to second that computer calls control module Optical signal converts, and by poor to scaling results and the first fluorescence signal, obtains final detection result.
Before formula (1) and formula (2) are programmed into the step of control module, also include using in fact Proved recipe formula obtains the parameters (A1, A2, B1, B2) of formula (1).
Particularly as follows:
Preparation interference solution, comprises interference element in described interference solution;
Preparation blank solution, does not include interference element and object element in described blank solution.
By object element light source, described interference solution is tested, obtain fluorescence signal A1;
By object element light source, described blank solution is tested, obtain fluorescence signal A2;
By button background light source, described interference solution is tested, obtain fluorescence signal B1;
By button background light source, described blank solution is tested, obtain fluorescence signal B2.
4th embodiment
Fig. 4 is the knot that the present invention uses the atomic fluorescence spectrometer of atomic fluorescence spectrometer background deduction method Structure schematic diagram.
As shown in Figure 4, a kind of atomic fluorescence spectrometer, including: atomizer 1, object element light source 2, Button background light source 3, detector 4 and computing module.
Atomizer 1, for carrying out atomization to sample.Element included in sample from The easiest atomizing angle divides, and is divided into easily by atomizing element and being difficult to by atom The element changed, wherein, object element belongs to easily by atomization, is difficult to be included interference by atomizing element Element.In prior art, interference element includes aluminium element, calcium constituent etc..Described interference element is easily and oxygen In conjunction with the short grained element of generation oxide, owing to the little granule of oxide produced can be to object element light The light in source produces refraction fluorescence signal, fluorescence signal produced by described refraction fluorescence signal and object element Overlap, detected by photomultiplier tube, and then make testing result produce error.
Object element light source 2, for exciting the atomization region of described sample.Object element light source Use the high-strength hollow cathode fluorescent lamp made by object element.Different according to test purpose, object element light Source changes the most accordingly.Such as, whether sample to be tested contains certain element (i.e. this The object element of test), then use the high-strength hollow cathode fluorescent lamp made by this element as object element light Source.More specifically, whether contain arsenic element in sample to be tested, then use made by arsenic is high-strength Degree hollow cathode lamp is as object element light source.
Button background light source 3, for exciting the atomization region of described sample.Button background light source uses The high-strength hollow cathode fluorescent lamp made by element not contained in sample.One of ordinary skill in the art exist During test sample, estimate according to the source of sample and sample may not contain or content pole Its low element, therefore uses the high-strength hollow cathode fluorescent lamp that this element is made as button background light source.? In the fields such as the food of prior art, environmental protection, medicine, disease control, with little or no containing expensive in sample Metallic element, therefore, when testing the sample in the fields such as food, environmental protection, medicine, disease control, typically selects The high-strength hollow cathode fluorescent lamp made with precious metal element is as button background light source.Wherein, noble metal includes The elements such as gold element, platinum element, palladium element.But often occur expensive in the samples such as mining industry field In the field of metallic element, select the high-strength hollow cathode fluorescent lamp that other elements are made as button background light source. Such as, the gold element content in a sample of test, then use the high intensity hollow cathode that cobalt element is made Lamp is as buckleing background light source.
Detector 4, for the atomization district when object element light source is lit, to described sample Territory is detected, and obtains the first fluorescence signal;It is additionally operable to when buckle back scape light source light source is lit, to institute The atomization region stating sample is detected, and obtains the second fluorescence signal.Wherein, described first glimmering Optical signal is the superposition letter of fluorescence signal produced by the object element in described sample and interference element Number;Described second fluorescence signal value is the fluorescence signal of the interference element in described sample.Computing mould Block, for described first fluorescence signal and the second fluorescence signal are made difference operation, obtains described target The fluorescence signal of element.Photomultiplier detector selected by described detector.
Control module 5, for sending enabled instruction to object element light source 2 and button background light source 3 respectively, Shown object element light source 2 and button background light source 3 are lit after receiving enabled instruction.
Computing module, for described first fluorescence signal and the second fluorescence signal are made difference operation, Fluorescence signal to described object element.When the little granule of the oxide of interference element is by object element light Source is irradiated on the premise of when irradiating with button background light source, the intensity level of produced fluorescence signal is consistent, by the The signal strength values of one fluorescence signal deducts the signal strength values of the second fluorescence signal, obtains object element and produces The signal strength values of raw fluorescence signal.
5th embodiment
On the basis of the 4th embodiment, in described atomic fluorescence spectrometer, control module 5 is also used In, after first scheduled time that object element light source point is lit, send out to described object element light source Send extinguishing instruction, to extinguish described object element light source;It is additionally operable to second extinguished at object element light source After the scheduled time, send enabled instruction to described button background light source, to light described button background light source.
The present embodiment is illustrated below as a example by example 1 in the first embodiment.
Sample C is sent into atomizer 1, and atomizer 1 starts, and carries out former to sample C Sonization, obtains the atomization region (i.e. the flame region part of test sample product C) of sample C.
Control module 5 sends the first enabled instruction to object element light source 2, and object element light source 2 receives Sending light beam after described first enabled instruction, the atomization region of this beam alignment sample C is with right In object element excite.Object element (for arsenic element in example 1) in sample C is subject to Current object element light source excited generation fluorescence signal, and lead in test sample product C, bismuth these are easy Will not be excited by current object element light source by atomizing element, although aluminium element also will not be worked as Front object element light source is excited, but, owing to aluminium element is difficult to atomization, can combine with oxygen and produce The little granule of oxide, the little granule of this oxide can produce refraction fluorescence to the light of current object element light source Signal, fluorescence signal produced by described refraction fluorescence signal and arsenic element overlaps, by atomic fluorescence spectrophotometry The photomultiplier tube of instrument is detected, the fluorescence signal (the i.e. first fluorescence signal) that therefore testing result obtains, Fluorescence produced by object element (arsenic element) in described sample and interference element (aluminium element) The superposed signal of signal.
After the scheduled time that object element light source 2 is lit, control module 5 is to button background light source 3 Sending the second enabled instruction, button background light source 3 sends light beam after receiving described second enabled instruction, should The atomization region of beam alignment sample C.Owing to sample C not containing gold element, therefore, In sample C, only aluminium element and the oxygen combination generation little granule of oxide can be to current object element light The light in source produces refraction fluorescence signal, and described refraction fluorescence signal is by the photomultiplier transit of atomic fluorescence spectrometer Pipe is detected, therefore, and fluorescence signal (the i.e. first fluorescence obtained after object element light source 2 is lit Signal), fluorescence signal produced by interference element (aluminium element) in described sample.
6th embodiment
On the basis of the first embodiment, the present invention studies discovery, the little granule of oxide of interference element The intensity level one of produced fluorescence signal when being irradiated by object element light source and button background light source irradiates Causing the most accidental situation, in most cases, the little granule of oxide of interference element is by target element It is not consistent that element light source irradiates the intensity level of produced fluorescence signal when irradiating with button background light source, Therefore, the 6th embodiment is on the basis of the 4th embodiment, and described computing module includes: the first meter Calculate unit and the second computing unit.
First computing unit, for being converted described second fluorescence signal by formula (1), is changed Calculate result.
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;F is to test sample obtained by button background light source Second fluorescence signal;A1 is by object element light source, interference solution to be tested obtained fluorescence to believe Number;A2 is, by object element light source, blank solution is tested obtained fluorescence signal;B1 is logical Cross button background light source and interference solution is tested obtained fluorescence signal;B2 is by button background light source Blank solution is tested obtained fluorescence signal.
Second computing unit, for carrying out described scaling results and the first fluorescence signal by formula (2) Calculate, obtain the fluorescence signal of described object element.
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;A is described first fluorescence signal;F is described conversion Result.
It should be appreciated that the above-mentioned detailed description of the invention of the present invention is used only for exemplary illustration or explanation The principle of the present invention, and be not construed as limiting the invention.Therefore, without departing from the present invention spirit and Any modification, equivalent substitution and improvement etc. done in the case of scope, should be included in the guarantor of the present invention Within the scope of protecting.Additionally, claims of the present invention be intended to fall into scope and Whole in the equivalents on border or this scope and border change and modifications example.

Claims (10)

1. the background deduction method of an atomic fluorescence spectrometer, it is characterised in that including:
By object element light source, sample is tested, obtain the first fluorescence signal;Described One fluorescence signal is fluorescence signal produced by object element and interference element in described sample Superposed signal;
By button background light source, described sample is tested, obtain the second fluorescence signal;Described Second fluorescence signal value is fluorescence signal produced by interference element in described sample;
Carry out making difference operation by described first fluorescence signal and the second fluorescence signal, obtain described target element The fluorescence signal of element.
Method the most according to claim 1, it is characterised in that described by object element light Sample is tested by source, and the step obtaining the first fluorescence signal includes:
By atomizer, described sample is carried out atomization;
Atomization region by sample described in object element light source activation;
Described atomization region is detected, obtains described first fluorescence signal.
Method the most according to claim 2, it is characterised in that described by button background light source Testing described sample, the step obtaining the second fluorescence signal includes:
Atomization region by sample described in buckle back scape light source activation;
Described atomization region is detected, obtains described second fluorescence signal.
4. according to the method described in any one of claim 2-3, it is characterised in that pass through described After the step in the atomization region of sample described in object element light source activation, including:
After first scheduled time, extinguish object element light source;
After second scheduled time that object element light source extinguishes, light described button background light source.
5. according to the method described in any one of claim 1-4, it is characterised in that pass through described Sample is tested by button background light source, after obtaining the step of the second fluorescence signal, also includes:
By formula (1), described second fluorescence signal is converted, obtain scaling results;
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;
F is, by button background light source, sample is tested the second obtained fluorescence signal;
A1 is, by object element light source, interference solution is tested obtained fluorescence signal;
A2 is, by object element light source, blank solution is tested obtained fluorescence signal;
B1 is, by button background light source, interference solution is tested obtained fluorescence signal;
B2 is, by button background light source, blank solution is tested obtained fluorescence signal.
Method the most according to claim 5, it is characterised in that described by described first fluorescence Signal and the second fluorescence signal carry out making difference operation, obtain the step bag of the fluorescence signal of object element Include:
By formula (2), described scaling results and the first fluorescence signal are calculated, obtain described The fluorescence signal of object element;
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;
A is described first fluorescence signal;
F is described scaling results.
7. according to the method described in claim 1-4,6 any one, it is characterised in that described buckle back Scape light source uses the high-strength hollow cathode fluorescent lamp made by element not contained in sample.
8. an atomic fluorescence spectrometer, it is characterised in that use any one of claim 1-7 institute The method stated, including:
Atomizer, for carrying out atomization to sample;
Object element light source, for exciting the atomization region of described sample;
Button background light source, for exciting the atomization region of described sample;
Detector, for the atomization district when object element light source is lit, to described sample Territory is detected, and obtains the first fluorescence signal;It is additionally operable to when buckle back scape light source light source is lit, right The atomization region of described sample is detected, and obtains the second fluorescence signal;
Described first fluorescence signal is produced by the object element in described sample and interference element The superposed signal of fluorescence signal;Described second fluorescence signal value is the chaff element in described sample The fluorescence signal of element;
Computing module, for described first fluorescence signal and the second fluorescence signal are made difference operation, Obtain the fluorescence signal of described object element.
A kind of atomic fluorescence spectrometer the most according to claim 8, it is characterised in that also wrap Include control module, after first scheduled time that object element light source point is lit, to described target Element light source sends and extinguishes instruction, to extinguish described object element light source;It is additionally operable at object element light After second scheduled time that source is extinguished, send enabled instruction to described button background light source, to light State button background light source.
A kind of atomic fluorescence spectrometer the most according to claim 9, it is characterised in that described Computing module includes: the first computing unit and the second computing unit;
Described first computing unit, for changing described second fluorescence signal by formula (1) Calculate, obtain scaling results;
F=A1-A2/B1-B2 (f-B2) formula (1);
Wherein, F is scaling results;
F is, by button background light source, sample is tested the second obtained fluorescence signal;
A1 is, by object element light source, interference solution is tested obtained fluorescence signal;
A2 is, by object element light source, blank solution is tested obtained fluorescence signal;
B1 is, by button background light source, interference solution is tested obtained fluorescence signal;
B2 is, by button background light source, blank solution is tested obtained fluorescence signal;
Described second computing unit, is used for by formula (2) described scaling results and the first fluorescence Signal calculates, and obtains the fluorescence signal of described object element;
P=A F formula (2);
Wherein, P is the fluorescence signal of object element;
A is described first fluorescence signal;
F is described scaling results.
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