CN106018368A - Atomic fluorescence spectrophotometer and working method thereof - Google Patents

Atomic fluorescence spectrophotometer and working method thereof Download PDF

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Publication number
CN106018368A
CN106018368A CN201610509347.8A CN201610509347A CN106018368A CN 106018368 A CN106018368 A CN 106018368A CN 201610509347 A CN201610509347 A CN 201610509347A CN 106018368 A CN106018368 A CN 106018368A
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CN
China
Prior art keywords
light
fluorescence spectrophotometer
atomic fluorescence
detector
emergent light
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610509347.8A
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Chinese (zh)
Inventor
曹育联
刘旻
寿淼钧
裴晓华
赵富荣
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BEIJING JITIAN INSTRUMENT Co Ltd
Beijing Titan Instruments Co Ltd
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BEIJING JITIAN INSTRUMENT Co Ltd
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Priority to CN201610509347.8A priority Critical patent/CN106018368A/en
Publication of CN106018368A publication Critical patent/CN106018368A/en
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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
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • 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
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • 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

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optics & Photonics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention provides an atomic fluorescence spectrophotometer and a working method thereof. The atomic fluorescence spectrophotometer comprises a light path system, an atomizer and an analytic system. The light path system comprises M excitation light sources and a detector, wherein M is not smaller than 2 and is an element of a set Z, characteristic spectral lines of emergent light of the M excitation light sources separately correspond to elements to be detected; the emergent light irradiates the same area of flame in the atomizer, and the emergent light entering the same area is not located in the same cross section vertical to the central axis of the flame; the detector is used for converting fluorescence, of which included angles with the emergent light entering the same area are acute angles or right angles, into electric signals and transmitting the electric signals to the analytic system. The atomic fluorescence spectrophotometer and the working method thereof have the advantages of many detected elements, simple structure, low cost and the like.

Description

Atomic fluorescence spectrophotometer and method of work thereof
Technical field
The present invention relates to fluorescence spectrum, particularly to atomic fluorescence spectrophotometer and method of work thereof.
Background technology
The operation principle of atomic fluorescence spectrophotometer is: utilizes potassium borohydride or sodium borohydride as reducing agent, incites somebody to action Element reduction to be analyzed in sample solution is volatility covalency gaseous hydride (or atom vapor), then borrows Help carrier gas to be conducted into atomizer, form ground state atom at Ar-H flame Atom.Element to be measured Flame is irradiated in the characteristic spectral line line focus that excitation source (generally hollow cathode modulation) is launched, and excites and wherein treats The atom surveying element produces fluorescence.Photomultiplier tube receives fluorescence and is converted to the signal of telecommunication, integrated amplification etc. Process, data handling system obtain being directly proportional to concentration of element in sample measurement result.
When in sample solution containing two kinds or during above element to be measured, atomic fluorescence spectrophotometer uses multichannel Measurement pattern, uses the excitation source identical with number of active lanes (i.e. the number of element to be measured in sample solution) High frequency time-division illumination flame, and make photomultiplier tube read each channel signal respectively by frequency corresponding with light source Value.Manifold Light Way is generally in the form of what the mode using light path to rotate tiling in the horizontal plane realized, many The exciting light of individual passage press certain angle (as 45 degree, 45 degree, 90 degree ,-90 degree, 135 degree ,-135 spend) Incident flame, then receives fluorescence, the exciting light of all passages and the final fluorescence received all 0 degree of position On the cross section of flame kernel.Tile mode has a following shortcoming:
1. relevant with fluorescence reception angle due to the intensity of fluorescence, several the inconsistent of channel reception angle cause Each passage consistency is poor, and the channel fluorescence efficiency of deviation 90 degree reception fluorescence drastically reduces;
2., time owing to receiving fluorescence more than 90 degree (such as+135 degree and-135 degree), fluorescence can be by transmission light Severe jamming, therefore for ensureing that veiling glare is less, receives fluorescence in general employing 90 degree;Owing to space limits, The number of channels can placed in 90 degree is usually no more than 4;
3. relatively big due to hollow cathode lamp drift, particularly mercury lamp, the drift of signal greatly have impact on instrument Stability and detection limit;
4. the lamp of multichannel fluorophotometer is that tiling is scattered mode, needs to change lamp from upward-acting door, changes fiber crops Tired.
Summary of the invention
In order to solve the deficiency in above-mentioned prior art, the invention provides a kind of detection efficiency height, fortune The atomic fluorescence spectrophotometer that line stabilization, interchannel interference are few.
It is an object of the invention to be achieved through the following technical solutions:
A kind of atomic fluorescence spectrophotometer, described atomic fluorescence spectrophotometer includes light path system, atomizer and divides Analysis system;Described light path system includes:
M excitation source, M >=2, and M ∈ Z, the characteristic spectral line of the emergent light of described M excitation source Correspond respectively to element to be measured;Described emergent light is irradiated to the same area in atomizer flame, incident It is in the same cross section being perpendicular to flame kernel axis to emergent light during described the same area is non-;
Detector, described detector by the angle incided between the emergent light of described the same area be acute angle or The fluorescence at right angle is converted to the signal of telecommunication, and is sent to described analysis system.
According to above-mentioned atomic fluorescence spectrophotometer, it is preferable that incide described M during described the same area The emergent light of excitation source is in same plane, and this plane is zero with the angle of the central axis of described flame Or acute angle.
According to above-mentioned atomic fluorescence spectrophotometer, alternatively, described light path system farther includes:
M beam splitting module, described beam splitting module is for being divided into by the light that each excitation source sends respectively Penetrate light, reference light.
According to above-mentioned atomic fluorescence spectrophotometer, alternatively, described light path system farther includes:
Closing bundle module, described conjunction bundle module is combined for M is restrainted reference light.
According to above-mentioned atomic fluorescence spectrophotometer, alternatively, described bundle module of closing includes:
Transmission medium, the outfan of described transmission medium together;Close the reference light after bundle and be coupled into institute State some transmission medium, received by described detector or the detector that separately sets afterwards, the detector separately set defeated Go out end and connect described analysis system.
According to above-mentioned atomic fluorescence spectrophotometer, it is preferable that the normal of the receiving plane of described detector is with incident Angle between emergent light during described the same area is acute angle or right angle.
According to above-mentioned atomic fluorescence spectrophotometer, alternatively, described light path system farther includes:
Handover module, described handover module is for being selectively transmitted to described the same area by described emergent light.
Present invention also offers the method for work applying above-mentioned atomic fluorescence spectrophotometer.This goal of the invention is to pass through Techniques below scheme realizes:
According to the method for work of above-mentioned atomic fluorescence spectrophotometer, described method of work comprises the following steps:
(A1) emergent light that excitation source sends is irradiated in flame;
(A2) element to be measured forms ground state atom in flame, and ground state atom absorbs described emergent light and is excited, And discharge fluorescence;
(A3) detector receives described fluorescence, knows the content of element to be measured in sample after analyzing.
Compared with prior art, the device have the advantages that into:
The fluorescence reception direction of the most all passages and the angle of the exciting light inciding flame are that right angle is (or sharp Angle), direction fluorescence is the strongest, and the veiling glare impact of the transmission light of stimulated luminescence is minimum;
2. can realize 4 or above passage is tested simultaneously, meet the demand of client's high efficiency test;
The most all passages are all parallel passages, can guarantee that passage consistency is good, and the interference between passage is little;
The most each passage has reference signal collection for deducting drift, and stability of instrument and detection are greatly improved Limit, is also greatly shortened the preheating time required for instrument simultaneously;
The excitation source of the most all passages is respectively mounted all on the panel of instrument, and structure design is simple, replacing side Just.
Accompanying drawing explanation
Referring to the drawings, the disclosure will be easier to understand.Skilled addressee readily understands that : these accompanying drawings are used only for illustrating technical scheme, and are not intended to the present invention's Protection domain is construed as limiting.In figure:
Fig. 1 is the structure diagram of the light path system of according to embodiments of the present invention 1.
Detailed description of the invention
Fig. 1 and following description describe the optional embodiment of the present invention with teaching those skilled in the art how Implement and reproduce the present invention.In order to instruct technical solution of the present invention, simplify or eliminated some conventional aspects. Those skilled in the art should understand that be derived from these embodiments modification or replace will be in the scope of the present invention In.Those skilled in the art should understand that following characteristics can combine to form the present invention in every way many Individual modification.Thus, the invention is not limited in following optional embodiment, and only by claim and they Equivalent limit.
Embodiment 1:
The atomic fluorescence spectrophotometer of the embodiment of the present invention, described atomic fluorescence spectrophotometer includes:
Sampling system, atomizer, analysis system, these are all the state of the art, at this no longer Repeat;
Fig. 1 schematically illustrates the structure diagram of the light path system of the embodiment of the present invention, as it is shown in figure 1, Described light path system includes:
M excitation source 1-4, such as hollow cathode lamp, M >=2, and M ∈ Z, going out of described M light source The characteristic spectral line penetrating light corresponds respectively to element to be measured;Described emergent light is irradiated in atomizer flame The same area, emergent light when inciding described the same area is non-to be in same being perpendicular to flame kernel axis Cross section in, the plane of central axis or center as described in being parallel to as described in emergent light is in same comprising In the plane of axis, or most emergent light is in this plane, and minority emergent light has less with this interplanar Angle, such as 3 degree, 5 degree, 10 degree;Or emergent light is in same plane, this plane and flame kernel The angle of axis is acute angle, such as 3 degree, and 5 degree, 10 degree;
M transflection mirror 5-8, as center has the lens of through hole, ratio transflection mirror etc., described transflection mirror is arranged Going out in light light path at excitation source, thus separate emergent light, reference light;
Closing bundle module, described conjunction bundle module uses M group transmission medium 11-14, such as fibre bundle, is used for restrainting M Transmission light is combined, the outfan of transmission medium together 19;The input row of each group of transmission medium It is classified as circle;
Detector 22, such as photomultiplier tube, an only detector by with the emergent light being transferred in flame Between the fluorescence that angle is acute angle or right angle be converted to the signal of telecommunication: the normal of the receiving plane of detector be transferred to The angle between emergent light in flame is acute angle or right angle, and is sent to described analysis system;
Reflecting mirror 21, this reflecting mirror is movably disposed on fluorescence light path, and described reference light output end exports Reference light reflected by described reflecting mirror, reflection light received by described detector;
Handover module, whether described handover module for controlling the unlatching of LASER Light Source, so that LASER Light Source Emergent light optionally inject the same area in the flame of atomizer.
The method of work of the above-mentioned atomic fluorescence spectrophotometer of the embodiment of the present invention, described method of work includes following Step:
(A1) by switching, it is irradiated in flame to the emergent light timesharing that excitation source sends;
(A2) element to be measured forms ground state atom in flame, and ground state atom absorbs described emergent light and is excited, And discharge fluorescence;
(A3) moving into described reflecting mirror, reference light is reflected by a reflector, and is received by a detector afterwards, thus For control comparisons, to correct drift;
Removing described reflecting mirror, detector receives described fluorescence, knows element to be measured in sample after analyzing Content.
Embodiment 2:
The atomic fluorescence spectrophotometer of the embodiment of the present invention and method of work thereof, as different from Example 1:
Close bundle module to include: transflection mirror, reflecting mirror, utilize reflecting mirror by the reference luminous reflectance that separates to transflection Mirror, thus realize the conjunction bundle of reference light.
Embodiment 3:
The atomic fluorescence spectrophotometer of the embodiment of the present invention, as different from Example 1:
Reflecting mirror replaces with transflection mirror, block body (or chopper), and described transflection mirror is fixed on described fluorescence light path On, reference light incides on detector after being reflected by transflection mirror, and fluorescence is connect by detector through described transflection mirror Receive;Block body is movably disposed in reference light light path.
When block body is removed, detector gathers fluorescent and the reference light that flame kernel comes simultaneously;Work as gear When body is in the light, only gather fluorescent, fluorescent and reference optical information can be obtained by software processes, By software processes reference light, fluorescent is carried out detain drift to process.
Embodiment 4:
The atomic fluorescence spectrophotometer of the embodiment of the present invention, as different from Example 1:
Using two detectors, one is used for receiving fluorescence, and another is used for receiving the output of reference light output end Reference light (without reflexing to the only reflecting mirror of detector receiving fluorescence), the signal of telecommunication of output Send analysis system.
Embodiment 5:
The atomic fluorescence spectrophotometer of the embodiment of the present invention and method of work thereof, as different from Example 1:
Whether handover module no longer controls the unlatching of excitation source, but goes out light light path at each excitation source On removable block body is set, when needing the emergent light of this excitation source, reference light, block body is placed in other Going out to be in the light in light light path of excitation source, so that the emergent light of excitation source is optionally irradiated to flame In.

Claims (8)

1. an atomic fluorescence spectrophotometer, described atomic fluorescence spectrophotometer include light path system, atomizer and Analysis system;It is characterized in that: described light path system includes:
M excitation source, M >=2, and M ∈ Z, the characteristic spectral line of the emergent light of described M excitation source Correspond respectively to element to be measured;Described emergent light is irradiated to the same area in atomizer flame, incident It is in the same cross section being perpendicular to flame kernel axis to emergent light during described the same area is non-;
Detector, described detector by the angle incided between the emergent light of described the same area be acute angle or The fluorescence at right angle is converted to the signal of telecommunication, and is sent to described analysis system.
Atomic fluorescence spectrophotometer the most according to claim 1, it is characterised in that: incide described same The emergent light of described M excitation source during region is in same plane, in this plane and described flame The angle of mandrel line is zero or acute angle.
Atomic fluorescence spectrophotometer the most according to claim 1, it is characterised in that: described light path system enters One step includes:
M beam splitting module, described beam splitting module is for being divided into by the light that each excitation source sends respectively Penetrate light, reference light.
Atomic fluorescence spectrophotometer the most according to claim 3, it is characterised in that: described light path system enters One step includes:
Closing bundle module, described conjunction bundle module is combined for M is restrainted reference light.
Atomic fluorescence spectrophotometer the most according to claim 4, it is characterised in that: described conjunction restraints module bag Include:
Transmission medium, the outfan of described transmission medium together;Close the reference light after bundle and be coupled into institute State some transmission medium, received by described detector or the detector that separately sets afterwards, the detector separately set defeated Go out end and connect described analysis system.
Atomic fluorescence spectrophotometer the most according to claim 1, it is characterised in that: connecing of described detector Angle between the normal in receipts face and emergent light when inciding described the same area is acute angle or right angle.
Atomic fluorescence spectrophotometer the most according to claim 1, it is characterised in that: described light path system enters One step includes:
Handover module, described handover module is for being selectively transmitted to described the same area by described emergent light.
8. according to the method for work of the arbitrary described atomic fluorescence spectrophotometer of claim 1-7, described work side Method comprises the following steps:
(A1) emergent light that excitation source sends is irradiated in flame;
(A2) element to be measured forms ground state atom in flame, and ground state atom absorbs described emergent light and is excited, And discharge fluorescence;
(A3) detector receives described fluorescence, knows the content of element to be measured in sample after analyzing.
CN201610509347.8A 2016-06-30 2016-06-30 Atomic fluorescence spectrophotometer and working method thereof Pending CN106018368A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN109342344A (en) * 2018-11-30 2019-02-15 南京工程学院 A kind of the non-calibrating device and its measuring method of mercury analyzer
CN109342344B (en) * 2018-11-30 2021-02-02 南京工程学院 Calibration-free device of mercury analyzer and determination method thereof

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Application publication date: 20161012