CN1858580A - Multipath merge spectrum chemical analysis method and its instrument - Google Patents
Multipath merge spectrum chemical analysis method and its instrument Download PDFInfo
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- CN1858580A CN1858580A CN 200510067965 CN200510067965A CN1858580A CN 1858580 A CN1858580 A CN 1858580A CN 200510067965 CN200510067965 CN 200510067965 CN 200510067965 A CN200510067965 A CN 200510067965A CN 1858580 A CN1858580 A CN 1858580A
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Abstract
This invention provides a multi-channel spectrum-merging chemical analysis method and an instrument, in which, the method includes: same light sources of two or more than two channels radiate a tested sample and test a same element at the same time in a multi-channel spectrometer to get the density data of said element, which is equal to overlap the strength of multiple light sources and increase the radiation strength of single light source so as to strengthen the strength of light sources to increase the sensitivity of the instrument and check-out limit.
Description
Technical field
The present invention relates to the instrumental analysis field, particularly a kind of spectral class analytical approach and instrument.
Background technology
At present, the spectral class analytical instrument is widely used in the quantitative measurement of element.The spectral class analytical instrument is made up of excitation source, atomizer and three major parts of detecting device.Atomic fluorescence spectrometer is wherein a kind of spectral class analytical instrument commonly used.The basic functional principle of its whole test process is: each element in the specimen forms corresponding hydride after reacting, mix with hydrogen and carrier gas, after entering atomizer realization atomization, send specific wavelength atomic fluorescence signal under the irradiation of excitation source, detecting device is collected this fluorescence signal and is obtained the concentration data of element according to the characteristic that this fluorescence signal intensity is directly proportional with concentration of element.
According to the number of atomic fluorescence spectrometer passage, atomic fluorescence spectrometer can be divided into single channel atomic fluorescence spectrometer and hyperchannel atomic fluorescence spectrometer.Owing to have the advantage that can analyze multiple element simultaneously, the hyperchannel atomic fluorescence spectrometer is widely used in fields such as environmental protection, health, food, medicine, metallurgy, geologic prospecting.Why the hyperchannel atomic fluorescence spectrometer is different from the single channel atomic fluorescence spectrometer, can analyze multiple element simultaneously, its ultimate principle is: the hyperchannel atomic fluorescence spectrometer disposes several passages, when measuring several different elements at the same time, the elements corresponding illuminator is housed on several passages.Under the control of signal generator, in a certain moment in a test period, have only a unique illuminator to be excited.The steam of the atom that produced in the atomizer this moment can send a characteristic fluorescence signal under the radiation of this feature light source.Owing in atomic vapour, have a plurality of tested elemental compositions, and each tested element is only radiosensitive to own corresponding characteristic wavelength.Therefore, in a test period, each illuminator that order is lighted produces the fluorescence signal of the pairing varying strength of each tested element, and the fluorescence signal of this sequence is detected and convert to electric signal by photoelectric detector.Mix electric signal from this group of photoelectric detector output and be separated into the signal of representing each tested element, varying strength.Finally, to data processing such as the collection of institute's input signal, conversions, obtain the concentration results of each tested element by signal processing unit simultaneously.
Excitation source tool in the spectrochemical analysis method plays a very important role, and its intensity directly influences the sensitivity of method of testing, so light source is the important component part of spectral class analytical instrument.Existing multi-channel spectral alanysis instrument, at the same time during the contained multiple element of analytic sample, single passage is corresponding measures an element, and each interchannel is separate.Like this, the sensitivity of instrument detection device is subjected to the restriction of single source intensity.
In order to increase the intensity of single source, the apparatus manufacturers light source technology that developed on a large scale greatly.Aspect atomic fluorescence spectrometer, light source to hollow cathode lamp, develops into the high strength hollow cathode lamp of present stage domestic manufacturer employing from initial electrodeless discharge lamp at last.Publishing house of Jilin University publish by James D.Ingle, in the domestic compiling books " spectrochemical analysis " that people such as Jr. write the high strength hollow cathode lamp has been done detailed introduction.The high strength hollow cathode lamp is compared with electrodeless discharge lamp, and the intensity of light source is greatly improved.At present, adopting the atomic fluorescence spectrometer of high strength hollow cathode lamp source can detection elements concentration be 10
-9～10
-12The sample of g/ml.But along with the raising of people's living standard and the development of environmental protection cause, the environmental monitoring of department system such as ocean, fishery, agricultural, and with industries such as the closely-related water quality of people, soil pollution, food, mineral water, medicine, medical treatment harmful poisonous element is detected the detection limit of instrument is had higher requirement, requirement detection elements concentration exactly is 10
-10～10
-13The small concentration sample of g/ml.Measurement for this small concentration sample, the single source intensity of existing high strength hollow cathode lamp source instrument still is apparent not enough, accuracy and precision are poor when causing testing small concentration sample or test small concentration sample, can not obtain gratifying result.
Light source technology is restricting the further raising of instrument test sensitivity, brings difficulty for the sample of test small concentration.At present, when test small concentration sample, take other chemical treatment method such as enrichment usually, make it reach the scope that instrument can accurately be measured to increase the concentration of element to be measured.But this chemical treatment method complex steps wastes time and energy, and can cause the loss of composition to be measured in the sample, can't guarantee the test precision of instrument, thereby has influenced the reliability and the accuracy of experimental data.
Summary of the invention
One of purpose of the present invention is the shortcoming of accuracy and precision difference when overcoming existing spectral class analytical technology and can not test small concentration sample or test small concentration sample, and a kind of multipath merge spectrum chemical analysis method is provided.
Two of purpose of the present invention provides a kind of hyperchannel of above-mentioned analytical approach of realizing and merges the spectral class analytical instrument.
The multipath merge spectrum chemical analysis method of one of the object of the invention is achieved in that
Multipath merge spectrum chemical analysis method of the present invention shines sample simultaneously by the same light source that makes two or more passages in the multi-channel spectrometer based, be equivalent to these same light source are merged into a light source irradiation sample behind the intensity of light source superposition, test identity element jointly, obtain the concentration data of this element.
During concrete enforcement, the preferred hyperchannel of multipath merge spectrum chemical analysis method of the present invention merges the atomic fluorescence spectrometer chemical analysis method.
It is as follows that two the hyperchannel of the object of the invention merges spectral class analytical instrument implementation:
The composition that the hyperchannel of the above-mentioned multipath merge spectrum chemical analysis method of realization of the present invention merges the spectral class analytical instrument comprises:
Signal generator is used for the irradiation sequence and the irradiation time of the illuminator of each passage are controlled, and makes that the irradiation sequential of the same light source lamp that is equipped with in different passages is identical; In concrete the enforcement, above-mentioned signal generator can be signal trigger.And can adjust a little with the signal generator of general multi-channel spectral alanysis instrument and get final product;
The hyperchannel excitation source, in concrete the enforcement, above-mentioned hyperchannel excitation source can be the hyperchannel excitation source of routine;
Atomizer, in concrete the enforcement, above-mentioned atomizer can be the atomizer of routine;
Photomultiplier, in concrete the enforcement, above-mentioned photomultiplier can be the photomultiplier of routine;
Conventional amplifier;
Data acquisition unit, this unit carries out acquisition order to each channel data, keeps general-purpose chip LF1/2/398 and modulus conversion chip to constitute by data sampling;
The data computation unit, the light intensity data of the tested element of this unit handle input is converted to the concentration of tested element, and in concrete the enforcement, above-mentioned data computation unit can be the data computation unit of routine.
Wherein, the functional sequence of each ingredient of instrument is: under the control of signal generator, the atomic vapour of the illuminator of each passage to be produced in the predetermined sequential irradiated atoms device in the hyperchannel excitation source, produce light signal, after photomultiplier detection, the amplification of conventional amplifier, by data acquisition unit each channel data is carried out acquisition order again, after the data computation unit is converted to the light intensity data of the tested element of input the concentration of tested element.
During concrete enforcement, hyperchannel of the present invention merges the preferred hyperchannel of spectrometric instrument and merges atomic fluorescence spectrometer; The light signal of above-mentioned generation is a fluorescence signal.
Because the above-mentioned method and structure characteristics of the present invention, the present invention has following outstanding effect:
When 1, adopting merge channels technical measurement small concentration sample of the present invention, the same light source of two or more passages is shone sample simultaneously, be equivalent to the intensity of a plurality of light sources has been carried out superposition, equivalence has strengthened the radiation intensity of single source, increase the intensity of light source so greatly, improved the detection limit of instrument.And because the electrical noise of instrument does not increase, so improved signal to noise ratio (S/N ratio) simultaneously.Compare with the single channel technology, under the same terms, detection limit has obtained improving greatly, can guarantee high precision simultaneously.
When 2, adopting merge channels technical measurement small concentration sample of the present invention, can exempt other complex chemical treatment steps such as enrichment, not only save sample but also improved work efficiency.
Description of drawings
Fig. 1: four-way atomic fluorescence spectrometer structure principle chart
Fig. 2: each passage cathode modulation sequential synoptic diagram of common four-way atomic fluorescence spectrometer
Fig. 3: each passage cathode modulation sequential synoptic diagram in the four-way atomic fluorescence spectrometer that triple channel merges
Fig. 4: each passage cathode modulation sequential synoptic diagram in the four-way atomic fluorescence spectrometer of two group of two passage merging
Embodiment
Below, by embodiment and in conjunction with the accompanying drawings, further specify the technical scheme of method of the present invention and instrument, and the technique effect that reaches.But protection scope of the present invention is as the criterion with claims, is not subjected to
The restriction of embodiment.
Embodiment 1 uses arsenic and the tellurium element in the four-way merging atomic fluorescence spectrometer specimen that realizes multipath merge spectrum chemical analysis method;
Dispose serial arsenic tellurium mixed standard solution.In accompanying drawing 1, pack on A, B, the C-channel hollow cathode lamp of identical special-purpose arsenic excitation source, the D passage hollow cathode lamp of special-purpose tellurium excitation source of packing in the accompanying drawing 1.By signal generator 5 in the accompanying drawing 1, A in the control accompanying drawing 1, B, C, the lamp pulse sequential of D passage is shown in the accompanying drawing 3, be A in the accompanying drawing 1, B, the hollow cathode lamp of the identical arsenic excitation source of C-channel shines atomizer 4 in the accompanying drawing 1 simultaneously, the hollow cathode lamp of the tellurium excitation source of D passage shines atomizer 4 in the accompanying drawing 1 at interval subsequently in the accompanying drawing 1, being in the analyzed element arsenic of ground state and tellurium atom successively is subjected to the characteristic wavelength radiant rays and excites, send specific wavelength atomic fluorescence signal respectively, photomultiplier 3 detects in accompanying drawing 1, after data acquisition unit 1 order is finished collection in the accompanying drawing 1, by data computation unit 6, obtain by the element arsenic after the test fluorescence intensity conversion of element arsenic and tellurium and the concentration of tellurium.Relevant regulations according to instrument detection limit and precision mensuration, adopt four-way to merge atomic fluorescence spectrometer and test the series standard solution that above-mentioned arsenic tellurium mixes, drawing arsenic and tellurium as calculated detects and be limited to: arsenic: 0.006ng/ml, tellurium: 0.02ng/ml, precision is: arsenic: tellurium 0.9%: 0.9%.
Embodiment 2 uses arsenic and the tellurium element in the four-way merging atomic fluorescence spectrometer working sample of realizing multipath merge spectrum chemical analysis method;
Dispose serial arsenic tellurium mixed standard solution.In accompanying drawing 1, pack on A, the B passage hollow cathode lamp of identical special-purpose arsenic excitation source, the hollow cathode lamp of the identical special-purpose tellurium excitation source of in accompanying drawing 1, packing on C, the D passage.By signal generator 5 in the accompanying drawing 1, the lamp pulse sequential of A, B, C, D passage is shown in the accompanying drawing 4 in the control accompanying drawing 1, the hollow cathode lamp that is the special-purpose arsenic excitation source of A in the accompanying drawing 1, B passage shines atomizer 4 in the accompanying drawing 1 simultaneously, and the hollow cathode lamp of the special-purpose tellurium excitation source of C, D passage shines atomizer 4 in the accompanying drawing 1 subsequently simultaneously in the accompanying drawing 1.Being in the analyzed element arsenic of ground state and tellurium atom is subjected to the characteristic wavelength radiant rays and excites, send specific wavelength atomic fluorescence signal respectively, photomultiplier 3 detects in accompanying drawing 1, after data acquisition unit 1 order is finished collection in the accompanying drawing 1, by data computation unit 6 in the accompanying drawing 1, obtain by the element arsenic after the test fluorescence intensity conversion of element arsenic and tellurium and the concentration of tellurium.Relevant regulations according to instrument detection limit and precision mensuration, adopt four-way to merge atomic fluorescence spectrometer and test the series standard solution that above-mentioned arsenic tellurium mixes, drawing arsenic and tellurium as calculated detects and be limited to: arsenic: 0.012ng/ml, tellurium: 0.011ng/ml, precision is: arsenic: tellurium 0.9%: 0.9%.
The element that embodiment 3 uses in common four-way atomic fluorescence spectrometer test implementation example 1 sample.
Dispose serial arsenic tellurium mixed standard solution.Pack on the A channel in accompanying drawing 1 hollow cathode lamp of special-purpose arsenic excitation source, the hollow cathode lamp of the special-purpose tellurium excitation source of packing on the D passage in the accompanying drawing 1 is not adorned hollow cathode lamp on B, the C-channel in the accompanying drawing 1.By signal generator 5 in the accompanying drawing 1, the lamp pulse sequential of A, B, C, D passage is shown in the accompanying drawing 2 in the control accompanying drawing 1, and promptly the hollow cathode lamp of the hollow cathode lamp of the special-purpose arsenic excitation source of A, D passage and special-purpose tellurium excitation source successively shines atomizer 4 in the accompanying drawing 1 in the accompanying drawing 1.Being in the analyzed element arsenic of ground state and tellurium atom is subjected to the characteristic wavelength radiant rays and excites, send specific wavelength atomic fluorescence signal respectively, photomultiplier 3 detects in accompanying drawing 1, after data acquisition unit 1 order is finished collection in the accompanying drawing 1, by data computation unit 6, obtain by the element arsenic after the test fluorescence intensity conversion of element arsenic and tellurium and the concentration of tellurium.According to the relevant regulations that instrument detection limit and precision are measured, common four-way atomic fluorescence spectrometer is tested the series standard solution that above-mentioned arsenic tellurium mixes, and draws arsenic and tellurium after as calculated and detects and be limited to: arsenic: 0.02ng/ml, tellurium: 0.02ng/ml; Precision is: arsenic: tellurium 0.9%: 0.9%.
The embodiment comparing result sees Table 1.
The detection limit of arsenic and tellurium element and precision contrast among table 1 embodiment 1, embodiment 2, the embodiment 3
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Assay method | Triple channel merges | Two passages merge | Prior art |
| Arsenic detection limit (ng/ml) | 0.006 | 0.012 | 0.02 |
| Tellurium detection limit (ng/ml) | 0.012 | 0.02 | |
| Arsenic precision | 0.9％ | 0.9％ | 0.9％ |
| Tellurium precision | 0.9％ | 0.9％ | 0.9％ |
As shown in Table 1, adopt multipath merge spectrum chemical analysis method of the present invention when guaranteeing high precision, greatly reduce the detection limit of element.
Claims (7)
1, a kind of multipath merge spectrum chemical analysis method is characterized in that:
This method is shone sample simultaneously by the same light source that makes two or more passages in the multi-channel spectrometer based, be equivalent to these same light source are merged into a light source irradiation sample behind the intensity of light source superposition, test identity element jointly, obtain the concentration of this element.
2, multipath merge spectrum chemical analysis method according to claim 1 is characterized in that:
Described multi-channel spectrometer based is the hyperchannel atomic fluorescence spectrometer.
3, multipath merge spectrum chemical analysis method according to claim 2 is characterized in that:
In wherein 2～4 passages of 2～12 passage atomic fluorescence spectrometer, pack into the hollow cathode lamp of identical tested element special use;
By signal generator, the lamp pulse sequential of controlling the identical hollow cathode of this 2～4 passage is identical, promptly shines sample simultaneously, and the analyzed element that is in ground state is subjected to the characteristic wavelength radiant rays and excites, and sends specific wavelength atomic fluorescence signal;
Above-mentioned specific wavelength atomic fluorescence signal detects through photomultiplier, and conventional amplifier amplifies, and after data acquisition unit is finished collection, by the data computation unit, obtains the concentration by the tested element after the test fluorescence intensity conversion of tested element.
4, multipath merge spectrum chemical analysis method according to claim 2 is characterized in that:
In wherein 2 passages of 4～12 passage atomic fluorescence spectrometer, the hollow cathode lamp of the identical a kind of tested element special use of packing into, the hollow cathode lamp of the identical another kind of tested element special use of in other 2 passages, packing into;
Pass through signal generator, control these two groups of different hollow cathode lamps with different lamp pulse sequential, and identical hollow cathode lamp shines sample with identical lamp pulse sequential in two groups, two kinds of tested elements that are in ground state successively are subjected to the characteristic wavelength radiant rays and excite, and send specific wavelength atomic fluorescence signal respectively;
Above-mentioned specific wavelength atomic fluorescence signal detects through photomultiplier, conventional amplifier amplifies, after data acquisition unit is finished collection in proper order,, obtain concentration by two kinds of tested elements after the test fluorescence intensity conversion of two tested elements by the data computation unit.
5, a kind of hyperchannel of the described multipath merge spectrum chemical analysis method of one of claim 1～4 of realizing merges the spectral class analytical instrument, it is characterized in that the composition of this instrument comprises:
Signal generator is used for the irradiation sequence and the irradiation time of the illuminator of each passage are controlled, and makes that the irradiation sequential of the same light source lamp that is equipped with in different passages is identical;
The hyperchannel excitation source;
Atomizer;
Photomultiplier;
Conventional amplifier;
Data acquisition unit, this unit carries out acquisition order to each channel data;
Data computation unit, this unit are converted to the light intensity data of the tested element of input the concentration of tested element;
Wherein, the functional sequence of each ingredient of instrument is: under the control of signal generator, the atomic vapour of the illuminator of each passage to be produced in the predetermined sequential irradiated atoms device in the hyperchannel excitation source, produce light signal, after photomultiplier detection, the amplification of conventional amplifier, by data acquisition unit each channel data is carried out acquisition order again, after the data computation unit is converted to the light intensity data of the tested element of input the concentration of tested element.
6, hyperchannel according to claim 5 merges the spectral class analytical instrument, it is characterized in that:
Described signal generator is a signal trigger.
7, merge the spectral class analytical instrument according to claim 5 or 6 described hyperchannels, it is characterized in that:
It is that hyperchannel merges atomic fluorescence spectrometer that above-mentioned hyperchannel merges the spectral class analytical instrument;
The light signal of above-mentioned generation is a fluorescence signal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100679653A CN100417932C (en) | 2005-04-30 | 2005-04-30 | Multipath merge spectrum chemical analysis method and its instrument |
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|---|---|---|---|
| CNB2005100679653A CN100417932C (en) | 2005-04-30 | 2005-04-30 | Multipath merge spectrum chemical analysis method and its instrument |
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| CN1858580A true CN1858580A (en) | 2006-11-08 |
| CN100417932C CN100417932C (en) | 2008-09-10 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102374978A (en) * | 2010-08-06 | 2012-03-14 | 上海光谱仪器有限公司 | Atomic fluorescence analyzing device |
| CN102507518A (en) * | 2011-10-25 | 2012-06-20 | 天津港东科技发展股份有限公司 | 12-lamp multi-channel atomic fluorescence spectrometer |
| CN107479432A (en) * | 2017-07-11 | 2017-12-15 | 北京海光仪器有限公司 | Multielement is combined with survey and merges measuring system |
| CN109507167A (en) * | 2018-11-16 | 2019-03-22 | 深圳达闼科技控股有限公司 | A kind of substance detecting method, calculates equipment and computer storage medium at device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2655229Y (en) * | 2003-09-03 | 2004-11-10 | 西北有色地质研究院 | Multi-channel atomic fluorescent spectrograph |
-
2005
- 2005-04-30 CN CNB2005100679653A patent/CN100417932C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102374978A (en) * | 2010-08-06 | 2012-03-14 | 上海光谱仪器有限公司 | Atomic fluorescence analyzing device |
| CN102507518A (en) * | 2011-10-25 | 2012-06-20 | 天津港东科技发展股份有限公司 | 12-lamp multi-channel atomic fluorescence spectrometer |
| CN102507518B (en) * | 2011-10-25 | 2013-05-08 | 天津港东科技发展股份有限公司 | 12-lamp multi-channel atomic fluorescence spectrometer |
| CN107479432A (en) * | 2017-07-11 | 2017-12-15 | 北京海光仪器有限公司 | Multielement is combined with survey and merges measuring system |
| CN109507167A (en) * | 2018-11-16 | 2019-03-22 | 深圳达闼科技控股有限公司 | A kind of substance detecting method, calculates equipment and computer storage medium at device |
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| Publication number | Publication date |
|---|---|
| CN100417932C (en) | 2008-09-10 |
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