CN1178321A - Method of and apparatus for qualitative analysis - Google Patents
Method of and apparatus for qualitative analysis Download PDFInfo
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- CN1178321A CN1178321A CN 97112468 CN97112468A CN1178321A CN 1178321 A CN1178321 A CN 1178321A CN 97112468 CN97112468 CN 97112468 CN 97112468 A CN97112468 A CN 97112468A CN 1178321 A CN1178321 A CN 1178321A
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Abstract
A qualitative analysis is carried out by first storing reference spectral line data of various elements in different compound forms, exciting a sample and spectroscopically analyzing signal light emitted from the sample to obtain measured spectral line data, determining whether these measured spectral line data include spectral lines of specified compound-forming elements, and comparing the reference spectral line data with the measured spectral line data, if the measured spectral line data are found to include spectral lines of any of the compound-forming elements, to thereby identify elements in the sample.
Description
The invention relates to qualitative analysis methods and equipment, for example fluorescent X-ray spectrometry and emission spectrographic analysis, wherein a kind of sample are subjected to optical excitation and the flashlight of therefrom launching are carried out spectral analysis to identify some elements that contained in this sample.More particularly, the present invention is the technology of carrying out accurate qualitative analysis with the effect of eliminating chemical shift.
In order to carry out the qualitative analysis of sample, for example use the fluorescent X-ray spectrometer, then known at first the need deposits in the memory device wavelength of various elements as database in, seeking sample then is subjected to fluorescent X-ray to excite corresponding wavelength in the spectrum that is produced, promptly detect the wavelength of angle 2 θ corresponding to each spectrum spectrum peak, they and database are compared, and identify the desire survey element that its value approaches element value in the database.Yet the various target elements that will analyze in sample (for example Al, Si, O, SMg and B) usually do not exist with element form, and often are in compound form, for example are a kind of oxide or nitride.When a kind of element is when being in compound form, just can be observed so-called " chemical shift ", that is the spectrum peak of element is compared with the element of element form in the compound, be come across displacement wavelength in.Fig. 3 explanation, the profile diagram of the element boron of representing with solid line is how to change at B
2O
3With the represented profile diagram of dotted line, the latter is the fashionable peak shift that Δ 2 θ distances occur of boron and oxidation under the situation.
To having some elements or the light element of little atomic number, its chemical shift is more obvious.This may be since light element the few electronics of quantity is only arranged, and since chemical bond due to its energy state as if be subjected to its K-layer electronics condition effect bigger.In one case, promptly as chemical shift Δ 2 θ during greater than the error of the optical system of measuring fluorescent X-ray, then measured peak position and the peak position in the database are inconsistent, therefore this element can not obtain identifying that the element of identifying out in other words is the element corresponding to an incorrect spectral line.
Therefore purpose of the present invention is in order to solve in qualitative analysis of samples because the problem of the incorrect evaluation element that the chemical shift of element causes, thereby improves the reliability of qualitative analysis.
Embodiment a kind of qualitative analysis equipment of the present invention can reach above-mentioned or other purpose with it, it is characterized in that including: a data-carrier store is used to store by the resulting spectral analysis flashlight of having surveyed spectral line data and having been launched by sample of optical excitation sample; One archival memory, the reference spectral line data that is used for storing the various elements that are in different compound forms; And a data-analyzing machine, be used to measure measured spectral line data whether and include the element spectral line of oxygen and nitrogen for example that forms specific compound; If measured spectral line data includes any spectral line of the element that forms compound, through contrast with reference to spectral line data and measured spectral line data, just can identify some elements in the sample like this.
Writing some accompanying drawings of this instructions and a formation instructions part, is the explanation of the embodiment of the invention, and they are used for illustrating principles more of the present invention with instructions.
In the accompanying drawings:
Fig. 1 is a block scheme of implementing present device, is used for analysis of fluorescence X-ray;
Fig. 2 is a process flow diagram of implementing method for qualitative analysis of the present invention, is to use equipment shown in Figure 1, and
Fig. 3 is the curve map of explanation chemical shift.
Instructions of the present invention be at last mode with analysis of fluorescence X-ray equipment as qualitative analysis equipment one example, described.Shown in the block scheme of Fig. 1, this equipment 1 comprises a sample analyzer 2, one data-carrier stores 4, one archival memories 6, one input media 8, one data-analyzing machines, 10, one controller units 12 and output units 14.This sample analyzer 2 comprises an x-ray generator, and a spectrum and an x-ray detector (not shown) and as the flashlight that is obtained by excited sample of spectral analysis come the spectral line of contained various elements in the measuring samples with this.Data-carrier store 4 can comprise the memory device such as the random-access memory (ram) of a known kind, is used for storing by the measured data relevant for the sample spectral line of sample analyzer 2.Archival memory 6 can comprise an external memory device such as CD-ROM, and the line wavelength data that are in the element of various chemical states, for example be in the line wavelength data of some elements in oxide, nitride, the carbonide, just be stored in the archival memory 6 originally.For example concerning boron, not only deposited the line wavelength data of element boron in, formed boride but also deposited in, as B with oxygen, nitrogen, carbon etc.
2O
3And B
2N
3Deng the line wavelength data.In other words, the data of the every kind of element that has chemical shift have also been deposited in.In addition, it sees some element for convenience, oxygen and nitrogen element that for example can other element of oxidation, be called " oxidation element " in this article, and can form some elements such as Al, Si, P, S, Mg and the B of chemical bond with these oxidation elements, all be called " oxidized element " for simplicity.
Input media 8 can comprise an input interface, for example keyboard or Genius mouse, and its effect is to be convenient to the user to set measuring condition and data analysis condition with sample analyzer.
Data-analyzing machine 10 is to be used for measuring being stored in any spectral line whether data that data-carrier store 4 recorded contain oxidation element such as oxygen and nitrogen, and this spectral line is that to be used for the element of authenticating compound form necessary.If this oxidation element is found to be contained in wherein, then the database that deposits in the archival memory 6 is retrieved, oxidized element that i.e. retrieval combines with the sort of oxidation element and the chemical shift that has, and compare with measured data, some elements that are contained in the sample can be identified out.
Secondly, the process flow diagram of Fig. 2 is to be used for illustrating the qualitative analysis of samples that is undertaken by equipment 1 is how can carry out automatically.
When carrying out quantitative test, be that sample is exposed to initial X-beam, at this moment record some spectral lines of contained each element in the sample respectively, and a detecting device is used for detecting the fluorescent X-ray (step S1) that sends from sample by spectral device.At this moment also can obtain the spectral line data that oxidation element such as oxygen and nitrogen and other element form compound.These are stored in the data-carrier store 4 by sample analyzer 2 resulting each element data.Deposit some data of data-carrier store 4 like this in, analyze by data-analyzing machine 10 again, obtain detection angle 2 θ of these spectral lines and the intensity I (step S2) at each spectrum peak then.Then, data-analyzing machine 10 is measured, and sees that the packet that whether is stored in the data-carrier store 4 contains the spectral line of oxidation element such as oxygen and nitrogen, and these spectral lines are the element of authenticating compound form needed (step S3).The practice of this step is, some spectral strengths tentatively are set, as threshold value (threshold values), these peak intensities are equivalent to the content of oxidation element, it promptly in sample oxide, the content of the oxidation element of nitride and carbonide form, and measure see whether measured a certain oxidation element line strength greater than threshold value.As if because these oxidation elements are compared with some oxidized elements, its chemical shift is less relatively, so wrong evaluation can not take place.
Exist if determined these oxidation elements, just data-analyzing machine 10 retrieve data storehouse memorizers 6 then, so that obtain combining the spectral line data (step S4) of some oxidized elements that cause chemical shift with the oxidation element.If data-analyzing machine 10 has detected oxygen, as oxidation element one example, just retrieved the spectral line data of the oxidized element that combines with oxygen.Data-analyzing machine 10 compares this database and measured data and mates then, to identify some elements (step S5) that contained in the sample.Comprehensive, the present invention has considered the effect of chemical shift to the evaluation of each element to every kind of element.Like this, because the displacement at the detection angle that chemical shift causes can not have adverse influence to the performance of equipment or various elements are caused wrong evaluation, promptly can correctly identify the spectral line of in esse each element.
Learn if in step S3, measure, in the data that record, do not contain spectral line, then just searching database 6 spectral line data (step S6) of seeking each element that is in element morphology (that is not being the chemical combination form that is in the oxidation element) of data-analyzing machine 10 to the necessary a certain oxidation element of authenticating compound form.Then, measured data and the data in the database are compared and mate, be contained in some elements (step S5) in the sample with evaluation.
The result that will identify by data-analyzing machine 10 is sent in the output unit 14, is displayed on CRT or LCD or the machine that is printed prints (step S7).
Though described the present invention in a kind of mode of fluorescent X-ray spectrometer above, this does not mean limitation of the scope of the invention.Much less, the present invention can be effectively applied to emission spectrum etc. equally.Generally speaking, one of advantage of the present invention is to have eliminated in qualitative analysis the possibility that mistake that the chemical shift owing to each element spectral line causes is identified.Another advantage of the present invention is when quantitative test is carried out automatically, can be achieved.Though around detecting the center, angle some permissible error can take place according to the present invention in spectrum analysis, because some source of error of optical system adopts permissible error, yet the permissible error of generation can lower greatly.Because chemical shift need not to consider.In analytical work, the quantity that reduces the back benefit spectral line that needs search (retrieval) has favourable influence, and the time that analysis needs can also shorten.
Claims (6)
1. a qualitative analysis equipment is characterized in that by exciting a sample and identifying the various elements that are contained in this sample with spectral analysis from the flashlight of this sample this equipment includes:
One data-carrier store is used for storing the spectral line data that has recorded that obtains from sample;
One archival memory deposits the reference spectral line data of the various elements that are in different compound forms in; And
One data-analyzing machine, in order to measure the spectral line that the spectral line data that whether has recorded includes some elements of specific compound formation, if and the spectral line data that has recorded includes the spectral line of the element of any formation compound, just will compare each element that can identify in the sample with reference to spectral line data and measured spectral line data.
2. equipment as claimed in claim 1 is characterized in that more described specific compound forming elements are can form some compounds in above-mentioned different compound forms.
3. equipment as claimed in claim 1 is characterized in that described compound forming element comprises oxygen, nitrogen and carbon.
4. method for qualitative analysis is characterized in that it contains following each step:
Deposit the reference spectral line data of the various elements that are in different compound forms in;
Optical excitation sample and the spectral line data of flashlight of from this sample, sending with spectral analysis to obtain to have predicted;
Deposit the described spectral line data that has predicted in;
Measure described some spectral lines whether spectral line includes the specific compound forming element that predicted; And
To compare with reference to spectral line data and the described spectral line data that predicted, if this spectral line data that has recorded includes some spectral lines of any compound forming element, just identify each element in the sample with this.
5. method as claimed in claim 4 is characterized in that more described specific compound forming elements are some compounds that can form said different compound forms.
6. method as claimed in claim 4 is characterized in that more described compound forming elements comprise oxygen, nitrogen and carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97112468 CN1178321A (en) | 1996-09-30 | 1997-06-12 | Method of and apparatus for qualitative analysis |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP259225/96 | 1996-09-30 | ||
| CN 97112468 CN1178321A (en) | 1996-09-30 | 1997-06-12 | Method of and apparatus for qualitative analysis |
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| CN1178321A true CN1178321A (en) | 1998-04-08 |
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| CN 97112468 Pending CN1178321A (en) | 1996-09-30 | 1997-06-12 | Method of and apparatus for qualitative analysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102495039A (en) * | 2011-10-27 | 2012-06-13 | 瓮福（集团）有限责任公司 | Raman spectrum qualitative detection method for compound fertilizer nitrogen forms |
-
1997
- 1997-06-12 CN CN 97112468 patent/CN1178321A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102495039A (en) * | 2011-10-27 | 2012-06-13 | 瓮福（集团）有限责任公司 | Raman spectrum qualitative detection method for compound fertilizer nitrogen forms |
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