CN102830108A - Method and device for photocurrent integration of AC-DC arc direct-reading spectrometer, and spectrometer - Google Patents
Method and device for photocurrent integration of AC-DC arc direct-reading spectrometer, and spectrometer Download PDFInfo
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- CN102830108A CN102830108A CN2012103038410A CN201210303841A CN102830108A CN 102830108 A CN102830108 A CN 102830108A CN 2012103038410 A CN2012103038410 A CN 2012103038410A CN 201210303841 A CN201210303841 A CN 201210303841A CN 102830108 A CN102830108 A CN 102830108A
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Abstract
The invention provides a method for photocurrent integration of AC-DC arc direct-reading spectrometer. The method comprises performing arc excitation on reference samples for one time to obtain evaporation characteristic of each element in the reference samples; respectively determining initial integration time and end integration time of corresponding photocurrent of the same elements in the to-be-detected samples in accordance with the evaporation characteristic of each element; and integrating photocurrent of each element in the to-be-detected samples between the initial integration time and end integration time of the corresponding photocurrent. The integration method provided by the invention improves signal-to-noise ratio and sensitivity of the analysis method, and therefore improves accuracy of the analysis results.
Description
Technical field
The present invention relates to the Atomic Emission Spectral Analysis instrument field, relate in particular to photocurrent integration method and device, the spectrometer of AC/DC electric arc direct-reading spectrometer.
Background technology
One meter or two meters grating spectrographs of arc excitation are important branch in the Atomic Emission Spectrometer AES device; The characteristics of this instrument can directly be analyzed powdered samples such as soil, rock, water system sediment and high pure metal oxide in the geological sample; Need not chemical digesting and dilution; Thereby avoided clearing up the diluted reduction sensitivity for analysis of content of some element in the solution of back, but also very easily brought unmanageable pollution into.
For a long time; One meter or two meters grating spectrographs of arc excitation that China produces are carried out the analysis task that hundreds of thousands spare geochemical sample is arranged in the geochemical prospecting " 1:5 ten thousand regional geochemical exploration whole nation surface sweeping plans " every year in the whole nation, geology field; And measure 17～19 kinds of impurity contents in a large amount of high pure metal tungsten oxide, molybdena and other noble metal sample in coloured, the metallurgical system, therefore be used widely in the numerous laboratories of China.And one meter or two meters grating spectrographs of traditional arc excitation adopt phase-plate record usually, wash flow processs such as phase, photometry and carry out spectral analysis; Its running program is cumbersome, inefficiency, labour intensity is big and drawback such as easy contaminated environment; Therefore, users extremely expect the birth of novel arc excitation photo-electric direct reading spectrometer.
Arc excitation photo-electric direct reading spectrometer groundwork principle is: utilize interchange or direct-current arc light source that sample is inspired characteristic spectrum; Characteristic spectrum is diffracted to the spectrum line of different wave length through the beam splitting system of concave grating; Then this light signal is converted into electric signal, electric signal through amplification and data processing after obtain the sample experimental data because the intensity of spectrum line becomes certain functional relation with the content of different element; Therefore; Through the sample experimental data is handled the content that can calculate tested element in the sample, this arc excitation photo-electric direct reading spectrometer has simple to operate, and advantage such as work efficiency height.
Be to export when light signal is converted into electric signal with the form of photocurrent; The size of photocurrent changes with the characteristic spectral line light intensity; And each elemental characteristic spectral line light intensity changes in time, therefore, is not the instantaneous value of measuring light electric current usually; But the method for employing integration, the integral voltage value of photocurrent on electric capacity in record a period of time.At present, different elements adopt usually and carry out integration identical integral time, yet because the difference of each element volatilization complexity, in excitation process, the time period that from sample, evaporates is different.Carry out integration in the identical time, can increase the Volatile Elements background, signal to noise ratio (S/N ratio) reduces; And, not only can increase background for difficult volatile element, and also possibly cause signals collecting incomplete, reduce Sensitivity of Analytical Method.
Summary of the invention
Embodiments of the invention provide a kind of photocurrent integration method, device and spectrometer of AC/DC electric arc direct-reading spectrometer, and spectral lines with different is adopted different somes integral time, improve Sensitivity of Analytical Method.
For realizing above-mentioned purpose, the embodiment of the invention provides following technical scheme:
A kind of photocurrent integration method of AC/DC electric arc direct-reading spectrometer comprises:
Reference sample is carried out arc excitation one time, obtain the evaporation characteristic of each element in the reference sample;
According to the evaporation characteristic of each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element;
At the integration zero-time of corresponding photocurrent and integration in the concluding time, the photocurrent of each element in the testing sample is carried out integration.
Alternatively, the time that the integration zero-time of photocurrent occurs for this elements vaporization, the time that the integration concluding time of photocurrent finishes for this elements vaporization.
Alternatively, said integration is the integration of photocurrent on electric capacity.
Alternatively, the integrating capacitor that each element is corresponding is different.
The formula that adopts when alternatively, carrying out integration is:
Wherein, t1 is the integration zero-time, and t2 is the integration concluding time, and C is the integrating capacitor value, U
0Be starting potential.
Alternatively, said reference sample is one or more standard models with testing sample element, and/or is testing sample.
In addition, the present invention also provides a kind of photocurrent integrating gear of AC/DC electric arc direct-reading spectrometer, comprising:
Arcing device is used for reference sample is carried out arc excitation one time;
The evaporation characteristic deriving means is used for obtaining the evaporation characteristic of each element of reference sample;
Integral time, determination module was used for the evaporation characteristic according to each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element;
Integration module was used at the integration zero-time of corresponding photocurrent and integration in the concluding time, and the photocurrent of each element in the testing sample is carried out integration.
In addition, the present invention also provides the direct-reading spectrometer of the AC/DC electric arc with above-mentioned photocurrent integrating gear.
The photocurrent integration method of AC/DC electric arc direct-reading spectrometer of the present invention; Through the evaporation characteristic of reference sample, confirm corresponding integration zero-time of each element and concluding time in the testing sample respectively, thereby can carry out the integration of different time sections respectively to them according to the characteristic of different elements in the testing sample; Reduced background (noise signal); Promptly improve signal to noise ratio (S/N ratio), improved Sensitivity of Analytical Method, thereby improved the accuracy of analyzing.
Description of drawings
Fig. 1 is the process flow diagram according to the photocurrent integration method of the embodiment of the invention;
Fig. 2 is sample evaporation family curve synoptic diagram according to an embodiment of the invention.
Embodiment
For make above-mentioned purpose of the present invention, feature and advantage can be more obviously understandable, does detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
A lot of details have been set forth in the following description so that make much of the present invention; But the present invention can also adopt other to be different from alternate manner described here and implement; Those skilled in the art can do similar popularization under the situation of intension of the present invention, so the present invention does not receive the restriction of following disclosed specific embodiment.
As the description in the background technology, when photocurrent was carried out integration, the photocurrent corresponding to different elements adopted identical integral time, has the phase mutual interference between the spectral line of different elements, can the accuracy of integration data be impacted.For this reason, the invention provides a kind of photocurrent integration method of AC/DC electric arc direct-reading spectrometer,, improve Sensitivity of Analytical Method through confirming section integral time of elements different in the sample respectively.
With reference to shown in Figure 1, this method comprises: S01, reference sample is carried out arc excitation one time, and obtain the evaporation characteristic of each element in the reference sample; S02, according to the evaporation characteristic of each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element; S03 at the integration zero-time of corresponding photocurrent and integration in the concluding time, carries out integration to the photocurrent of each element in the testing sample.
Be to have adopted arc excitation one time in the present invention, obtain evaporation characteristic, like the evaporation characteristic curve, put the integral time of then from evaporation characteristic, selecting specific time point to be used as different elements, mainly is to have utilized arc excitation sample and fractionation effect.Particularly; When geological sample is carried out an arc excitation; Be about to sample and be placed on and carry out arcing in the electrode hole, sample is molten condition very soon after the starting the arc, and wherein each kind of material (element) will evaporate and get into discharge gap according to its fusing point and boiling point successively; Each element is called fractionation effect by the phenomenon that its different evaporation characteristics get into discharge gap in order, and the present invention also realizes that through making full use of this fractionation effect different element adopts the integral time section just.
When selecting reference sample, the content of middle element is selected per sample, to obtain more tangible evaporation characteristic; For example; Can select the high standard substance of constituent content to be used as reference sample, when the constituent content in the testing sample is high, also can just select testing sample sample as a reference; The perhaps combination of the two; As required, need select a plurality of reference samples to carry out an arc excitation to obtain the evaporation characteristic of each element in the testing sample sometimes, this evaporation characteristic can appear with the form of data or curve.
Evaporation characteristic curve as shown in Figure 2, as to obtain behind the arc excitation for one embodiment of the invention, wherein; Horizontal ordinate is that the time, (unit second, s), ordinate was a light intensity; The evaporation characteristic curve of different elements has been shown among the figure, and the evaporation complexity of different elements is different, and its evaporation time is inequality; Can see that element Bi belongs to more evaporable element, about 21s, has just evaporated; Element al belongs to the element of medium volatilization, about 33s, evaporates; Element ti then belongs to the element of difficult volatilization, about 43s, just can evaporate, if select unified 0-43s integral time; That is for tested element Bi, and after the integration 21s, the spectral line of element al and Ti is background spectrum to it; Be noise signal, can reduce the signal to noise ratio (S/N ratio) of tested element Bi, therefore; According to this evaporation characteristic, can element Bi be chosen in about 0-21s integral time, avoid the influence of background spectral line; In like manner, element al can be chosen in 0-33s its integral time, and element ti can be chosen in 0-43s its integral time.In the example here, be that the integration zero-time of photocurrent that each element is corresponding is chosen in starting point 0, the concluding time is chosen in the time point that evaporation finishes; But it is understandable that; Can also select between starting point to the end point the more typical time period as integral time, can be chosen in integral time about 6-20s etc. like element Bi, i.e. the time point of concluding time point selection before its evaporation finishes; In addition; What it will be appreciated by those skilled in the art that is, the starting point of evaporation and end point are time point roughly, and different people has certain difference to its judgement; The present invention does not make qualification to the numerical value of this concrete time point, and giving an example here is merely example.
After the integral time of from evaporation characteristic, having confirmed each element, at the integration zero-time of corresponding photocurrent and integration in the concluding time, the photocurrent of each element in the testing sample is carried out integration.In this embodiment, adopt the integration of photocurrent on electric capacity, promptly obtain the integral voltage value behind the integration, the formula of employing is:
Wherein, t1 is the integration zero-time, and t2 is the integration concluding time, and C is the integrating capacitor value, U
0Be starting potential.Because the integration to the photocurrent of different elements adopts the different time section, has reduced background, has improved Sensitivity of Analytical Method, thereby improve analytical accuracy.
More than the photocurrent integration method and the embodiment of AC/DC electric arc direct-reading spectrometer of the present invention carried out detailed description, accordingly, the invention allows for a kind of photocurrent integrating gear of AC/DC electric arc direct-reading spectrometer, comprising:
Arcing device is used for reference sample is carried out arc excitation one time;
The evaporation characteristic deriving means is used for obtaining the evaporation characteristic of each element of reference sample;
Integral time, determination module was used for the evaporation characteristic according to each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element;
Integration module was used at the integration zero-time of corresponding photocurrent and integration in the concluding time, and the photocurrent of each element in the testing sample is carried out integration.
Through above-mentioned device, realize that different elements divide the time period to carry out the purpose of photocurrent integration.
Moreover correspondingly, the present invention also provides the direct-reading spectrometer of the AC/DC electric arc with above-mentioned photocurrent integrating gear.
Right the present invention discloses as above with preferred embodiment, yet is not in order to limit the present invention.Any those of ordinary skill in the art; Do not breaking away under the technical scheme scope situation of the present invention; All the method for above-mentioned announcement capable of using and technology contents are made many possible changes and modification to technical scheme of the present invention, or are revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical scheme of the present invention, all still belongs in the scope of technical scheme protection of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (8)
1. the photocurrent integration method of an AC/DC electric arc direct-reading spectrometer is characterized in that, comprising:
Reference sample is carried out arc excitation one time, obtain the evaporation characteristic of each element in the reference sample;
According to the evaporation characteristic of each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element;
At the integration zero-time of corresponding photocurrent and integration in the concluding time, the photocurrent of each element in the testing sample is carried out integration.
2. photocurrent integration method according to claim 1 is characterized in that, the time that the integration zero-time of photocurrent occurs for this elements vaporization basically, the time that the integration concluding time of photocurrent finishes for this elements vaporization basically.
3. photocurrent integration method according to claim 1 is characterized in that, said integration is the integration of photocurrent on electric capacity.
4. photocurrent integration method according to claim 3 is characterized in that, the integrating capacitor that each element is corresponding is different.
5. photocurrent integration method according to claim 3 is characterized in that, the formula that adopts when carrying out integration is:
Wherein, t1 is the integration zero-time, and t2 is the integration concluding time, and C is the integrating capacitor value, U
0Be starting potential.
6. photocurrent integration method according to claim 1 is characterized in that, said reference sample is one or more standard models with testing sample element, and/or is testing sample.
7. the photocurrent integrating gear of an AC/DC electric arc direct-reading spectrometer is characterized in that, comprising:
Arcing device is used for reference sample is carried out arc excitation one time;
The evaporation characteristic deriving means is used for obtaining the evaporation characteristic of each element of reference sample;
Integral time, determination module was used for the evaporation characteristic according to each element, confirm respectively with testing sample in the integration zero-time and integration concluding time of the identical corresponding photocurrent of element;
Integration module was used at the integration zero-time of corresponding photocurrent and integration in the concluding time, and the photocurrent of each element in the sample to be tested is carried out integration.
8. an AC/DC electric arc direct-reading spectrometer is characterized in that, comprises the photocurrent integrating gear described in the claim 7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237178A (en) * | 2014-10-09 | 2014-12-24 | 重庆邮电大学 | Method and device for detecting trace metal elements in water body by using laser-induced breakdown spectroscopy assisted by direct current discharging vaporization |
| CN110044853A (en) * | 2019-05-06 | 2019-07-23 | 北京北分瑞利分析仪器(集团)有限责任公司 | A kind of determination method of tested elemental signals acquisition time section |
| CN118465735A (en) * | 2024-07-15 | 2024-08-09 | 浙江禾川科技股份有限公司 | Dual-photoelectric sensor and signal processing method thereof |
Citations (1)
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| CN102608104A (en) * | 2011-09-06 | 2012-07-25 | 北京瑞利分析仪器有限公司 | Direct-reading spectrometer based on combination of alternating current/direct current arc and concave grating beam splitting system |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102608104A (en) * | 2011-09-06 | 2012-07-25 | 北京瑞利分析仪器有限公司 | Direct-reading spectrometer based on combination of alternating current/direct current arc and concave grating beam splitting system |
Non-Patent Citations (2)
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| MAURA MAHAR ET AL.: "Direct Determination of Trace Elements in Solid Samples by DC Arc With Emphasis on the Analysis of High-Purity Copper", 《AMERICAN LABORATORY》 * |
| 张文华等: "交、直流电弧直读光谱仪的研制及其应用", 《光谱仪器与分析》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237178A (en) * | 2014-10-09 | 2014-12-24 | 重庆邮电大学 | Method and device for detecting trace metal elements in water body by using laser-induced breakdown spectroscopy assisted by direct current discharging vaporization |
| CN104237178B (en) * | 2014-10-09 | 2017-11-03 | 重庆邮电大学 | The method and apparatus of trace metal element in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body |
| CN110044853A (en) * | 2019-05-06 | 2019-07-23 | 北京北分瑞利分析仪器(集团)有限责任公司 | A kind of determination method of tested elemental signals acquisition time section |
| CN118465735A (en) * | 2024-07-15 | 2024-08-09 | 浙江禾川科技股份有限公司 | Dual-photoelectric sensor and signal processing method thereof |
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