CN102539351A - Measurement method of atomic absorption - Google Patents
Measurement method of atomic absorption Download PDFInfo
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- CN102539351A CN102539351A CN2010106212602A CN201010621260A CN102539351A CN 102539351 A CN102539351 A CN 102539351A CN 2010106212602 A CN2010106212602 A CN 2010106212602A CN 201010621260 A CN201010621260 A CN 201010621260A CN 102539351 A CN102539351 A CN 102539351A
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- light source
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Abstract
The invention belongs to the technical field of analytical chemistry, in particular relates to a measurement method of atomic absorption. The measurement method is used for measuring atomic absorption through correcting light emission of an element to be measured in a glow atomizer. The measurement method comprises the following steps of: respectively supplying power to the glow atomizer and a light source by adopting different frequencies of pulses; and respectively acquiring a signal I0 of light source light emission, a signal IG of glow discharge pulse light emission and a signal IH generated when a light source light-emitting pulse is overlapped with a glow discharge light-emitting pulse, correcting the signal of glow light emission to obtain a signal IH-IG of light source transmission light, calculating an absorbance A=logI0/(IH-IG) generated by the element to be measured in the glow atomizer, and figuring out the content of the element to be measured according to a function relationship of the absorbance and the content of the element to be measured and the absorbance of a sample. By adopting the measurement method of the atomic absorption, the change before and after light emitted by the light source penetrates through the glow atomizer is accurately measured, and the content of the element to be measured in the sample can be accurately figured out.
Description
Technical field
The invention belongs to technical field of analytical chemistry, particularly a kind of measuring method of atomic absorption.
Background technology
Atomic absorption spectrography (AAS) is a kind of analysis means that is widely used, and is mainly used in trace or trace metal element analysis.Existing commodity atomic absorption spectrophotometer (AAS) mainly is to adopt flame atomizer or electrothermic atomizer to realize measuring atoms of elementsization; So can only in advance solid sample be processed solution, perhaps solid sample is ground into tiny particle and just can carry out atomic absorption detecting.
Glow discharge is a kind of low pressure gaseous discharge phenomenon, when keeping glow discharge with high voltage direct current, the cathodic sputtering effect takes place on the negative electrode, and the atom of cathode material is overflowed from material surface, can form ground state atom, excited atom or ion.According to the glow discharge device of this principle development, light source and the mass spectrometric ionization source of aura as emission spectrometer obtains to use widely.Utilize the phenomenon of the cathodic sputtering effect generation ground state atom of glow discharge, developed the glow discharge atomizer, successfully be applied to the atomization of block conductor sample.
Atomic absorption analysis is to make the light of specific wavelength through atom vapor, realizes quantitative test through measuring through the attenuation degree of light behind the atom vapor.Existing atomic absorption instrument mainly adopts flame atomizer and electrothermic atomizer; In atomizer, there is not the luminous intensity meter of measurement light source under the state of sample to make I; Make sample in atomizer, realize atomization then, and the intensitometer of measurement transmitted light this moment is made I
i, both ratio is taken the logarithm as absorbance A [A=(log (I/I
i))].Measure the known sample of content in advance, set up the funtcional relationship of sample content and absorbance, utilize this funtcional relationship to calculate the content of measuring element in the sample according to the absorbance that sample produces.
Summary of the invention
Adopt glow discharge atomization, the atom that sample (i.e. the negative electrode of discharge) sputters coexists with variforms such as ground state atom, excited atom and ions.At this moment, the consistent wavelength of the luminous complete and light source that this element of atomic absorption detecting is used of the excited atom of tested element adopts the accurately luminous variation that sees through aura atomizer front and back of measurement light source of traditional atomic absorption metering system.In order to realize the accurate measurement of aura atomization atomic absorption, the present invention proposes a kind of measuring method of using the aura atomizer to measure atomic absorption, has successfully solved this problem.
The measuring method of a kind of atomic absorption provided by the invention, this method comprises the steps: that through proofreading and correct the luminous method of carrying out the atomic absorption measurement of tested element in the aura atomizer aura atomizer and light source adopt the pulse power supply of different frequency; Gather the signal I of light source luminescent respectively
0, the glow discharge pulse luminous signal I
GSignal I with light source luminescent pulse and glow discharge led pulse when overlapping
H, the light source optical signal transmissive of then proofreading and correct behind the aura luminous signal is I
H-I
G, calculate absorbance A=logI that tested element produces in the aura atomizer
0/ (I
H-I
G), calculate the content of tested element according to the absorbance of the funtcional relationship of absorbance and tested constituent content and sample.
Adopt respectively in aura atomizer power supply pulse, light source power supply pulse and power supply pulse that both are overlapping and gather photosignal down, in order to obtain the light source optical signal transmissive behind the correction aura luminous signal.
Aura atomizer and light source can adopt the DC pulse power supply.The line frequency of the frequency ratio light source of aura atomizer power supply is high; Every pulse that is separated with a light source between certain and aura pulse complete overlapping or overlap; For example the frequency of aura atomizer power supply is 2 times of said light source pulse glow frequencies; The pulse width of aura atomizer power supply is identical or inequality with the pulse width of hollow cathode lamp power supply, and the pulse width of aura atomizer power supply can be greater than the width of light source pulse, also can be less than the width of light source pulse; Such as one in two the adjacent pulses that can adopt aura atomizer power supply synchronous with light source pulse, two synchronous pulses are fully overlapping or overlap, another adjacent pulse and light source pulse are not overlapping fully.
Adopt gate technology to gather the signal I of light source luminescent respectively
0, the aura power pulse signal I
GSignal I with light source pulse and aura power pulse when overlapping
HProofread and correct the luminous back of aura atomizer and calculate absorbance; Measure the sample of known content in advance; Set up the funtcional relationship of tested constituent content and absorbance A in the sample,, set up the funtcional relationship between absorbance and tested constituent content through measuring the absorbance of the known sample of content; Measure the absorbance of the tested element of unknown content in the sample, calculate the measuring method of tested constituent content in the sample according to the funtcional relationship between absorbance and tested constituent content.
Said glow discharge atomizer places on the light source light path.
Said glow discharge atomizer is a device of realizing tested atoms of elementsization in the sample.
Said glow discharge atomizer comprises that both sides have the cavity of the band vacuum system of the quartz window that can make light transmission, have an anode and a negative electrode that serves as with the conduction sample; Keep between negative electrode and anode by power supply and to discharge, realize the device of tested atoms of elementsization in the sample.
Said light source can be line sources such as hollow cathode lamp, electrodeless discharge lamp, also can be the incandescent luminous continuous light source through mechanical modulation.
Beneficial effect of the present invention is: adopt the accurately luminous variation that sees through aura atomizer front and back of measurement light source of atomic absorption measuring method of the present invention, realize correct atomic absorption measurement.Adopt atomic absorption measuring method of the present invention can accurately calculate the content of tested element in the sample.
Description of drawings
Fig. 1 is the frequency and the time sharing sampling synoptic diagram of aura atomizer power supply pulse;
Fig. 2 glow discharge atomizer synoptic diagram;
Fig. 3 is a glow discharge atomizer side view synoptic diagram;
Fig. 4 is a glow discharge atomizer side view synoptic diagram (band seal closure);
Label among the figure: 1. hollow cavity; 2. quartzy window; 3. mounting seat; 4 bleeding points; 5 vacuum meter interfaces; 6. air intake opening; 7. anode (connecing positive supply); 8 samples (connecing negative supply); 9. the hollow cathode beam of light; 10. sample platform; 11. O-ring seal; 12. seal closure; 13. electric contact; 14. via.
Embodiment
Below in conjunction with embodiment the present invention is described further:
The used glow discharge atomizer of the inventive method is as shown in Figure 2, side view such as Fig. 3 or shown in Figure 4, and it comprises:
A hollow cavity 1 is provided with the air intake opening 6 that bleeding point that an ability is connected with vacuum pump 4, vacuum meter interface 5 that ability is connected with vacuum meter and an ability are connected with supply air line on it;
Two suprasil windows 2, its sealing-in is at the two ends of said hollow cavity 1;
An anode 7, its connect said hollow cavity 1 inside and outside and with said hollow cavity 1 insulation sealing-in, this anode 7 links to each other with the positive pole of power supply;
A mounting seat 3, it links to each other with said hollow cavity 1 downside;
A sample platform 10, its be arranged at said hollow cavity 1 the top and with said hollow cavity 1 sealing-in, there is a via 14 at the center of this sample platform 10 as being communicated with the inside and outside passage of said hollow cavity 1;
Discharging surface part and atmospheric isolation that " O " RunddichtringO 11 makes sample 8 are set between said sample 8 and said sample platform 10, and said sample 8 links to each other with power cathode; Perhaps with the seal closure 12 that has " O " RunddichtringO 11 sample 8 is covered in the said seal closure 12, make sample 8 and atmospheric isolation, said sample 8 contacts with said seal closure 12, and said seal closure 12 is connected with the negative pole of power supply.
Keep between negative electrode and anode by said power supply and to discharge, realize tested atoms of elementsization in the sample.Place the enterprising capable atomic absorption of light source light path to measure said glow discharge atomizer.
The present invention adopts with the atomic absorption spectrophotometer (AAS) of hollow cathode lamp as light source and glow discharge atomizer and carries out the atomic absorption measurement.The influence that the stimulated luminescence of determined element is measured atomic absorption during for fear of glow discharge; Adopt the hollow cathode lamp of DC pulse power supply mode; Adopt direct current pulse power source to drive the aura atomizer simultaneously; Take time sharing sampling technology on out of phase; Measurement is measured the luminous intensity of glow discharge again as luminous both the intensity level sum of the luminous and glow discharge of the hollow cathode lamp of light source, from the former measured value, deducts the latter; See through the light intensity behind the aura atomizer as the hollow cathode lamp source, the ratio that hollow cathode lamp (aura atomizer off-position) and this hollow cathode lamp source when the aura atomizer of glow discharge does not take place are seen through the light intensity of aura atomizer duty is taken the logarithm and is obtained the absorbance that tested element produces in the aura atomizer.
Present embodiment uses the direct current square-wave pulse power source to drive hollow cathode lamp, and is as shown in Figure 1.Hollow cathode lamp sends pulsed light with the power supply impulsive synchronization, every pulse that is separated with a light source between certain and aura pulse overlapping fully.The duty of aura atomizer is produced by the ground state atom of analytical element by the cathodic sputtering effect, and meanwhile a part of tested atoms of elements is excited luminous.Because this luminous wavelength is identical with the wavelength of hollow cathode lamp light source luminescent, because of the luminous overlapping with it of tested element in the aura atomizer can not accurately be measured the degree of absorption of the ground state atom of tested element to light source luminescent.In order to deduct the luminous of tested element in the aura atomizer, present embodiment adopts direct current pulse power source to drive the aura atomizer.As shown in Figure 1, the frequency of aura atomizer power supply pulse is 2 times of hollow cathode lamp power pulse, and pulse width is less than the pulse width of hollow cathode lamp power supply.Two adjacent pulses are in respectively and the complete overlapping and complete nonoverlapping state of the pulse of hollow cathode lamp.
For the luminous photosignal when overlapping of the luminous photosignal of tested element in the photosignal of gathering independent hollow cathode lamp respectively, the independent aura atomizer and hollow cathode lamp and aura, adopt the time resolution Sampling techniques.The phase place of sampling gate pulse is as shown in Figure 1, T
1Constantly have only hollow cathode lamp luminous, what collected this moment is the independent luminous signal of hollow cathode lamp, and note is made I
0T
2Constantly the luminous signal of luminous and the hollow cathode lamp of aura atomizer is overlapping, and what collect is the luminous sum of tested element in transmitted light and the aura atomizer after the luminous determined element absorption of hollow cathode lamp, remembers and makes I
HT
3Constantly have only the luminous of tested element in the aura atomizer, the luminous signal in the aura atomizer that collect this moment, note is made I
GFrom I
HIn deduct I
GPromptly be the transmitted light after hollow cathode lamp passes through the determined element absorption of aura atomizer, note is made I
i, i.e. I
i=I
H-I
G, to (I
0/ I
i) value take the logarithm log (I
0/ I
i)=A obtains measuring in the aura atomizer absorbance A that element produces.The tested atoms of elements density in the zone that the absorbance A and the hollow cathode beam of light pass through has proportional relationship; Measure the sample of known content in advance; Set up the funtcional relationship of tested constituent content and absorbance A in the sample, the absorbance A that produces according to unknown sample can calculate the content of tested element in the unknown sample.
Claims (10)
1. the measuring method of an atomic absorption is characterized in that this method through proofreading and correct the luminous method of carrying out the atomic absorption measurement of tested element in the aura atomizer, comprises the steps: that aura atomizer and light source adopt the pulse power supply of different frequency; Gather the signal I of light source luminescent respectively
0, the glow discharge pulse luminous signal I
GSignal I with light source luminescent pulse and glow discharge led pulse when overlapping
H, the light source optical signal transmissive of then proofreading and correct behind the aura luminous signal is I
H-I
G, calculate absorbance A=logI that tested element produces in the aura atomizer
0/ (I
H-I
G), calculate the content of tested element according to the absorbance of the funtcional relationship of absorbance and tested constituent content and sample.
2. method according to claim 1 is characterized in that: adopt the photosignal under the power supply of aura atomizer pulse, light source power supply pulse and both overlapping power supply pulses respectively, proofread and correct the aura luminous signal, in order to obtain the light source optical signal transmissive.
3. method according to claim 1 is characterized in that: aura atomizer and light source adopt the DC pulse power supply.
4. method according to claim 1 is characterized in that: the line frequency of the frequency ratio light source of aura atomizer power supply is high, every pulse that is separated with a light source between certain and aura pulse complete overlapping or overlap.
5. method according to claim 1 is characterized in that: the pulse width of aura atomizer power supply is identical or inequality with the pulse width of light source.
6. method according to claim 1 is characterized in that: adopt gate technology to gather the signal I of light source luminescent respectively
0, the aura power pulse signal I
GSignal I with light source pulse and aura power pulse when overlapping
H
7. method according to claim 1 is characterized in that: said glow discharge atomizer places on the light source light path.
8. method according to claim 1 is characterized in that: said glow discharge atomizer is a device of realizing tested atoms of elementsization in the sample.
9. method according to claim 1; It is characterized in that: said glow discharge atomizer comprises that both sides have the cavity of the band vacuum system of the quartz window that can make light transmission, have an anode and a negative electrode that serves as with the conduction sample; Keep between negative electrode and anode by power supply and to discharge, realize the device of tested atoms of elementsization in the sample.
10. method according to claim 1 is characterized in that: said light source is line sources such as hollow cathode lamp, electrodeless discharge lamp, or the incandescent luminous continuous light source of process mechanical modulation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103674866A (en) * | 2013-11-26 | 2014-03-26 | 上海光谱仪器有限公司 | Optical system used for multielement atomic absorption test and test method |
| CN106338478A (en) * | 2016-11-17 | 2017-01-18 | 云南民族大学 | Measurement method for lead speciation in cigarette smoke |
| CN106383164A (en) * | 2016-11-17 | 2017-02-08 | 云南民族大学 | Cigarette smoke arsenic form determination method |
| CN111665204A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Water body nitrogen and phosphorus element content analysis based on photoelectric characteristics of photoresistor |
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| US3924950A (en) * | 1974-09-16 | 1975-12-09 | Perkin Elmer Corp | Atomic absorption spectroscopy with background correction |
| CN2407345Y (en) * | 2000-02-25 | 2000-11-22 | 高英奇 | High performance hollow cathode electric source for background calibration of self absorption effect |
| CN2482075Y (en) * | 2001-04-25 | 2002-03-13 | 王澎蛟 | Atomic absorption spectrophotometer |
| CN2646699Y (en) * | 2003-10-08 | 2004-10-06 | 北京吉天仪器有限公司 | Equipment for deducting shifting and pulsing of light source for atomic fluorescence spectrometer |
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2010
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3924950A (en) * | 1974-09-16 | 1975-12-09 | Perkin Elmer Corp | Atomic absorption spectroscopy with background correction |
| CN2407345Y (en) * | 2000-02-25 | 2000-11-22 | 高英奇 | High performance hollow cathode electric source for background calibration of self absorption effect |
| CN2482075Y (en) * | 2001-04-25 | 2002-03-13 | 王澎蛟 | Atomic absorption spectrophotometer |
| CN2646699Y (en) * | 2003-10-08 | 2004-10-06 | 北京吉天仪器有限公司 | Equipment for deducting shifting and pulsing of light source for atomic fluorescence spectrometer |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103674866A (en) * | 2013-11-26 | 2014-03-26 | 上海光谱仪器有限公司 | Optical system used for multielement atomic absorption test and test method |
| CN103674866B (en) * | 2013-11-26 | 2016-05-11 | 上海光谱仪器有限公司 | A kind of optical system for multielement atomic absorption detecting and assay method |
| CN106338478A (en) * | 2016-11-17 | 2017-01-18 | 云南民族大学 | Measurement method for lead speciation in cigarette smoke |
| CN106383164A (en) * | 2016-11-17 | 2017-02-08 | 云南民族大学 | Cigarette smoke arsenic form determination method |
| CN106338478B (en) * | 2016-11-17 | 2019-01-08 | 云南民族大学 | A kind of measuring method of cigarette smoke Lead speciation |
| CN106383164B (en) * | 2016-11-17 | 2019-01-08 | 云南民族大学 | A kind of measuring method of form of arsenic in cigarette smoke |
| CN111665204A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Water body nitrogen and phosphorus element content analysis based on photoelectric characteristics of photoresistor |
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| CN102539351B (en) | 2014-08-27 |
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Effective date of registration: 20160829 Address after: Yang Yanlu 101407 Beijing city Huairou District Yanqi Economic Development Zone No. 88 Patentee after: National standard (Beijing) inspection & Certification Co., Ltd. Patentee after: Puxi General Instrument Co., Ltd., Beijing Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals Patentee before: Puxi General Instrument Co., Ltd., Beijing |