WO2009090608A1 - Spectrométrie d'absorption atomique - Google Patents

Spectrométrie d'absorption atomique Download PDF

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Publication number
WO2009090608A1
WO2009090608A1 PCT/IB2009/050138 IB2009050138W WO2009090608A1 WO 2009090608 A1 WO2009090608 A1 WO 2009090608A1 IB 2009050138 W IB2009050138 W IB 2009050138W WO 2009090608 A1 WO2009090608 A1 WO 2009090608A1
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Prior art keywords
aas
radiation
operable
array
pixels
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Dmitri Katskov
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Tshwane University of Technology
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Tshwane University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/3103—Atomic absorption analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces

Definitions

  • THIS INVENTION relates generally to atomic absorption spectrometry and particularly to an atomic absorption spectrometer and a method of atomic absorption spectrometry.
  • the Inventor is aware that, in atomic absorption spectrometry (or spectroscopy), electromagnetic radiation is directed at a sample, the composition of which is to be analysed. The presence and concentration of a particular element is determined based on an amount of radiation absorbed by the sample vapour at a particular wavelength. Each element has a characteristic absorption wavelength (or combination of wavelengths) which uniquely differentiates it from other elements.
  • electromagnetic radiation e.g. light
  • a linear spectrum light source passes through the cavity of a fast heated graphite tube atomiser [1 ].
  • the sample is fully vaporised in an argon atmosphere from the wall or special substrate (platform) in the centre of the tube.
  • the cavity serves as absorption volume, and the sample vapour is transported from the centre to the open ends of the tube on account of diffusion or argon flow.
  • Radiation corresponding to specific resonance line A 1 in the spectrum of the element to be determined (analyte) is monitored as electric output of the detector, I 0 (A 1 ) and I ,(A 1 ) , before and during the vaporisation pulse, respectively.
  • Time dependent linear absorbance A 1 (A j ) IOg[I 0 (A 1 )II 1 (A 1 )] is used to characterise an amount of atomic vapour of the analyte N 1 in the vapour phase.
  • N 1 At low absorbance ( A t ( ⁇ ⁇ ) ⁇ 03 ⁇ 0A for the most sensitive atomic lines) N 1 is proportional to A 1 ; above that limit function A 1 (A 1 ) vs. N 1 depends on a structure of the spectral line and characteristics of the radiation source. Total amount of the analyte in the sample N 0 within the proportionality range
  • a 1 (A 1 ) vs. N 1 is thus characterised by the absorption peak area:
  • ⁇ is residence time of atoms in the absorption volume. Calibration of the measurements is performed using the reference material with known content N 0 (parameter ⁇ is considered to be equal for the analyte from the sample and reference material).
  • ETAAS As the most popular technique for determination of trace elements has been reduced owing to fast development and broad distribution of ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometry) and ICP-MS (Inductively Coupled Plasma Mass Spectrometry) instrumentation for multi-element analysis.
  • ICP-OES Inductively Coupled Plasma Optical Emission Spectrometry
  • ICP-MS Inductively Coupled Plasma Mass Spectrometry
  • a concentration of analyte atoms in the absorption volume is measured using absorption at wavelength ⁇ within the absorption proiWe, A 1 (A) ⁇ A(p ⁇ ,n) , where p and n are pixel and scan numbers respectively, and p ⁇ is the pixel between p +w and p. w adjacent the
  • Equation (3) permits correction of the non-specific spectral background next to 1 10 the absorption line, A(p ⁇ m ⁇ w ,n) and use of the sum of all scans for characterisation of full amount of the analyte in the sample,
  • the lines of several elements can be detected with an HR instrument and used for true simultaneous determination only if they belong to the selected narrow spectral area (0.5 nm for the instrument described in [4]), which can be scanned fast to provide large
  • a spectral range between 200 and 400 nm is needed where the main sensitive resonance lines normally used in AAS, are situated. In this spectral area the number of CCD pixels should be large enough to resolve main absorption
  • the inventor wishes to overcome or at least alleviate the sequential sampling drawback of AASs.
  • an atomic absorption spectrometer which includes: an electromagnetic (EM) radiation emitter operable to emit a radiation continuum across a broad spectrum;
  • EM electromagnetic
  • a detector arrangement including a spectrograph and an array of photosensitive pixels, the spectrograph being operable to spread EM radiation across substantially the entire broad spectrum at once to the array of pixels to measure radiation across substantially the entire broad spectrum; an electro-thermal atomiser operable to vaporise an analyte; and
  • control module operable to calculate and linearise the function of absorbance against concentration of the analyte vapour in the atomiser based on the measured radiation.
  • broad spectrum refers to a 180 spectral range (e.g. 200 nm) which includes absorption wavelengths of a plurality of elements
  • narrow spectrum refers to a spectral range (e.g. 1 nm) centred at or near the absorption line of a specific element, with a small tolerance either side.
  • the broad spectrum may be at least one, and optionally two or more, order of magnitude wider than the narrow spectrum.
  • the AAS may be a low or high resolution AAS. It is to be appreciated that the pixel array of a low resolution, wide spectrum AAS in accordance with the invention may have a similar number of pixels as that of a high resolution, narrow spectrum AAS in accordance with the prior art.
  • the pixel array itself may be similar to those of prior art AASs.
  • the pixel array (of the AAS in accordance with the invention) may, for example, include between 3000 and 4000 pixels.
  • the EM radiation emitter may include a single continuum light 195 source, which may, for example, have a broad emission spectrum of at least
  • the spectrograph may be configured to spread substantially the entire broad spectrum across the pixel array in relatively large increments per
  • the wavelength increment may be approximately 0.05 nm.
  • the AAS may include a housing which defines therein an 205 absorption volume and which accommodates, in use, a vapour sample to be analysed. The AAS may then measure the concentration of one or more elements comprising the vapour sample.
  • the AAS may include an electronic processor.
  • the control module 210 may be a conceptual module which corresponds to a functional task performed by the processor.
  • the AAS may include a machine-readable medium, main memory, and/or a hard disk drive, which carries a set of instructions to direct the operation of the processor, the set of instructions for example being in the form of a computer program. 215
  • the control module (or other controller operatively connected to the array of pixels) may be operable to take a measurement from the array of pixels at a plurality of periodic time intervals, e.g. 4 ms, for a pre-defined or pre-definable period, e.g. 1 s to 3 s. 220
  • the processor may be one or more microprocessors, controllers, digital signal processors (DSPs), or any other suitable computing device, resource, hardware, software, or embedded logic.
  • DSPs digital signal processors
  • the control module need not necessarily be 225 consolidated into the same device as the EM radiation emitter and the detector arrangement.
  • the control module may be hosted by a remote computer which is connectable to the device housing the EM radiation emitter and the detector arrangement.
  • an AAS system which includes: an AAS device which includes an electromagnetic (EM) radiation emitter operable to emit a radiation continuum across a broad spectrum;
  • EM electromagnetic
  • a detector arrangement including a spectrograph and an array of photo-sensitive pixels, the spectrograph being operable to spread EM radiation across substantially the entire broad spectrum at once to the array of pixels to measure radiation across substantially the entire broad spectrum;
  • an electro-thermal atomiser operable to vaporise an analyte
  • a computer in communication with the AAS device, the computer being operable to receive from the AAS device a communication indicative of measured radiation and including a control module operable to calculate and linearise absorbance based on the measured radiation.
  • the control module (whether part of the AAS defined above or part of the AAS system defined above) may be operable to calculate absorbance from the radiation measured by respective pixels. More particularly, the control module may be operable to square respective calculated absorbances
  • the control module may be configured to apply at least one of the equations (or mathematical equivalents thereof) selected from the group 255 composed of equations (10) to (17) defined below.
  • the definition and description of the invention assumes a high degree of atomisation and similar residence time of atoms evolved from the sample and reference material in the absorption volume.
  • the array of pixels may be a provided by one selected from the group comprising a Charge Coupled Device (CCD) array (or at least be connected to a CCD arrangement) and a Diode Array Detector.
  • Contemporary linear CCD array may consist of about 4000 pixels, which can
  • the CCD array of pixels may detect the
  • the wavelength increment would be 0.05 nm per pixel, that is more than 25 times higher than that in HR
  • a 275 method of atomic absorption spectrometry including: directing an EM radiation emitter at a vapour sample to be analysed, the emitter being operable to emit EM radiation across a broad spectrum; spreading substantially the entire broad spectrum at once across an array of pixels,
  • the method may include pulse-vaporisation and atomisation of the 285 sample.
  • the method may include summing a plurality of sequential linearised absorbances to determine, or at least provide an indication, of the amount of an element in a sample. 290
  • the calculation and linearising of the absorbance and summation of the linearised absorbance may be done automatically and electronically, for example by a control module as defined above. At least some of the method steps may be repeated periodically at intervals (e.g. 10 ms) for a duration of 295 an atomisation pulse (e.g. 1 s to 3 s).
  • the method may include a prior step of analysing a reference sample.
  • the calculation, linearising and summing may be done in accordance with at least one of the equations (or mathematical equivalents 300 thereof) selected from the group composed of equations (10) to (17) defined below.
  • the invention extends to a machine-readable medium having stored thereon a set of instructions which, when executed by a machine, 305 causes the machine to perform a method as above defined.
  • A' t ( ⁇ ) JF( ⁇ ')A t ( ⁇ - ⁇ ')d ⁇ ' . (6)
  • absorbance should be proportional to the wavelength integrated absorbance S 1 .
  • the absorbance maximum should be reduced, compared to that for HR instrument, approximately proportional to the respective resolution ratio, depending on the half width of the instrumental transmittance profile F(A) . Accordingly, a higher amount of the analyte
  • linearisation (9) can be automatically introduced into the absorbance data for each pixel p ⁇ .
  • N t a p - [A(p ⁇ , n)f - sign[A(p ⁇ , n)] (10) is suggested, where sign is a function equal to +1 or -1 , if A'(p ⁇ ,n) > or ⁇ 0, respectively, and a p is a sensitivity coefficient for the particular pixel. For the signals above the noise level, (10) is equal to (9). Otherwise, short noise 360 causes random deviations similar to that in the traditional or HR-CS ETAAS.
  • the amount of a particular element N Oe in the sample can be found using linearisation (10) and summation of absorbance data at absorption maximum (at the pixel p M ),
  • BG correction can be performed using the admission that average output /( ⁇ ⁇ A , «) of pixels P 21n+1 , and p ⁇ m _ A on the distance ⁇ from p ⁇ m within the line profile is equal to I o (p ⁇ m ,n) .
  • An AAS in accordance with the invention provides true simultaneous multi-element determination using a low resolution CCD spectrometer, which broadens the absorption lines more than 10-20 times compared to natural line width at the ET vaporisation experimental conditions.
  • the determination of several elements may be performed using the 410 information obtained during sample vaporisation within a single run of temperature programme and calibration data obtained independently.
  • Figure 1 shows a schematic view of an AAS system in accordance with the invention
  • Figure 2 shows a flowchart of a method in accordance with the invention
  • Figures 3 and 4 show, respectively, the measured CCD output and peak atomic absorption for the sampled solution 10 ppm Ag and 5 ppm Na and Mg 425 in water;
  • Figure 5 shows absorption spectrum corresponding to Figure 3 after linearisation of the measurements according to equation (10);
  • Figure 6 shows profile of absorption line Ag 328.068 before and after linearisation of the measurements (a and b, respectively);
  • Figures 9A and 9B show Mn (64 ppb) atomic absorption at Mn 279.482 nm spectral line calculated according to equations (12) and (14) without (A) and with (B) correction to short noise;
  • Figure 10 shows spectrum of integrated linearised absorbances for the solution 8 ppm (part per million) Ag, Bi, Cd, Ga, In, Mn, Mg, Na, K, Pb and Tl; 440 and Figures 1 1 and 12 show the determination ranges for Cd, Ga, In, Tl and Ag, Bi, Mn, Pb, respectively, in the mixed solutions of equal amounts of Ag, Bi, Cd, Ga, In, Mn, Mg, Na, K, Pb, and Tl.
  • reference numeral 100 generally indicates an AAS system in accordance with the invention.
  • the AAS system 100 450 comprises an AAS device 102 and a computer 120 operatively connected to the AAS device 102 via a communication link 1 12.
  • the AAS device 102 has a light source 104 which is operable to emit EM radiation having a continuum spectrum in a range, for example, 200
  • the radiation is directed at an absorption cavity of an atomiser
  • the atomiser 106 includes a graphite furnace (not illustrated) to vaporise a sample. Once the radiation has passed through the absorption cavity, it is directed to a spectrometer 108 which spreads the entire broad spectrum at once across an array of pixels 1 10.
  • the computer 120 has a processor 122 and a memory module 126.
  • the processor 122 has a control module 124 which is operable to calculate
  • the computer 120 further has a display 130 which is operable to provide an indication to a user of the system 100 of the elements determined
  • a high-level flow diagram illustrates a method of atomic absorption spectrometry indicated by reference numeral 475 200.
  • the method 200 includes directing, at block 202, EM radiation having continuous broad spectrum at a sample to be analysed. Once the radiation has passed through the sample vapour, the entire radiation is spread, at block 204, at once across an array of pixels. The radiation received by the array of pixels is measured, at block 206, across the entire broad spectrum and the
  • the elemental composition of the sample is then displayed, at 485 block 210. If desired, a reference sample can be analysed, at block 201 , for calibration purposes.
  • the method 200 may conveniently be implemented on the system 100, although its application is not necessarily limited to such a system. 490
  • ballast design of the atomiser and respective power supply provided a heating rate of the furnace 10 K/ms and temperature stabilisation at the pre-set level; the ballast delayed the vaporization of the analyte thus providing vapour enter in the absorption volume at high temperature.
  • Optimal sampling volume for the fast heated ballast atomiser was 10 ⁇ l_. 510
  • the measurements included two runs of temperature program (refer to Table 1 ) with and without sampling the sample solution, spectra acquisition during the atomisation step, and sequential transfer of the CCD outputs with and without sample ( I(p,n) and I 0 (p,n) , respectively) to
  • 605 15 to 17 is to be composed from the measurement data for each single element.
  • matrix inversion method [10] only one line of each element could be presented in the reference matrix.
  • Table 3 The example of matrix composed for the constituents of the tested mixture is presented in Table 3.
  • the diagonal members of the matrix characterise the 610 determination sensitivity at most sensitive for each particular element wavelengths (Table 2, column 3).
  • the example shows that the invention provides the methodology of fast simultaneous determination of plurality of elements within broad concentration range and limits of detection close to those in traditional flame
  • the concentration range can be still enlarged and limits of detection reduced an account of radiation source, more efficient in the short wavelength area (e.g. similar to that used in HR CS AAS [4]) and increase of 630 data collection frequency using special software.
  • the determination errors caused by residual memory can be reduced by optimisation of temperature program and gas flow during the cleaning step.
  • electrothermal atomisation should also permit getting rid of specific safety problems connected with storage and use of flammable gases and open the way to miniaturisation of the AAS instrumentation.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

La présente invention concerne, d'une part un spectromètre d'absorption atomique ou 'AAS' pour 'Atomic Absorption Spectrometer' (102), d'autre part un système AAS (100), et enfin un procédé (200) de spectrométrie d'absorption atomique. L'AAS (102) comporte un émetteur (104) de rayonnement électromagnétique (EM) servant à l'émission d'un continuum dans toute l'étendue d'un large spectre, et un dispositif détecteur comprenant un spectrographe (108) et une matrice de pixels photosensibles (110). Le spectrographe (108) a pour fonction d'étaler instantanément le rayonnement électromagnétique sur toute la largeur du spectre en direction de la matrice de pixels (110) de façon à mesurer le rayonnement sur toute la largeur du spectre. L'AAS comporte également un atomiseur électrothermique (106) servant à vaporiser un analysat, et un module de commande (124) servant à calculer puis à linéariser, sur la base du rayonnement mesuré, la fonction de l'absorbance par rapport à la concentration de la vapeur d'analysat dans l'atomiseur (106).
PCT/IB2009/050138 2008-01-15 2009-01-15 Spectrométrie d'absorption atomique Ceased WO2009090608A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012006782A1 (fr) * 2010-07-15 2012-01-19 北京吉天仪器有限公司 Procédé spectral de fluorescence atomique par vaporisation électrothermique et spectromètre pour la détermination du cadmium
CN103411909A (zh) * 2013-09-03 2013-11-27 江苏沥泽生化科技有限公司 一种检测纳米银敷料中银含量的方法
CN110213509A (zh) * 2019-05-27 2019-09-06 浙江工业大学 一种ccd自适应积分时间与频谱可视化系统
WO2021082117A1 (fr) * 2019-10-29 2021-05-06 长沙开元弘盛科技有限公司 Dispositif et procédé de mesure simultanée du mercure, du cadmium, du zinc et du plomb
CN114660008A (zh) * 2022-04-20 2022-06-24 中国市政工程东北设计研究总院有限公司 一种校正火焰原子吸收法干扰的方法

Citations (2)

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US3565567A (en) * 1968-06-25 1971-02-23 Bausch & Lomb Method of and apparatus for measuring the presence and/or concentration of an element in an atomic vapor
US5315528A (en) * 1991-12-03 1994-05-24 The Perkin-Elmer Corporation Method of, and apparatus for, absorbance correction in atomic absorption spectroscopy

Patent Citations (2)

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US3565567A (en) * 1968-06-25 1971-02-23 Bausch & Lomb Method of and apparatus for measuring the presence and/or concentration of an element in an atomic vapor
US5315528A (en) * 1991-12-03 1994-05-24 The Perkin-Elmer Corporation Method of, and apparatus for, absorbance correction in atomic absorption spectroscopy

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Title
HARNLY JAMES M: "Future of atomic absorption spectrometry: A continuum source with a charge coupled array detector", JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, ROYAL SOCIETY OF CHEMISTRY, CAMBRIDGE, GB, vol. 14, no. 2, 1 February 1999 (1999-02-01), pages 137 - 146, XP007908568, ISSN: 0267-9477 *
SCHUETZ M ET AL: "Continuum source-atomic absorption spectrometry using a two-dimensional charge coupled device", SPECTROCHIMICA ACTA. PART B: ATOMIC SPECTROSCOPY, NEW YORK, NY, US, US, vol. 55, no. 12, 15 December 2000 (2000-12-15), pages 1895 - 1912, XP007908610, ISSN: 0584-8547 *
WELZ B ET AL: "High-Resolution Continuum-Source Atomic Absorption Spectrometry What Can We Expect?", JOURNAL OF THE BRAZILIAN CHEMICAL SOCIETY, SAO PAULO, BR, vol. 14, no. 2, 1 March 2003 (2003-03-01), pages 220 - 229, XP007908579, ISSN: 0103-5053 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012006782A1 (fr) * 2010-07-15 2012-01-19 北京吉天仪器有限公司 Procédé spectral de fluorescence atomique par vaporisation électrothermique et spectromètre pour la détermination du cadmium
CN103411909A (zh) * 2013-09-03 2013-11-27 江苏沥泽生化科技有限公司 一种检测纳米银敷料中银含量的方法
CN110213509A (zh) * 2019-05-27 2019-09-06 浙江工业大学 一种ccd自适应积分时间与频谱可视化系统
CN110213509B (zh) * 2019-05-27 2021-05-18 浙江工业大学 一种ccd自适应积分时间与频谱可视化系统
WO2021082117A1 (fr) * 2019-10-29 2021-05-06 长沙开元弘盛科技有限公司 Dispositif et procédé de mesure simultanée du mercure, du cadmium, du zinc et du plomb
US11754494B2 (en) 2019-10-29 2023-09-12 Changsha Kaiyuan Hongsheng Technology Co., Ltd Device and method for simultaneously measuring mercury, cadmium, zinc and lead
CN114660008A (zh) * 2022-04-20 2022-06-24 中国市政工程东北设计研究总院有限公司 一种校正火焰原子吸收法干扰的方法

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