CN102338745B - Electro-thermal vaporization atomic fluorescence spectrometry method and spectrometer used for determining cadmium - Google Patents
Electro-thermal vaporization atomic fluorescence spectrometry method and spectrometer used for determining cadmium Download PDFInfo
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- CN102338745B CN102338745B CN2010102273791A CN201010227379A CN102338745B CN 102338745 B CN102338745 B CN 102338745B CN 2010102273791 A CN2010102273791 A CN 2010102273791A CN 201010227379 A CN201010227379 A CN 201010227379A CN 102338745 B CN102338745 B CN 102338745B
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Abstract
The invention discloses an electro-thermal vaporization atomic fluorescence spectrometry method and a spectrometer used for determining cadmium. An atomizer of the electro-thermal vaporization atomic fluorescence spectrometer comprises an atomizing apparatus and a collecting trap. The collecting trap is composed of a tungsten filament or a molybdenum filament, a support, a housing and a power source. A sealed space is formed by the housing and the support. The tungsten filament or the molybdenum filament is arranged on the support. The tungsten filament or the molybdenum filament is positioned in the sealed space formed by the housing and the support. An inlet and an outlet are arranged on the housing. The electro-thermal vaporization atomic fluorescence spectrometry method used for determining cadmium comprises steps that: a sample requiring testing is dried in air, and is cinerated, such that ash is obtained; under an argon atmosphere, the ash is heated to 1600 to 2000 DEG C, and the obtained vapor contacts the tungsten filament or the molybdenum filament; under an atmosphere of hydrogen and argon, the temperature of the tungsten filament or the molybdenum filament is increased to 1600 to 2000 DEG C, cadmium atoms are released, and the content of the cadmium atoms are analyzed by using a fluorescence spectrometry method. With the electro-thermal vaporization atomic fluorescence spectrometry method and the spectrometer used for determining cadmium provided by the invention, matrix interference can be effectively eliminated, and accurate measuring of cadmium can be realized.
Description
Technical field
The present invention relates to a kind of Electrothermal evaporation atomic fluorescence spectroscopic methodology and spectrometer of measuring cadmium.
Background technology
Because large amount of sewage is irrigated and abuse fertilizer, China has been subject to serious cadmium (Cd) and has polluted, the degree of production " cadmium rice " has been developed in some areas: in the rice that dirty irrigated area, Shenyang produces Cd concentration up to 0.4-1.0 mg/kg, met or exceeded bring out " Itai-itai diseases " on average contain Cd concentration.In view of this, the fast survey technology of Cd has been subject to paying attention to widely in recent years, has developed based on a series of fast determining methods such as biology sensor, colourimetry, enzyme inhibition, galvanochemistry and atomic spectrum.But wherein most methods only can detect heavy metal ion in the solution, still can not avoid the sample pretreatment process of time and effort consuming; And because the impact of matrix is difficult to realize Measurement accuracy that rate of false alarm is higher, although can simplify to a great extent the heavy metals measurement in soil and the agricultural product, can't thoroughly solve this difficult problem.Really can realize the atomic spectrum method heavy metal direct-detection or electric heating evaporation (ETV) or laser ablation (LA) realization Sample introduction in soil and the agricultural product, wherein comparatively ripe electric heating evaporation-inductively coupled plasma atomic emission (ETV-ICPOES), mass spectrum (ETV-ICPMS) or sampling Graphite Furnace Atomic Absorption (GFAAS) technology all are useful on the report that direct injected detects, along with the development of background correction technology and continuous light source technology, the electric heating evaporation direct insertion technique is more and more near practical.But be applied in soil and agricultural product fast detecting field, disturb although above-mentioned technology can suppress matrix to a certain extent, but still be difficult to overcome fully, for comparatively complicated matrix still power institute difficult and.So after using electric heating evaporation as the Sample introduction means, above-mentioned test problems is actual to be exactly to develop a kind of method that can eliminate the matrix interference, with the various complicated substrates of accommodate sample.
Atomic fluorescence spectrophotometry (AFS) method is faster a kind of atomic spectrum technology of China's development, because atomic fluorescence spectrophotometry is simple, overlap of spectral lines is few, so can use dispersionless detection mode, this just makes its apparatus structure greatly simplify, and realizes easily miniaturization, possesses the possibility of Site Detection.But atomic fluorescence spectrometer commonly used is based on hydride generation (HG) Sample introduction technology at present, the Electrothermal evaporation atomic fluorescence that sees bibliographical information has and uses graphite furnace to be used for measuring the lead of solution as evaporation and atomizing apparatus, and is used for the report that rear solution heavy metal is cleared up in measurement based on electric heating evaporation-atomic fluorescence (ETV-AFS) of tungsten filament (TC).More than two kinds of devices all possessed the potentiality of ETV direct injected, but still be difficult to thoroughly solve the matrix interference problem.
It is a great problem that is perplexing direct injected atomic spectrum technology that matrix disturbs always, although being alleviated through behind the matrix correction, can not fundamentally address this problem, and need to take other thinking.The solid based on Atomic absorption that has developed since the nineties in last century is surveyed the mercury technology and has been provided a good enlightenment, this technology utilizes sample at pure oxygen or airborne burning and further catalytic combustion, when oxidation operation decomposes, mercury is discharged with atomic state, the mercury of atomic state caught by the adsorbent of gold-supported and and Matrix separation, at last again heating adsorption agent disengages the mercury of catching and is brought in the atomic absorption instrument by carrier gas and detects.This technology has been utilized the very strong noble metal of selectivity to catch trap and has been realized separating of mercury and matrix, thereby has eliminated the matrix interference fully, and this illustrates that online trapping technique should be that very effectively matrix disturbs the elimination means.The online trapping technique that sees at present bibliographical information is used for Cd when measuring, mostly can only catch the free atom that forms in hydride or the flame, and the Cd that catches the electric heating evaporation importing yet there are no report, this mainly is because the Cd of generally electric heating evaporation formation mostly exists with nanoparticle form, can't effectively be captured.
Summary of the invention
The Electrothermal evaporation atomic fluorescence spectroscopic methodology and the spectrometer that the purpose of this invention is to provide a kind of mensuration cadmium of effective elimination matrix interference.
The electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium provided by the present invention is comprised of sampling system, light source, atomizer, light path system, detection system, display device, and wherein: described sampling system comprises electric heating evaporation device and collecting trap; Described collecting trap is comprised of tungsten filament or molybdenum filament, support, outer cover and power supply, and outer cover and support form seal cavity, and tungsten filament or molybdenum filament are arranged on the support, and described tungsten filament or molybdenum filament are arranged in the seal cavity of outer cover and support formation, and outer cover is provided with import and outlet.
The electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium of the present invention, wherein: described electric heating evaporation device is comprised of radome, evaporation boat, electrode, electrode bracket and power supply; Electrode is positioned at the bottom of evaporation boat, be connected with evaporation boat, electrode is arranged on the electrode bracket, power supply is electrically connected with electrode, radome and electrode bracket form seal cavity, and described evaporation boat is arranged in described seal cavity, and radome is connected with electrode bracket is movable, radome is provided with import and outlet, and the outlet of radome links to each other by three-way pipe with the import of the outer cover of collecting trap.
The electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium of the present invention, wherein: the main line of described three-way pipe is provided with the first transfer valve, and the bye-pass of described three-way pipe is provided with the second transfer valve.
The Electrothermal evaporation atomic fluorescence spectroscopic methodology of mensuration cadmium provided by the present invention comprises the steps:
Testing sample is dry, ashing obtain ash content in the air;
Under argon gas atmosphere, described ash content is warmed up to 1600～2000 ℃, the steam that obtains contacts with tungsten filament or molybdenum filament;
Under hydrogen and argon gas atmosphere, the temperature of described tungsten filament or molybdenum filament is elevated to 1600～2000 ℃, discharge the cadmium atom, the content of fluorescent spectroscopy cadmium.
The Electrothermal evaporation atomic fluorescence spectroscopic methodology of mensuration cadmium of the present invention, wherein: under described hydrogen and the argon gas atmosphere, the percent by volume of hydrogen is 10～90%.
Electrothermal evaporation atomic fluorescence spectroscopic methodology and the spectrometer of mensuration cadmium of the present invention, that utilizes cadmium free atom collecting trap high selectivity catches the cadmium free atom, then in reducing atmosphere, the cadmium of catching is disengaged again, can effectively eliminate matrix and disturb, realize the Measurement accuracy of cadmium.
Description of drawings
Fig. 1 is the structural representation of sampling system of the electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium of the present invention.
Embodiment
The electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium of the present invention is comprised of sampling system, light source, atomizer, light path system, detection system, display device; Light source, atomizer, light path system, detection system, display device are all identical with existing fluorescence spectrophotometer; Connection between light source, light path system, detection system, display device, the atomizer is identical with existing atomic fluorescence spectrometer with position relationship, only the structure of sampling system is different, sampling system comprises electric heating evaporation device and collecting trap, and the electric heating evaporation device is comprised of with power supply 16 radome 4, evaporation boat 1, electrode 3, electrode bracket 5; Electrode 3 is positioned at the bottom of evaporation boat 1, is connected with evaporation boat 1, and electrode bracket 5 support electrodes 3, power supply 16 is electrically connected with electrode 3, and radome 4 is fastened and connected with electrode bracket 5, forms seal cavity; Evaporation boat 1 arranges in the seal cavity, radome 4 and 5 movable connections of electrode bracket, and when radome 4 was opened, evaporation boat 1 was exposed in the air, and radome 4 is provided with import 10 and outlet 11; Collecting trap is comprised of tungsten filament or molybdenum filament 6, support 15, outer cover 7 and power supply 17, and outer cover 7 and support 15 are fastened and connected, and forms seal cavity; Support 15 supports tungsten filament or molybdenum filament 6, and tungsten filament or molybdenum filament 6 are arranged in the seal cavity of outer cover 7 and support 15 formation, and outer cover 7 is provided with import 12 and outlet 13; The outlet 11 of radome 4 and the import of outer cover 7 13 link to each other by three-way pipe, and main line is provided with the first transfer valve 8, and bye-pass is provided with the second transfer valve 9.
Sample places the atomic fluorescence spectrometer evaporation boat 1 of mensuration cadmium of the present invention, radome 4 is opened evaporation boat 1 and is exposed in the air, heating evaporation boat 1, make evaporation boat 1 temperature reach 450～600 ℃, with sample drying, ashing, then close radome 4, radome 4 forms seal cavity with electrode bracket 5, argon gas enters from the import 10 of radome 4, and the first transfer valve 8 is opened, and the second transfer valve 9 cuts out, evaporation boat 1 temperature reaches 2000 ℃, Cd in the sample disengages with the form of free Cd atom, enters collecting trap, tungsten filament or molybdenum filament 6 high selectivities catch the Cd free atom; Then the first transfer valve 8 cuts out, the second transfer valve 9 is opened, the mixed gas of hydrogen (10%～90%) and argon gas (10%～90%) is entered by bye-pass, the temperature of tungsten filament or molybdenum filament 6 reaches 1600～2000 ℃, the Cd atom disengages again, is centered around atomizer hollow cathode lamp on every side and excites, and launches fluorescence signal, this signal is through behind the lens focus, and detected system detects through light path system.
Take 10mg Chinese cabbage (GB thing GBW10014) as example, be 41 microgram/kilograms with cadmium in the atomic fluorescence spectrometer working sample of mensuration cadmium of the present invention, within standard value 35 ± 6 microgram/kilograms of this standard substance, high, medium and low (20,40,80 microgram/kilograms) recovery of standard addition of level is all between 90～110%.
Take 10mg ground rice (GB thing GBW (E) 080684) as example, be 7.8 microgram/kilograms with cadmium in the atomic fluorescence spectrometer working sample of mensuration cadmium of the present invention, within standard value 9 ± 4 microgram/kilograms of this standard substance, high, medium and low (20,40,80 microgram/kilograms) recovery of standard addition of level is all between 90～105%.
Above-mentioned two example explanation the method can accurately record the Cd in the solid sample.
Above embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (5)
1. measure the electric heating evaporation atomic fluorescence spectrometer of cadmium, be comprised of sampling system, light source, atomizer, light path system, detection system, display device, it is characterized in that: described sampling system comprises electric heating evaporation device and collecting trap; Described collecting trap is comprised of tungsten filament or molybdenum filament (6), support (15), outer cover (7) and power supply (17), outer cover (7) and support (15) form seal cavity, tungsten filament or molybdenum filament (6) are arranged on the support (15), described tungsten filament or molybdenum filament (6) are arranged in the seal cavity of outer cover (7) and support (15) formation, and outer cover (7) is provided with import (12) and outlet (13).
2. the electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium according to claim 1 is characterized in that: described electric heating evaporation device is comprised of with power supply (16) radome (4), evaporation boat (1), electrode (3), electrode bracket (5); Electrode (3) is positioned at the bottom of evaporation boat (1), be connected with evaporation boat (1), electrode (3) is arranged on the electrode bracket (5), power supply (16) is electrically connected with electrode (3), radome (4) forms seal cavity with electrode bracket (5), described evaporation boat (1) is arranged in described seal cavity, radome (4) and movable connection of electrode bracket (5), radome (4) is provided with import (10) and outlet (11), and the outlet (11) of radome (4) links to each other by three-way pipe with the import (12) of the outer cover (7) of collecting trap.
3. the electric heating evaporation atomic fluorescence spectrometer of mensuration cadmium according to claim 1 and 2, it is characterized in that: the main line of described three-way pipe is provided with the first transfer valve (8), and the bye-pass of described three-way pipe is provided with the second transfer valve (9).
4. measure the Electrothermal evaporation atomic fluorescence spectroscopic methodology of cadmium, comprise the steps:
Testing sample is dry, ashing obtain ash content in the air;
Under argon gas atmosphere, described ash content is warmed up to 1600～2000 ℃, the steam that obtains contacts the cadmium atom of catching wherein with tungsten filament or molybdenum filament;
Under hydrogen and argon gas atmosphere, the temperature of described tungsten filament or molybdenum filament is elevated to 1600～2000 ℃, discharge the cadmium atom, and with the content of atomic fluorescence spectrometry cadmium.
5. Electrothermal evaporation atomic fluorescence spectroscopic methodology according to claim 4, it is characterized in that: under described hydrogen and the argon gas atmosphere, the percent by volume of hydrogen is 10～90%.
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