CN213875430U - Solid organic sample on-line digestion device based on vapor generation-atomic fluorescence spectrometer - Google Patents
Solid organic sample on-line digestion device based on vapor generation-atomic fluorescence spectrometer Download PDFInfo
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- CN213875430U CN213875430U CN202022761282.0U CN202022761282U CN213875430U CN 213875430 U CN213875430 U CN 213875430U CN 202022761282 U CN202022761282 U CN 202022761282U CN 213875430 U CN213875430 U CN 213875430U
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Abstract
The utility model relates to a solid organic sample online digestion device based on vapor generation-atomic fluorescence spectrometer belongs to digestion device technical field. The method solves the technical problems of complex operation, poor repeatability, low accuracy and low analysis efficiency of the prior similar technology. The utility model discloses an online digestion equipment of solid organic sample, including argon gas holding vessel, oxygen holding vessel, absorption liquid holding vessel, reaction vessel, reductant holding vessel and waste liquid collection tank. The digestion device effectively avoids open volatilization loss, transfer loss risk and human operation error in the conventional offline sample treatment, and greatly improves the analysis accuracy, repeatability, analysis flux and sensitivity of the vapor generation-atomic fluorescence spectrometer.
Description
Technical Field
The utility model belongs to the technical field of digestion device, concretely relates to solid organic sample online digestion device based on vapour takes place-atomic fluorescence spectrum appearance.
Background
The vapor generation-atomic fluorescence spectrometer (CVG-AFS) is an analytical instrument combining a vapor generation and sample introduction mode with an atomic fluorescence spectrometer, is mainly used for quantitative analysis of elements of simple substances or compounds capable of forming high-volatility vapor, and mainly comprises more than ten analytical elements such As Hg, As, Se, Te, Sb, Ge, Bi, Pb, Cd, Sn, Zn and the like.
The sample of the vapor generation-atomic fluorescence spectrometer must be in a solution state, so for the analysis of the solid sample, the solid-liquid conversion of the sample is required as in all the solution sampling techniques. In the prior art, the treatment process of a solid sample for element quantitative analysis by using a vapor generation-atomic fluorescence spectrometer comprises the following steps: the solid sample is digested by mineral acid under the condition of normal pressure/high pressure-heating, and then the obtained digestion solution is pre-reduced to obtain a sample solution suitable for the determination of a steam generation-atomic fluorescence spectrometer.
The existing method for digesting the solid sample comprises the following steps: soaking the sample overnight, wet digesting the sample (8h), low temperature acid-dispelling and reducing (8h), masking or interfering with component chemical separation by reagents if necessary, and the like. However, the method is complex to operate, and has the problems of poor analysis repeatability, accuracy and low analysis efficiency due to the non-uniform operation methods of different samples and the difference of levels of analysts.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a solve present solid organic sample and clear up method operation complicacy on line, repeatability is poor, the degree of accuracy and the lower technical problem of analytical efficiency provide a solid organic sample clears up device on line based on vapour takes place-atomic fluorescence spectrometer.
The utility model provides a technical scheme as follows that above-mentioned technical problem took.
The utility model discloses a solid organic sample on-line digestion device based on a vapor generation-atomic fluorescence spectrometer, which comprises an argon storage tank, an oxygen storage tank, an absorption liquid storage tank, a reaction vessel, a reducing agent storage tank and a waste liquid collecting tank;
the reaction container is a container with an opening at the top end, and the opening at the top end is sealed by a sealing plug; a first conveying pipe penetrating through the wall of the reaction vessel is arranged on the side wall of the reaction vessel; the top of the reaction container is provided with a first exhaust pipe and a second exhaust pipe, the first exhaust pipe is communicated with the inner cavity of the reaction container and the atmosphere, and the first exhaust pipe is provided with a first exhaust valve; the second exhaust pipe is communicated with the inner cavity of the reaction container and the steam generation-atomic fluorescence spectrometer, and a second exhaust valve is arranged on the second exhaust pipe; a sample fixing piece is arranged in the reaction container and used for fixing a sample to be detected;
the argon storage tank is communicated with the first conveying pipe through a second conveying pipe, and a first control valve is arranged on the second conveying pipe;
the oxygen storage tank is communicated with the first conveying pipe through a third conveying pipe, and a second control valve is arranged on the second conveying pipe;
the absorption liquid storage tank is communicated with the first conveying pipe through a fourth conveying pipe, and a first peristaltic pump is arranged on the fourth conveying pipe;
the reducing agent storage tank is communicated with the reaction container through a fifth conveying pipe, and a second peristaltic pump is arranged on the fifth conveying pipe;
the waste liquid collecting tank is communicated with the bottom of the reaction container through a sixth conveying pipe, and a third peristaltic pump is arranged on the sixth conveying pipe.
Further, the reaction container is a combustion bottle.
Further, the first exhaust pipe and the second exhaust pipe are both arranged on the sealing plug.
Further, the sample fixing part is a hook, the hook end of the hook is used for fixing a sample to be detected, and the other end of the hook is fixed on the sealing plug; furthermore, the hook is made of quartz.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model discloses an online digestion device of solid organic sample based on vapour takes place-atomic fluorescence spectrum appearance is based on off-line oxygen bottle combustion technology, and the sample directly gets into the vapour after the reaction and takes place-atomic fluorescence spectrum appearance and detect, reduce the intermediate process by a wide margin, uncovered volatilizing, transfer loss risk and the human operation error that exist in the current sample processing have effectively been avoidd, the analysis accuracy, the analysis repeatability, analysis flux and the analytical sensitivity of vapour emergence-atomic fluorescence spectrum appearance have been promoted by a wide margin, make it more have industrial value.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the embodiments are briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an online digestion device for solid organic samples based on a vapor generation-atomic fluorescence spectrometer according to the present invention;
FIG. 2 is a schematic structural diagram of a reaction vessel of the solid organic sample online digestion device based on the vapor generation-atomic fluorescence spectrometer of the present invention;
in the figure, 1, an argon storage tank, 2, an oxygen storage tank, 3, an absorption liquid storage tank, 4, a reaction container, 4-1, a first conveying pipe, 4-2, a first exhaust pipe, 4-3, a second exhaust pipe, 4-4, a sealing plug, 4-5, a sample fixing part, 5, a reducing agent storage tank, 6, a waste liquid storage tank, 7 and a vapor generation-atomic fluorescence spectrometer are adopted.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below in conjunction with the detailed description, but it is to be understood that the descriptions are intended to further illustrate the features and advantages of the invention, rather than to limit the invention.
The utility model discloses a solid organic sample online digestion device based on vapour takes place-atomic fluorescence spectrometer, including argon gas holding vessel 1, oxygen holding vessel 2, absorption liquid holding vessel 3, reaction vessel 4, reductant holding vessel 5 and waste liquid collection tank 6.
Wherein the reaction vessel 4 is a vessel with an open top end, such as a combustion bottle, and the open top end is sealed by a sealing plug 4-4. The side wall of the reaction vessel 4 is provided with a first conveying pipe 4-1, and the first conveying pipe 4-1 penetrates through the wall of the reaction vessel 4, namely one end is positioned in the reaction vessel 4, and the other end is positioned outside the reaction vessel 4. The top of the reaction vessel 4 is provided with a first exhaust pipe 4-2 and a second exhaust pipe 4-3, the first exhaust pipe 4-2 is communicated with the inner cavity of the reaction vessel 4 and the atmosphere, the first exhaust pipe 4-2 is provided with a first exhaust valve, and the first exhaust pipe 4-2 is used for exhausting oxygen in the reaction vessel 4 to the atmosphere; the second exhaust pipe 4-3 is communicated with the inner cavity of the reaction container 4 and the steam generation-atomic fluorescence spectrometer, a second exhaust valve is arranged on the second exhaust pipe 4-3, and the gas to be detected in the reaction container 4 is transmitted to the steam generation-atomic fluorescence spectrometer for analysis. Preferably, the first exhaust pipe 4-2 and the second exhaust pipe are provided on the sealing plug 4-4. A sample fixing piece 4-5 is arranged in the reaction container 4, and the sample fixing piece 4-5 is used for fixing a sample; preferably, the sample fixing part 4-5 is a hook, one end of the hook is used for fixing a sample, and the other end of the hook is fixed on the sealing plug 4-4; the material of the hook is preferably quartz.
The argon storage tank 1 is communicated with the first conveying pipe 4-1 through a second conveying pipe, and a first control valve is arranged on the second conveying pipe. Argon gas holding vessel 1 is used for storing argon gas, and the argon gas that stores in the argon gas holding vessel 1 gets into reaction vessel 4 through second conveyer pipe and first conveyer pipe 4-1 in, and the flow and the pressure of argon gas are controlled to first control valve.
The oxygen storage tank 2 is communicated with the first delivery pipe 4-1 through a third delivery pipe, and a second control valve is arranged on the second delivery pipe. The oxygen storage tank 2 is used for storing oxygen, the oxygen stored in the oxygen storage tank 2 enters the reaction vessel 4 through the third delivery pipe and the first delivery pipe 4-1, and the second control valve controls the flow and pressure of the oxygen.
The absorption liquid storage tank 3 is communicated with the first conveying pipe 4-1 through a fourth conveying pipe, and a first peristaltic pump is arranged on the fourth conveying pipe. The absorption liquid storage tank 3 is used for storing absorption liquid, the absorption liquid stored in the absorption liquid storage tank 3 enters the reaction container 4 through the fourth conveying pipe and the first conveying pipe 4-1, and the first peristaltic pump accurately meters the volume of the absorption liquid input into the reaction container 4.
The reducing agent storage tank 5 is communicated with the reaction vessel 4 through a fifth delivery pipe, and a second peristaltic pump is arranged on the fifth delivery pipe. The reducing agent storage tank 5 is used for storing a reducing agent, the reducing agent stored in the reducing agent storage tank 5 enters the reaction container 4 through a fifth delivery pipe, and the second peristaltic pump accurately meters the volume of the reducing agent input into the reaction container 4.
The waste liquid collecting tank 6 is communicated with the bottom of the reaction container 4 through a sixth conveying pipe, and a third peristaltic pump is arranged on the sixth conveying pipe; the waste liquid in the reaction vessel 4 enters a waste liquid collecting tank 6 through a sixth conveying pipe. The third peristaltic pump accurately meters the volume of waste liquid flowing into the waste liquid collection tank 6.
The utility model discloses a solid organic sample online digestion device's application method based on vapour takes place-atomic fluorescence spectrometer: opening a second control valve and a first exhaust valve, closing the first control valve and the second exhaust valve, operating a first peristaltic pump, introducing absorption liquid in an absorption liquid storage tank 3 into a reaction container 4, meanwhile, weighing a sample to be detected, placing the sample to be detected on a combustion carrier, tightly wrapping and coating a igniting agent, fixing the sample to be detected on a hook, igniting the sample to be detected, quickly screwing a sealing plug 4-4, closing the second control valve after the sample to be detected is completely combusted, opening the first control valve, discharging residual oxygen in the reaction container, closing the first exhaust valve after the oxygen is completely discharged, opening the second exhaust valve, operating a second peristaltic pump simultaneously, introducing a reducing agent in a reducing agent storage tank 5 into the reaction container 4, introducing steam generated by reaction into a steam generation-atomic fluorescence spectrometer 7 for analysis, and operating a third peristaltic pump after the analysis is completed, and discharging waste liquid.
Wherein, the burning carrier and the burning agent are not necessary to be the components of the solid organic sample on-line digestion device based on the steam generation-atomic fluorescence spectrometer, and can be directly obtained when in use. The combustion carrier is a combustible and porous material and is used for wrapping a sample to be tested, and quartz cloth is preferred. The ignition agent is coated on the combustion carrier to promote the combustion of the sample to be tested, and the ignition agent is preferably glycerin with analytical purity.
The present invention is further illustrated by the following examples.
Example 1
Adopt the utility model discloses a solid organic sample on-line digestion device analysis based on vapour takes place-atomic fluorescence spectrometer. The analysis method comprises the steps of opening a second control valve (oxygen flow pressure is 0.1MPa) and a first exhaust valve, closing the first control valve and the second exhaust valve, operating a first peristaltic pump (30s), introducing absorption liquid (20 mL10 wt% HCl) into a reaction vessel 4(400mL combustion bottle), meanwhile, weighing 0.2g of solid organic sample to be detected, placing the solid organic sample on quartz cloth, tightly wrapping the solid organic sample, coating glycerin (analytically pure) on the outer side of the quartz cloth, fixing the solid organic sample on a hook 4 (30s), igniting the solid organic sample to be detected, rapidly screwing a sealing plug 4-4, closing the second control valve after the solid organic sample to be detected is completely combusted (45-60s), opening the first control valve (air flow argon pressure is 0.05MPa), discharging residual oxygen in the reaction vessel, closing the first exhaust valve after the oxygen is discharged, opening the second exhaust valve, operating the second peristaltic pump to introduce a reducing agent into the reaction vessel 4, reducing agent NaBH4(2 wt%) into a combustion bottle to start steam generation reaction to generate SeH4And (4) entering an atomic fluorescence spectrometer atomizer 7 for detection (reading time is 20s), completing the detection (38s), operating a third peristaltic pump, and discharging waste liquid. The test samples, test amounts and test results are shown in tables 1 and 2.
TABLE 1 detection amount and detection result of two national standard substances with different selenium contents
TABLE 2 examination of the actual samples and the examination results
In Table 2, the aSe standard values were obtained from wet digestion (hydride atomic fluorescence spectrometry for selenium in rice, Guangzhou chemical, 2016 (02)) and off-line oxygen-bottle combustion (Fast and clean determination of total selenium in biological materials by an improved oxygen lance combustion method with hydrogen generation technology, Microchemical Journal, 2019) experiments. (n ═ 6, mean ± 3 SD). As can be seen from tables 1 and 2, the utility model discloses a solid organic sample on-line digestion device based on vapor generation-atomic fluorescence spectrometer analysis precision is high, and stability is good.
It should be understood that the foregoing detailed description is by way of example only, and not intended to limit the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious changes and modifications can be made without departing from the scope of the invention.
Claims (5)
1. The on-line digestion device for the solid organic sample based on the vapor generation-atomic fluorescence spectrometer is characterized by comprising an argon storage tank (1), an oxygen storage tank (2), an absorption liquid storage tank (3), a reaction container (4), a reducing agent storage tank (5) and a waste liquid collecting tank (6);
the reaction container (4) is a container with an opening at the top end, and the opening at the top end is sealed by a sealing plug (4-4); a first conveying pipe (4-1) penetrating through the wall of the reaction vessel (4) is arranged on the side wall of the reaction vessel (4); a first exhaust pipe (4-2) and a second exhaust pipe (4-3) are arranged at the top of the reaction container (4), the first exhaust pipe (4-2) is communicated with the inner cavity of the reaction container (4) and the atmosphere, and a first exhaust valve is arranged on the first exhaust pipe (4-2); the second exhaust pipe (4-3) is communicated with the inner cavity of the reaction container (4) and the steam generation-atomic fluorescence spectrometer, and a second exhaust valve is arranged on the second exhaust pipe (4-3); a sample fixing piece (4-5) is arranged in the reaction container (4), and the sample fixing piece (4-5) is used for fixing a sample to be detected;
the argon storage tank (1) is communicated with the first conveying pipe (4-1) through a second conveying pipe, and a first control valve is arranged on the second conveying pipe;
the oxygen storage tank (2) is communicated with the first conveying pipe (4-1) through a third conveying pipe, and a second control valve is arranged on the second conveying pipe;
the absorption liquid storage tank (3) is communicated with the first conveying pipe (4-1) through a fourth conveying pipe, and a first peristaltic pump is arranged on the fourth conveying pipe;
the reducing agent storage tank (5) is communicated with the reaction container (4) through a fifth conveying pipe, and a second peristaltic pump is arranged on the fifth conveying pipe;
the waste liquid collecting tank (6) is communicated with the bottom of the reaction container (4) through a sixth conveying pipe, and a third peristaltic pump is arranged on the sixth conveying pipe.
2. The on-line solid organic sample digestion device based on vapor generation-atomic fluorescence spectrometer of claim 1, characterized in that the reaction vessel (4) is a combustion bottle.
3. The on-line digestion apparatus for solid organic samples based on vapor generation-atomic fluorescence spectrometer of claim 1, characterized in that the first exhaust pipe (4-2) and the second exhaust pipe (4-3) are both disposed on the sealing plug (4-4).
4. The on-line digestion device for the solid organic sample based on the vapor generation-atomic fluorescence spectrometer as claimed in claim 1, wherein the sample fixing member (4-5) is a hook, the hook end of the hook is used for fixing the sample to be measured, and the other end of the hook is fixed on the sealing plug (4-4).
5. The on-line solid organic sample digestion device based on the vapor generation-atomic fluorescence spectrometer of claim 4, wherein the material of the hook is quartz.
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| CN202022761282.0U CN213875430U (en) | 2020-11-25 | 2020-11-25 | Solid organic sample on-line digestion device based on vapor generation-atomic fluorescence spectrometer |
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