CN211235697U - Sample introduction device for element morphological analysis based on thin-layer chromatography technology - Google Patents
Sample introduction device for element morphological analysis based on thin-layer chromatography technology Download PDFInfo
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- CN211235697U CN211235697U CN201921764280.8U CN201921764280U CN211235697U CN 211235697 U CN211235697 U CN 211235697U CN 201921764280 U CN201921764280 U CN 201921764280U CN 211235697 U CN211235697 U CN 211235697U
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Abstract
The utility model discloses a sampling device for element morphological analysis based on thin-layer chromatography technique. The sample introduction device of the utility model comprises a sample chamber which can be sealed and a movable heating device; the two opposite walls of the sample chamber are respectively provided with an air inlet and an air outlet; the movable heating device is arranged in a cavity of the sample chamber and can move along the direction from the air inlet to the air outlet. The utility model can heat and desorb the material in the chromatography spot for sample injection detection, the heating is more concentrated and efficient, and the suction can be quickly and efficiently desorbed; the device has simple structure, simple and convenient operation and low cost.
Description
Technical Field
The utility model relates to a sampling device for element morphological analysis based on thin-layer chromatography technique.
Background
The environmental effects of inorganic elements, in particular trace heavy metals (such as arsenic, mercury, cadmium, chromium, lead, etc.) and the biological activity of trace elements are not only related to their total amount, but are to a greater extent determined by their morphology, which differs in its environmental effects or availability. The element morphology analysis has important significance for environmental hazard assessment, disease research, food safety, standard preparation and the like. The separation of different forms of elements by chromatographic techniques (such as gas chromatography, liquid chromatography, thin-layer chromatography, etc.), capillary electrophoresis, solid-phase extraction, etc. is an indispensable step in the analysis of element forms. Compared with other separation technologies, thin-layer chromatography has the advantages of simplicity, convenience, rapidness, economy and practicability, and is widely applied to separation of inorganic and organic compounds. The form separation of Cr, As and Hg elements is successfully realized by silica gel plate thin-layer chromatography, and the quantitative analysis of element forms can be realized by introducing the forms of the Cr, As and Hg elements on the thin-layer chromatography plate into an analytical instrument after desorption. At present, the methods for desorbing the element form on the thin-layer chromatographic plate and introducing the element form into an analytical instrument for detection mainly comprise laser ablation and plasma desorption, but a laser ablation system generally has a complex optical path and high cost; the plasma desorption method needs a high-voltage power supply, and has high safety requirement; and the operation of the two methods is relatively cumbersome. Therefore, it is necessary to establish a method for rapidly, simply and efficiently desorbing the element morphology on the TLC plate.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a sample introduction device for element morphology analysis based on thin-layer chromatography technology, which can heat and desorb the substances in chromatography spots for sample introduction detection, the heating is more concentrated and efficient, and the suction can be quickly and efficiently desorbed; the device has simple structure, simple and convenient operation and low cost.
The utility model aims at providing a sample introduction device for element morphology analysis based on thin-layer chromatography technology, which comprises a sealable sample chamber and a movable heating device;
the two opposite walls of the sample chamber are respectively provided with an air inlet and an air outlet;
the movable heating device is arranged in a cavity of the sample chamber and can move along the direction from the air inlet to the air outlet.
In the above device, the mobile heating device comprises two thin-layer chromatography plate clamps, two thin-layer chromatography plate clamp bases, an electric rotating platform and a heating head;
the positions of the thin-layer chromatography plate clamps are oppositely arranged, and the thin-layer chromatography plate clamps are fixed on one end of the base of the thin-layer chromatography plate clamp and are used for fixing two ends of a thin-layer chromatography plate; the thin-layer chromatography plate clamp base is fixed at the bottom of the cavity of the sample chamber; the electric rotating platform comprises a stepping motor and a moving shaft connected with the stepping motor, and the moving shaft penetrates through the other end of the thin-layer chromatography plate clamp base; one end of the heating head is fixedly arranged on the moving shaft through a heating head base, and the other end of the heating head is used for heating the thin-layer chromatography plate; the thin-layer chromatographic plate, the air inlet and the air outlet are arranged on the same horizontal plane.
The device of the utility model is suitable for the heating analysis of thin-layer chromatographic plates with different stationary phases, different thicknesses and different sizes after the element forms are separated;
the mobile heating device is movable for heating the thin layer chromatography plate.
In the device, the sample chamber is in at least one of a cuboid, a cube, a cylinder and a shuttle shape, and the shape is favorable for gas transmission;
one side or the multiaspect material of sample room is transparent material, specifically can be at least one in quartz glass, silica glass and the organic glass to observe at any time in the experimental process the condition in the sample room cavity.
In the above device, the heating head is heated by resistance heating or thermal radiation heating; the resistance heating can be at least one of resistance wire heating, ceramic heating and resistance coil heating; the thermal radiation heating is specifically infrared thermal radiation heating.
In the above device, one end of the heating head for heating the thin layer chromatography plate is circular.
In the device, the diameter of the heating head is larger than that of the chromatographic spot heated in use, so that the heating is concentrated and efficient, and the element form in the chromatographic spot can be rapidly and efficiently desorbed;
the specific diameter of the diameter of heating head can be 2 ~ 10 mm.
In the above device, the electric rotating platform moves in one-dimensional, two-dimensional or three-dimensional manner to heat different positions on the thin-layer chromatography plate.
When the device of the utility model is used, the gas outlet can be connected with an analysis instrument;
the analytical instruments comprise an atomic fluorescence spectrometer, an atomic absorption spectrometer, an inductively coupled plasma emission spectrometer or an inductively coupled plasma mass spectrometer and other analytical instruments.
When the device is used, computer software can be used for controlling the heating time, the input voltage and the input current of the heating head, so as to control the temperature and the time for heating the chromatographic spot on the thin-layer chromatographic plate; computer software can be used for controlling the one-dimensional, two-dimensional or three-dimensional movement of the electric rotating platform, so as to control the heating of the heating head at different positions of the thin-layer chromatographic plate; the gas outlet can be connected with analytical instruments such as an atomic fluorescence spectrometer, an atomic absorption spectrometer, an inductively coupled plasma emission spectrometer or an inductively coupled plasma mass spectrometer through an inert gas conduit to detect the elementary substances.
Adopt the utility model discloses the device carries out and is used for elementary morphology analysis's sampling method based on thin-layer chromatography technique, including following step: separating each form of elements in the sample by thin-layer chromatography to obtain chromatography spots on the thin-layer chromatography plate; then heating to desorb the element form in the chromatography spot, introducing the element form into an analytical instrument, and realizing the element form analysis sample injection.
The present invention relates to an analytical instrument, and more particularly to an analytical instrument for use in an atomic fluorescence spectrometer, an atomic absorption spectrometer, an inductively coupled plasma emission spectrometer, or an inductively coupled plasma mass spectrometer.
In the method, the heating is carried out to a temperature of 20-300 ℃.
In the above method, the heating is electric heating or thermal radiation heating.
In the above method, the elemental form is introduced into the analytical instrument by the action of a carrier gas.
In the above method, the carrier gas is at least one of helium, argon, neon and nitrogen;
the flow rate of the carrier gas is 200-1200 mL/min.
In the method, the sample injection method is performed by adopting the sample injection device for element morphology analysis based on the thin-layer chromatography technology, and specifically comprises the following steps: placing said sample on a thin layer chromatography plate, said thin layer chromatography plate being affixed to said mobile heating means in said sample chamber; separating each form of elements in the sample by thin-layer chromatography to obtain chromatography spots on the thin-layer chromatography plate; then the mobile heating device carries out mobile heating to desorb the element form in the chromatography spot, the carrier gas is introduced through the air inlet to introduce the element form into an analyzer, and the element form analysis sample introduction is realized.
The utility model has the advantages of it is following:
the utility model provides a based on thin-layer chromatography technique is used for elementary morphology analysis's advance kind method and device adopts the heating head to hug closely bottom surface under the thin-layer chromatography board, under the electric rotating platform drives, heats every chromatography spot in proper order, and the material in the desorption chromatography spot is introduced into analytical instrument again and is detected under the effect of carrier gas. The utility model discloses the diameter of the diameter ratio chromatography spot of the heating head that well adopted is slightly bigger, and this kind of design enables the heating and concentrates the high efficiency more, guarantees that the element form in the chromatography spot can fast high-efficiently solve the suction. Furthermore, the device of the utility model has the advantages of simple structure, high safety, simple operation and low cost.
Drawings
Fig. 1 is a schematic structural diagram of a sample introduction device for elemental morphology analysis based on thin-layer chromatography, wherein fig. 1(a) is a schematic structural diagram of the device of the present invention, and fig. 1(b) is a schematic structural diagram of a mobile heating device in a sample chamber in fig. 1 (a).
FIG. 2 is a qualitative analysis chart of the mercury morphology determined in example 2.
The respective labels in FIG. 1 are as follows: 1 sample chamber, 2 air inlets, 3 mobile heating devices, 4 air outlets, 5 thin-layer chromatography plate clamps, 6 thin-layer chromatography plate clamp bases, 7 stepping motors, 8 heating head bases, 9 moving shafts, 10 thin-layer chromatography plates and 11 heating heads.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.
Example 1 sample introduction device for elemental morphology analysis based on thin-layer chromatography
The sample introduction device for element morphology analysis based on thin-layer chromatography technology provided by the embodiment comprises a cuboid sample chamber 1 and a mobile heating device 3; the lower bottom surface of the sample chamber 1 is made of aluminum alloy, and the other five surfaces are made of organic glass, so that the condition in the sample chamber can be observed at any time in the experimental process; the organic glass plates are hermetically matched through chloroform, and the organic glass plates and the aluminum alloy plates are hermetically matched through vacuum silicone grease; the two opposite positions of the side wall of the sample chamber 1 are respectively provided with an air inlet 2 and an air outlet 4, the air inlet 2 is used for inputting carrier gas, and the air outlet 4 can be connected with analytical instruments such as an atomic fluorescence spectrometer, an atomic absorption spectrometer, an inductively coupled plasma emission spectrometer or an inductively coupled plasma mass spectrometer and the like; the centers of the air inlet 2 and the air outlet 4 are opposite to the side surface of the thin-layer chromatographic plate 10; the mobile heating device 3 is fixedly arranged on the lower bottom surface of the sample chamber 1 and comprises two thin-layer chromatography plate clamps 5 which are opposite to each other in position, a one-dimensional electric rotating platform and a heating head 11; the thin-layer chromatography plate clamp 5 is fixedly arranged on the lower bottom surface of the sample chamber 1 through a bridge-shaped thin-layer chromatography plate clamp base 6 and is used for fixing two ends of a thin-layer chromatography plate 10; the one-dimensional electric rotating platform comprises a stepping motor 7 and a moving shaft 9, and the moving shaft 9 penetrates through the bridge holes of the two thin-layer chromatography plate clamp bases 6; the upper end of a heating head 11 is tightly attached to the lower bottom surface of the thin-layer chromatographic plate 10, and the lower end of the heating head is fixedly arranged on a moving shaft 9 through a heating head base 8; the upper end of the heating head 11 is circular, the diameter of the heating head is 5mm, a resistance ring is arranged in the heating head 11, and the heating of different chromatography spots on the thin-layer chromatography plate 10 is realized by the heating head 11 through an electric rotating platform.
The feasibility of the method and the device is verified by the morphological analysis map which is shown in figure 2 and takes Hg as an example. The electric rotating platform can also select a two-dimensional or three-dimensional moving mode.
Example 2 analysis of Mercury morphology
Use the device in embodiment 1 of the utility model and inductively coupled plasma mass spectrometer (ICP-MS) cooperation are analyzed the mercury form, specifically as follows:
fixing two ends of the thin-layer chromatographic plate 10 which finishes Hg morphological chromatographic separation by using thin-layer chromatographic plate clamps 5; after the organic glass plate and the aluminum alloy plate of the sample chamber 1 are in closed fit through vacuum silicone grease, introducing carrier gas argon from the gas inlet 2, and controlling the flow rate of the carrier gas argon to be 600 mL/min; controlling a one-dimensional electric rotating platform by using conventional computer software, and moving a heating head 11 to be right below a chromatography spot on a thin-layer chromatographic plate 10; controlling the temperature of the heating head 11 to be 150 ℃ by using computer software, heating for 10s, and desorbing the Hg form in the chromatographic spot; the desorbed Hg form enters an ICP-MS connected with the device from the gas outlet 4 for analysis under the action of argon introduced from the gas inlet 2; analysis of all chromatographic spots on the TLC plate 10 according to the procedure described above resulted in Hg2+The qualitative analysis spectra of methylmercury (MeHg) and ethylmercury (EtHg) are shown in FIG. 2, from which it can be seen that the device is feasible as an elemental morphology analysis sample injection device based on thin layer chromatography.
In the above embodiment, the ICP-MS test conditions were RF power 1550W, plasma gas flow rate 15L/min, auxiliary gas flow rate 0.9L/min, and quadrupole vacuum 3.30 × 10-4Pa, mass number of Hg for data acquisition mode TRA, 202.
Claims (7)
1. A sample injection device for element morphology analysis based on thin layer chromatography technology is characterized in that: it comprises a sealable sample chamber and a mobile heating device;
the two opposite walls of the sample chamber are respectively provided with an air inlet and an air outlet;
the movable heating device is arranged in a cavity of the sample chamber and can move along the direction from the air inlet to the air outlet.
2. The apparatus of claim 1, wherein: the mobile heating device comprises two thin-layer chromatography plate clamps, two thin-layer chromatography plate clamp bases, an electric rotating platform and a heating head;
the positions of the thin-layer chromatography plate clamps are oppositely arranged, and the thin-layer chromatography plate clamps are fixed on one end of the base of the thin-layer chromatography plate clamp and are used for fixing two ends of a thin-layer chromatography plate; the thin-layer chromatography plate clamp base is fixed at the bottom of the cavity of the sample chamber; the electric rotating platform comprises a stepping motor and a moving shaft connected with the stepping motor, and the moving shaft penetrates through the other end of the thin-layer chromatography plate clamp base; one end of the heating head is fixedly arranged on the moving shaft through a heating head base, and the other end of the heating head is used for heating the thin-layer chromatography plate; the thin-layer chromatographic plate, the air inlet and the air outlet are arranged on the same horizontal plane.
3. The apparatus of claim 1 or 2, wherein: the shape of the sample chamber is at least one of a cuboid, a cube, a cylinder and a shuttle;
one or more surfaces of the sample chamber are made of transparent materials.
4. The apparatus of claim 2, wherein: the heating mode of the heating head is resistance heating or thermal radiation heating.
5. The apparatus of claim 2, wherein: one end of the heating head used for heating the thin-layer chromatography plate is round.
6. The apparatus of claim 5, wherein: the diameter of the heating head is larger than that of the chromatographic spot heated in use.
7. The apparatus of claim 2, wherein: the electric rotating platform moves in a one-dimensional movement mode, a two-dimensional movement mode or a three-dimensional movement mode.
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| CN201921764280.8U CN211235697U (en) | 2019-10-21 | 2019-10-21 | Sample introduction device for element morphological analysis based on thin-layer chromatography technology |
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| CN201921764280.8U CN211235697U (en) | 2019-10-21 | 2019-10-21 | Sample introduction device for element morphological analysis based on thin-layer chromatography technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110632239A (en) * | 2019-10-21 | 2019-12-31 | 清华大学 | Sample introduction device and method for element morphological analysis based on thin-layer chromatography technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110632239A (en) * | 2019-10-21 | 2019-12-31 | 清华大学 | Sample introduction device and method for element morphological analysis based on thin-layer chromatography technology |
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