阅读说明：本技术 一种基于薄层色谱技术用于元素形态分析的进样装置及方法 (Sample introduction device and method for element morphological analysis based on thin-layer chromatography technology ) 是由 邢志 李铭 黄秀 范博文 于 2019-10-21 设计创作，主要内容包括：本发明公开了一种基于薄层色谱技术用于元素形态分析的进样装置及方法。本发明的进样装置,它包括可密闭的样品室和移动加热装置；样品室相对两个壁上分设有一个进气口和一个出气口；移动加热装置设置于样品室的腔体内,所述移动加热装置可沿所述进气口至所述出气口的方向移动。本发明的进样方法,包括如下步骤：样品中元素的各形态经薄层色谱分离,薄层色谱板上得到层析斑点；然后加热将层析斑点中的元素形态解吸出,将元素形态引入分析仪器中,实现元素形态分析进样。本发明能加热解吸层析斑点中的物质以进样检测,加热更集中高效,能够快速高效地解吸出；装置结构简单,操作简便,成本低。(The invention discloses a sample introduction device and a sample introduction method for element morphology analysis based on a thin-layer chromatography technology. The sample introduction device 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 sample injection method comprises the following steps: separating each form of elements in the sample by thin-layer chromatography to obtain chromatography spots on a 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 element form analysis sample injection. The invention can heat and desorb the substances in the chromatography spots for sample injection detection, the heating is more concentrated and efficient, and the substances can be quickly and efficiently desorbed; the device has simple structure, simple and convenient operation and low cost.)

1. A sample introduction device for element morphology analysis based on thin layer chromatography technology 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 any one of claims 1-3, wherein: the heating mode of the heating head is resistance heating or thermal radiation heating;

one end of the heating head, which is used for heating the thin-layer chromatography plate, is round;

the diameter of the heating head is larger than that of the chromatographic spot heated in use.

5. The apparatus of any one of claims 1-4, wherein: the electric rotating platform moves in a one-dimensional movement mode, a two-dimensional movement mode or a three-dimensional movement mode.

6. A sample injection method for element morphological analysis based on thin layer chromatography technology comprises the following steps: 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.

7. The method of claim 6, wherein: heating to the temperature of 20-300 ℃;

the heating mode is electric heating or thermal radiation heating.

8. The method according to claim 6 or 7, characterized in that: the elemental form is introduced into the analytical instrument by the action of a carrier gas.

9. The method of claim 8, wherein: 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.

10. The method according to any one of claims 6-9, wherein: the sample injection method is carried out by adopting the sample injection device for element morphology analysis based on the thin layer chromatography technology, which is disclosed by any one of claims 1 to 4, and 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.

Technical Field

The invention relates to a sample introduction device and a sample introduction method for element morphology analysis based on a thin-layer chromatography technology, and belongs to the technical field of analytical chemistry.

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.

Disclosure of Invention

The invention aims to provide a sample injection device and a method for element morphology analysis based on thin-layer chromatography technology, which can heat and desorb substances in chromatography spots for sample injection detection, are heated more intensively and efficiently, and can be quickly and efficiently desorbed; the device has simple structure, simple and convenient operation and low cost.

The invention aims to provide 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 is suitable for heating and analyzing thin-layer chromatographic plates with different stationary phases, different thicknesses and different sizes after 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 infrared thermal radiation heating;

one end of the heating head, which is used for heating the thin-layer chromatography plate, is round;

the diameter of the heating head is larger than that of the chromatographic spot heated in use, so that the heating is more 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 is used, the air 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.

The invention also aims to provide a sample injection method for element morphological analysis based on thin-layer chromatography technology, which comprises the following steps: 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.

In the invention, the analytical instruments which can be used for the method comprise 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.

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 invention has the following advantages:

the invention provides a sample injection method and a sample injection device for element morphology analysis based on thin-layer chromatography technology. The diameter of the heating head adopted by the invention is slightly larger than that of the chromatographic spot, the design can enable the heating to be more concentrated and efficient, and the element form in the chromatographic spot can be rapidly and efficiently desorbed. In addition, the device has the advantages of simple structure, higher use safety, simple and convenient operation and low cost.

Drawings

Fig. 1 is a schematic structural diagram of a sample injection 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 experimental procedures used in the following examples are all conventional procedures unless otherwise specified.

Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.

The present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.