CN104007224A - Focusing gauge plate - Google Patents
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- CN104007224A CN104007224A CN201410257784.6A CN201410257784A CN104007224A CN 104007224 A CN104007224 A CN 104007224A CN 201410257784 A CN201410257784 A CN 201410257784A CN 104007224 A CN104007224 A CN 104007224A
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 2
- 230000007797 corrosion Effects 0.000 claims 1
- 238000005260 corrosion Methods 0.000 claims 1
- 238000005070 sampling Methods 0.000 abstract description 27
- 230000005526 G1 to G0 transition Effects 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004587 chromatography analysis Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 12
- 239000012488 sample solution Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000001292 planar chromatography Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000520 microinjection Methods 0.000 description 1
- 238000004816 paper chromatography Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
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Abstract
本发明为调焦规板,适用于平面色谱分析领域。是新型平面色谱点样仪的一个部件。是用于调整和规范微量喷嘴与点样平面及点样针针尖与点样平面之间距离的固定尺寸模板。新型平面色谱点样仪点样时,喷嘴与点样平面之间的距离、点样针针尖与点样平面之间的距离是影响点样效果的重要因素。本发明通过对位于点样针尖部位的液滴在环绕的喷射气流作用下、脱离点样针到达点样平面的过程进行了分析,设计制作了调焦规板。当点样仪使用不同厚度的固定相时,利用调焦规板可以很方便地调整和规范微量喷嘴与点样平面之间的距离及点样针尖与点样平面之间的距离。调焦规板结构简洁明了,简化了仪器的设计和使用,使新型点样仪可适用于各种厚度固定相的点样。
The invention is a focusing gauge plate, which is suitable for the field of plane chromatography analysis. It is a part of the new flat chromatographic pointing instrument. It is a fixed-size template used to adjust and standardize the distance between the micro nozzle and the pointing plane and the distance between the tip of the sampling needle and the pointing plane. The distance between the nozzle and the sample pointing plane, the distance between the tip of the sample needle and the sample pointing plane are the important factors affecting the sample pointing effect when the new planar chromatographic pointing instrument is pointing samples. The present invention designs and manufactures the focusing gauge plate by analyzing the process that the liquid drop located at the point of the pointing needle leaves the pointing needle and reaches the pointing plane under the action of the surrounding jet airflow. When the spotting instrument uses stationary phases of different thicknesses, the distance between the micro nozzle and the spotting plane and the distance between the point of the spotting needle and the spotting plane can be easily adjusted and standardized by using the focusing gauge. The structure of the focusing gauge plate is simple and clear, which simplifies the design and use of the instrument, making the new spotting instrument suitable for spotting samples of various thickness stationary phases.
Description
技术领域technical field
本发明为一种调整和规范微小距离范围的固定尺寸模板,特指一种用于控制平面色谱点样仪的微量喷嘴与点样平面的距离以及点样针针尖与点样平面距离的调焦规板。本发明适用于平面色谱分析领域。The invention is a fixed-size template for adjusting and standardizing the micro-distance range, in particular to a focus adjustment for controlling the distance between the micro-nozzle of a planar chromatographic spotting instrument and the spotting plane, and the distance between the tip of the spotting needle and the spotting plane regulation board. The invention is applicable to the field of plane chromatography analysis.
背景技术Background technique
分析化学中的平面色谱技术主要包括薄层色谱(固定相可采用硅胶、聚酰胺、氧化铝等)和纸色谱,试验过程中点样方法对分离效果的影响很大。目前常用的点样方法主要有点状点样和条带点样两种,近年来的研究表明条带状点样可显著提高平面色谱的分离容量和样品中各组分的分离度。然而手工点样很难获得样品均匀的条带,采用点样仪器可实现均匀的条带状点样。使用仪器点样时常采用非接触喷雾点样,此时所获得的样品条带的效果与多种因素有关,其中保证条带点样重复性最重要的因素为喷嘴至点样平面的距离和点样针尖至点样平面的距离。由于层析用薄层板或纸的厚度不完全一致,可能造成点样重复性不好,会使条带点样的重复性变差。Plane chromatography techniques in analytical chemistry mainly include thin layer chromatography (stationary phase can be silica gel, polyamide, alumina, etc.) and paper chromatography. During the test, the sampling method has a great influence on the separation effect. At present, the commonly used spotting methods are mainly spot spotting and strip spotting. Recent studies have shown that strip spotting can significantly improve the separation capacity of planar chromatography and the resolution of each component in the sample. However, it is difficult to obtain a uniform strip of the sample by manual spotting, and uniform strip-like spotting can be achieved by using a spotting instrument. Non-contact spraying is often used for sample spotting with instruments, and the effect of the sample band obtained at this time is related to many factors, among which the most important factor to ensure the repeatability of strip spotting is the distance and point from the nozzle to the spotting plane. The distance from the tip of the sample needle to the spotting plane. Because the thickness of the thin-layer plate or paper used for chromatography is not completely consistent, it may cause poor spotting repeatability, which will deteriorate the repeatability of strip spotting.
本发明在微量喷嘴喷射微量溶液原理的基础上,为了能够准确控制点样针针尖与点样平面的距离,通过大量实验数据的整理、分析、总结,设计了一种用于调整和规范微小距离范围的固定尺寸模板,其结构简单明了,便于使用,同时简化了仪器的构造,使新型平面色谱点样仪可适用于各种厚度的薄层板和纸的点样。The present invention is based on the principle of spraying a small amount of solution by a micro nozzle, in order to accurately control the distance between the tip of the sampling needle and the sampling plane, and through arranging, analyzing and summarizing a large number of experimental data, a device for adjusting and standardizing the micro distance is designed. The range of fixed-size templates is simple and clear in structure, easy to use, and at the same time simplifies the construction of the instrument, making the new planar chromatographic spotting instrument suitable for spotting of thin-layer boards and papers of various thicknesses.
发明内容Contents of the invention
在使用新型平面色谱点样仪进行点样时多为非接触条带状点样,用微量喷嘴和微量进样针配合完成(见附图1)。由附图1可以看出,当点样仪运行时,气流包围在点样针管周围,把样品溶液喷射到点样平面(薄层板或纸)上,此时气流从平头针尖到点样平面之间的空间形状,可近似看作一个被气流围成的倒置圆锥台,其下端某一高度的横截面为一个圆形,设该圆形横截面的直径为d。若该横截面与点样平面重合时,当点样针垂直于点样平面并沿着平行于点样平面的方向做匀速直线运动,由点样针匀速推出的溶液即可点成为一个直线型条带,它的宽度即为d。When using a new type of flat chromatographic spotting instrument for spotting, it is mostly non-contact strip spotting, which is completed with the cooperation of a micro nozzle and a micro injection needle (see accompanying drawing 1). As can be seen from Figure 1, when the spotting instrument is running, the airflow surrounds the spotting needle tube, and the sample solution is sprayed onto the spotting plane (thin-layer board or paper), and the airflow is from the flat needle tip to the spotting plane. The shape of the space between them can be approximated as an inverted truncated cone surrounded by airflow, the cross-section at a certain height at the lower end is a circle, and the diameter of the circular cross-section is d. If the cross-section coincides with the spotting plane, when the spotting needle is perpendicular to the spotting plane and moves in a straight line at a uniform speed along the direction parallel to the spotting plane, the solution pushed out by the spotting needle at a uniform speed can be spotted into a straight line. A strip whose width is d.
然而由附图1可见,圆形横截面的直径d的大小取决于点样针尖到点样平面的高度M。当M过大时,即M>h+Δh,倒置锥形圆台在点样平面上的圆形横截面的面积变小,即吸收样品溶液的固定相面积变小,但由于从喷嘴里喷出的气流量和吹带下来的样品溶液量不变,而固定相吸收溶液的速率是恒定的,因此过量的样品溶液被气流吹走,样品液滴被吹走时落下来的痕迹就导致在点样平面上形成发散现象。However, it can be seen from accompanying drawing 1 that the size of the diameter d of the circular cross section depends on the height M from the spotting needle tip to the spotting plane. When M is too large, that is, M>h+Δh, the area of the circular cross-section of the inverted conical truncated cone on the sampling plane becomes smaller, that is, the area of the stationary phase that absorbs the sample solution becomes smaller, but due to the The air flow rate and the amount of sample solution blown down are constant, while the rate of the stationary phase absorbing solution is constant, so the excess sample solution is blown away by the airflow, and the traces that fall when the sample droplets are blown away lead to Divergence is formed on the plane.
当M过小,即M<h(见附图1),即倒置锥形圆台在点样平面上的圆形横截面的面积变大,吸收样品溶液的固定相面积变大,由于从喷嘴里喷出的气流量、由气流吹带下来的样品溶液量和固定相吸收溶液的速率仍然保持一定,固定相在很短的时间(t)里迅速地吸收同样体积的样品溶液。由于溶液不是连续从点样针针尖到达固定相平面的,在前一滴溶液到达固定相平面后,后一滴溶液可能还挂在点样针针尖上,这时产生了一个间隙时间(Δt),而连续的气流在这个间隙时间(Δt)里吹到固定相平面上,形成漫反射,在点样针的平头针尖与固定相之间形成不可控制的气流,把点样针针尖上刚刚形成的溶液液滴向任意方向吹走,也会造成点样条带发散现象。When M is too small, that is, M<h (see Figure 1), that is, the area of the circular cross-section of the inverted conical truncated cone on the sampling plane becomes larger, and the area of the stationary phase that absorbs the sample solution becomes larger. The ejected air flow, the amount of sample solution blown down by the air flow and the rate at which the stationary phase absorbs the solution remain constant, and the stationary phase quickly absorbs the same volume of sample solution in a very short time (t). Since the solution does not continuously reach the stationary phase plane from the tip of the sampling needle, after the previous drop of solution reaches the stationary phase plane, the next drop of solution may still hang on the tip of the sampling needle, at this time a gap time (Δt) is generated, and The continuous airflow is blown onto the stationary phase plane during this gap time (Δt), forming diffuse reflection, and an uncontrollable airflow is formed between the blunt tip of the sampling needle and the stationary phase, and the newly formed solution on the sampling needle tip Droplets are blown away in any direction, which will also cause the spotting band to diverge.
因此,只有当微量点样针垂直于点样平面且点样针针尖与点样平面之间的距离处于某一范围内时,气流吹带下来的样品溶液的量,与固定相吸收的速度相配合,在点样平面上部又正好能够阻挡部分漫反射气流向倒置圆锥台内部吹去,该条件下点样仪可点出边界清晰的样品条带。这一调整高度M大小的方式类似相机调焦的过程,本发明借鉴相机调焦这一名称,将这一个过程也称为调焦,其物理现象解释如上所述。Therefore, only when the micro-sampling needle is perpendicular to the sampling plane and the distance between the tip of the sampling needle and the sampling plane is within a certain range, the amount of the sample solution blown down by the airflow is proportional to the absorption speed of the stationary phase. In combination, the upper part of the spotting plane can just block part of the diffuse reflection airflow from blowing to the inside of the inverted conical truncated cone. Under this condition, the spotting instrument can point out sample strips with clear boundaries. This method of adjusting the height M is similar to the process of camera focusing. The present invention refers to the name of camera focusing, and this process is also called focusing. The physical phenomenon is explained as above.
通过改变M的大小进行点样试验,比较M不同时的点样效果,并对大量的实验数据进行整理和总结,获得了样品条带效果最好时微量点样针针尖与点样平面之间的最小距离h及最大距离h+Δh,据此设计了一种固定尺寸模板,如附图2所示。使用时将模板置于点样针针尖与点样平面之间,点样针针尖应高于h,针尖在h高度平面上方运动不受阻碍;微量点样针针尖必须低于h+Δh的高度,移动模板时,针尖超越不了h+Δh高度的平面,即针尖与点样平面之间的距离符合h<M<h+Δh的要求。只要保证针尖与点样平面之间的高度M位于h~h+Δh的范围之内,点样仪点出的条带宽度一致,边缘清晰。因该模板用于调整和规范高度或高度范围,故本发明命名为调焦规板。调焦规板与微量点样针针尖配合使用图如附图3所示。所设计的调焦规板最高高度H还可用于调整微量喷嘴与点样平面之间的距离。By changing the size of M to carry out the spotting test, comparing the spotting effects of different M, and sorting out and summarizing a large number of experimental data, the distance between the tip of the micro-sampling needle and the spotting plane is obtained when the effect of the sample band is the best. The minimum distance h and the maximum distance h+Δh, based on which a fixed-size template is designed, as shown in Figure 2. When using, place the template between the tip of the sampling needle and the sampling plane. The tip of the sampling needle should be higher than h, and the movement of the needle tip above the h-height plane should not be hindered; the tip of the micro-volume sampling needle must be lower than the height of h+Δh , when the template is moved, the needle tip cannot go beyond the plane at the height of h+Δh, that is, the distance between the needle tip and the spotting plane meets the requirement of h<M<h+Δh. As long as the height M between the needle tip and the spotting plane is within the range of h~h+Δh, the strips spotted by the spotting instrument have the same width and clear edges. Because the template is used to adjust and standardize the height or height range, so the present invention is named focusing gauge plate. The diagram of using the focusing gauge plate in conjunction with the tip of the micro-dispensing needle is shown in Figure 3 of the accompanying drawing. The designed maximum height H of the focusing gauge can also be used to adjust the distance between the micro nozzle and the spotting plane.
由于平面色谱中使用的固定相厚度不同,例如最薄的如色谱用纸,厚的如制备用硅胶薄层板,其厚度可从0.1mm到3mm左右。将调焦规板与新型平面色谱点样仪配合使用,即可实现在不同厚度的固定相上重复点样的目的。使用时只要将调焦规板放在微量喷嘴与固定相点样平面之间,将微量喷嘴与调焦规板的最高平面接触,然后固定住微量喷嘴,微量喷嘴与点样平面之间的距离就调整好了。再插入点样针,移动规板的位置,即可检测点样针针尖与固定相点样平面的的高度是否符合要求,与新型平面色谱点样仪配合使用,此时即可在点样平面上点出符合要求的样品条带。Due to the different thicknesses of the stationary phases used in planar chromatography, for example, the thinnest such as chromatographic paper and the thickest such as preparative silica gel thin-layer plates, the thickness can range from 0.1 mm to about 3 mm. Using the focusing gauge plate together with the new planar chromatographic spotting instrument can achieve the purpose of repeated spotting on stationary phases of different thicknesses. When using, just place the focusing gauge between the micro nozzle and the imprinting plane of the stationary phase, contact the micro nozzle with the highest plane of the focusing gauge, and then fix the micro nozzle, the distance between the micro nozzle and the imprinting plane Just adjusted. Then insert the pointing needle and move the position of the gauge plate to check whether the height between the point of the pointing needle and the pointing plane of the stationary phase meets the requirements. It is used in conjunction with the new type of flat chromatographic pointing instrument, and at this time it can be placed on the pointing plane. Point out the sample bands that meet the requirements.
此外,当新型平面色谱点样仪用于纸色谱点样时,由于色谱用纸可能不够平整而改变M的大小,也有可能被气流吹得抖动,影响点样效果。此时可以利用调焦规板的自重,用作镇纸,可以保持点样时纸面的平整、不抖动,有利于点样。为了防止吹出来的气流被调焦规板的侧面挡回去,将90度的侧立面改为有一定角度的斜面。调焦规板上部立柱的设计是为了可以方便拿取与移动调焦规板,并对调焦规板进行配重。In addition, when the new flat chromatographic spotting instrument is used for paper chromatographic spotting, the size of M may be changed because the chromatographic paper may not be flat enough, and it may also be shaken by the airflow, which will affect the spotting effect. At this time, the self-weight of the focusing gauge can be used as a paperweight, which can keep the paper surface flat and not shaken during sample printing, which is beneficial to sample printing. In order to prevent the blown airflow from being blocked by the side of the focusing gauge plate, the 90-degree side elevation is changed to a slope with a certain angle. The column on the top of the focusing gauge is designed to facilitate the taking and moving of the focusing gauge and to counterweight the focusing gauge.
附图说明Description of drawings
附图1平面色谱点样仪微量喷嘴出口处气流与微量点样针针尖的相对位置关系及点样示意图。图中:1为微量喷嘴,2为点样针针管,3为点样平面,4为气流方向。h为点样针针尖到点样平面的最小距离,h+Δh为点样针针尖到点样平面的最大距离,M为点样针针尖到点样平面的距离。Accompanying drawing 1 is the relative positional relationship between the airflow at the outlet of the micro-volume nozzle of the planar chromatographic spotting instrument and the tip of the micro-volume spotting needle and the schematic diagram of spotting. In the figure: 1 is the micro nozzle, 2 is the needle tube of the sampling needle, 3 is the sampling plane, and 4 is the airflow direction. h is the minimum distance from the tip of the spotting needle to the spotting plane, h+Δh is the maximum distance from the tip of the spotting needle to the spotting plane, and M is the distance from the tip of the spotting needle to the spotting plane.
附图2调焦规板设计原理示意图。图中:1为微量喷嘴,2为点样针针管,3为点样平面,4为气流方向,5为调焦规板。h为点样针针尖到点样平面的最小距离,h+Δh为点样针针尖到点样平面的最大距离,M为点样针针尖到点样平面的距离。Figure 2 is a schematic diagram of the design principle of the focusing gauge. In the figure: 1 is the micro nozzle, 2 is the needle tube of the sampling needle, 3 is the sampling plane, 4 is the air flow direction, and 5 is the focusing gauge plate. h is the minimum distance from the tip of the spotting needle to the spotting plane, h+Δh is the maximum distance from the tip of the spotting needle to the spotting plane, and M is the distance from the tip of the spotting needle to the spotting plane.
附图3调焦规板在微量喷嘴、点样针针尖与固定相点样平面之间配合使用示意图。1为微量喷嘴,2为点样针针管,3为点样平面,4为调焦规板。h为点样针针尖到点样平面的最小距离,h+Δh为点样针针尖到点样平面的最大距离,H为喷嘴到点样平面的距离。Accompanying drawing 3 is a schematic diagram of the cooperating use of the focusing gauge plate between the micro nozzle, the tip of the sampling needle and the sampling plane of the stationary phase. 1 is a micro-volume nozzle, 2 is a sampling needle tube, 3 is a sampling plane, and 4 is a focusing gauge. h is the minimum distance from the spotting needle tip to the spotting plane, h+Δh is the maximum distance from the spotting needle tip to the spotting plane, and H is the distance from the nozzle to the spotting plane.
附图4直线型调焦规板Accompanying drawing 4 Linear focusing gauge plate
具体实施方式Detailed ways
具体实施例1.直线型调焦规板Specific embodiment 1. straight-line focusing regulation plate
为配合使用新型平面色谱点样仪,在固定微量喷嘴与点样平面之间的高度为2.8mm的基础上,经大量试验并对数据进行整理总结,获得一系列微量点样针针尖与点样平面的最佳距离M值的范围,本实施例取M值的范围为1.5-1.9mm(即h=1.5mm,Δh为0.4mm),当点样针针尖与点样平面之间的高度M在此范围内时,均可获得理想的样品条带。用不锈钢材料制作了如附图4所示的直线型调焦规板。In order to cooperate with the new planar chromatographic spotting instrument, on the basis of fixing the height between the micro-volume nozzle and the spotting plane at 2.8mm, after a large number of tests and sorting and summarizing the data, a series of micro-volume spotting needle tips and pointing samples were obtained. The range of the optimum distance M value of the plane, the scope of the M value taken in the present embodiment is 1.5-1.9mm (i.e. h=1.5mm, Δh is 0.4mm), when the height M between the spotting needle tip and the spotting plane Within this range, ideal sample bands can be obtained. The linear focusing gauge plate shown in Figure 4 was made of stainless steel.
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CN104965047A (en) * | 2014-10-13 | 2015-10-07 | 中国药科大学 | Novel planar chromatography sample application instrument and step repeated sample application method |
CN105334707A (en) * | 2015-12-15 | 2016-02-17 | 天津津芯微电子科技有限公司 | Multistage focusing device and method |
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