CN117451918A - Fully automatic and full-process Kjeldahl method measurement system and method - Google Patents
Fully automatic and full-process Kjeldahl method measurement system and method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000007696 Kjeldahl method Methods 0.000 title claims abstract description 21
- 238000005259 measurement Methods 0.000 title claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 108
- 230000029087 digestion Effects 0.000 claims abstract description 96
- 230000007246 mechanism Effects 0.000 claims abstract description 94
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 54
- 238000012546 transfer Methods 0.000 claims abstract description 36
- 230000001079 digestive effect Effects 0.000 claims description 165
- 238000002474 experimental method Methods 0.000 claims description 30
- 238000009434 installation Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims 1
- 210000001035 gastrointestinal tract Anatomy 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 19
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000005070 sampling Methods 0.000 abstract 1
- 238000004821 distillation Methods 0.000 description 20
- 230000008569 process Effects 0.000 description 19
- 239000002253 acid Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000032258 transport Effects 0.000 description 4
- 210000000078 claw Anatomy 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000036544 posture Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
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Abstract
Description
技术领域Technical field
本发明属于凯氏定氮仪技术领域,尤其涉及一种全自动全流程凯氏法测定系统及方法。The invention belongs to the technical field of Kjeldahl nitrogen analyzer, and in particular relates to a fully automatic and full-process Kjeldahl method determination system and method.
背景技术Background technique
凯氏定氮仪是根据蛋白质中氮含量恒定的原理,通过测定样品中氮的含量从而计算蛋白质含量的仪器;因蛋白质含量测量计算的方法叫做凯氏定氮法,故被称为凯氏定氮仪。凯氏定氮实验过程中共有4个过程,分别是消解、蒸馏、吸收和滴定部分。将样品中的有机物消解转化为无机铵盐,然后通过加碱蒸馏方式使氨气逸出,随后被硼酸溶液吸收,再用标准的盐酸或硫酸滴定液滴定硼酸吸收液恢复酸性,通过颜色判定终点。最终通过滴定酸的消耗体积及浓度计算氮含量。The Kjeldahl nitrogen analyzer is an instrument that calculates the protein content by measuring the nitrogen content in the sample based on the principle that the nitrogen content in the protein is constant. Because the method of measuring and calculating the protein content is called the Kjeldahl method, it is called the Kjeldahl nitrogen analyzer. Nitrometer. There are four processes in the Kjeldahl nitrogen determination experiment, namely digestion, distillation, absorption and titration. The organic matter in the sample is digested and converted into inorganic ammonium salts, and then the ammonia gas is released through alkali distillation, and then absorbed by the boric acid solution. The boric acid absorption solution is then titrated with a standard hydrochloric acid or sulfuric acid titrant to restore the acidity, and the end point is determined by the color. . Finally, the nitrogen content is calculated by titrating the consumed volume and concentration of the acid.
发明人发现,采用现有的凯氏定氮仪进行凯氏定氮实验时,其过程为将多个带有样品的消化管在消解仪中进行消解,然后对所有消化管按照一定的顺序逐一的放到定氮仪上进行蒸馏、吸收和滴定等过程,此种方式需要人为取放消化管,整个实验过程效率较低,不适用于多个消化管的批量实验;并且将消化管放置到定氮仪的过程中,每次放置新的消化管时,均需要人为的将蒸馏管进行倾斜后放入消化管,在此过程中,容易造成蒸馏管内残留样品溅到实验人员身上或定氮仪上,造成污染问题;而在智能化发展过程中,为了解决人为逐一取放消化管进行实验存在效率低的问题时,采用机械夹头夹持吸收管的方式,对消解仪中的多个消化管内的样品进行逐一吸收后送到定氮仪中的消化管中,然而此种方式,虽然避免了人为取放消化管,但是,样品的多次输送需要共用一个吸收管,多次输送样品会在吸收管内产生残留,残留样品会对后续实验产生影响,降低了实验精度,并且此种方式也不能代替定氮仪中消化管的取放问题。The inventor found that when using the existing Kjeldahl nitrogen analyzer to perform a Kjeldahl nitrogen determination experiment, the process is to digest multiple digestive tubes with samples in the digestion instrument, and then digest all the digestive tubes one by one in a certain order. Put it on the nitrogen analyzer for distillation, absorption, titration and other processes. This method requires manual handling of the digestive tube. The entire experimental process is inefficient and is not suitable for batch experiments with multiple digestive tubes; and the digestive tubes are placed in During the nitrogen determination process, each time a new digestion tube is placed, the distillation tube needs to be manually tilted and then placed into the digestion tube. During this process, it is easy to cause the residual sample in the distillation tube to splash onto the experimenter or to determine the nitrogen. on the instrument, causing contamination problems; and in the process of intelligent development, in order to solve the problem of low efficiency of manually picking and placing the digestive tubes one by one for experiments, a mechanical chuck is used to clamp the absorption tubes, and multiple tubes in the digestion instrument are The samples in the digestive tube are absorbed one by one and then sent to the digestive tube in the nitrogen analyzer. However, although this method avoids manual picking and placing of the digestive tube, the multiple transportation of the sample requires the sharing of an absorption tube, and the sample must be transported multiple times. Residue will be produced in the absorption tube, and the residual sample will have an impact on subsequent experiments and reduce the accuracy of the experiment. Moreover, this method cannot replace the problem of picking and placing the digestive tube in the nitrogen analyzer.
发明内容Contents of the invention
本发明为了解决上述问题,提出了一种全自动全流程凯氏法测定系统及方法,在消解仪和定氮仪之间设置了进样机,通过转运装置将消解仪中的消化管放置平台送入进样机中,再通过进样机中的取放机构逐一的将消化管送到定氮仪上进行实验,在保证实验精度的基础上,代替了人为取放消化管的试验方式,提高了实验效率。In order to solve the above problems, the present invention proposes a fully automatic and full-process Kjeldahl method measurement system and method. A sample introduction machine is provided between the digestion instrument and the nitrogen determiner, and the digestive tube in the digestion instrument is placed on a platform through a transfer device. into the sample feeder, and then the digestive tubes are sent to the nitrogen analyzer one by one through the pick-and-place mechanism in the sample feeder for experiment. On the basis of ensuring the accuracy of the experiment, it replaces the test method of manually picking and placing the digestive tubes. Improved experimental efficiency.
为了实现上述目的,第一方面,本发明提供了一种全自动全流程凯氏法测定系统,采用如下技术方案:In order to achieve the above objects, in the first aspect, the present invention provides a fully automatic and full-process Kjeldahl method measurement system, which adopts the following technical solutions:
一种全自动全流程凯氏法测定系统,包括用于向消化管进样的前处理机构、消解仪、进样机和定氮仪;A fully automatic and full-process Kjeldahl method determination system, including a pre-treatment mechanism for injecting samples into the digestive tube, a digestion instrument, a sample injector and a nitrogen determiner;
所述消解仪中设置有消化管放置平台,所述消化管放置平台上设置有多个消化管放置位;所述消解仪和所述进样机之间设置转运装置,所述转运装置将所述消化管放置平台转运到所述进样机中;The digestion instrument is provided with a digestive tube placement platform, and the digestive tube placement platform is provided with a plurality of digestive tube placement positions; a transfer device is provided between the digestion instrument and the sample introduction machine, and the transfer device transfers the The digestive tube placement platform is transferred to the sample introduction machine;
所述进样机中设置有取放机构,将所述消化管放置平台上的消化管逐一的运送到所述定氮仪上的消化管安装位置。The sample introduction machine is provided with a pick-and-place mechanism to transport the digestive tubes on the digestive tube placing platform one by one to the digestive tube installation position on the nitrogen determiner.
进一步的,所述进样机上设置有外罩。Further, the sample feeding machine is provided with an outer cover.
进一步的,所述消解仪中设置有多个消化管放置平台;所述进样机内设置有多个消化管放置平台放置位。Further, the digester is provided with multiple digestive tube placing platforms; the sample introduction machine is provided with multiple digestive tube placing platform placement positions.
进一步的,所述转运装置包括设置在所述消解仪和所述进样机之间的第一水平移驱动构、设置在所述第一水驱动机构上的竖直驱动机构以及设置在所述竖直驱动机构上的第二水平驱动机构;所述第一水平移驱动构和所述第二水平驱动机构的驱动方向垂直。Further, the transfer device includes a first horizontal driving mechanism provided between the digester and the sample feeder, a vertical driving mechanism provided on the first water driving mechanism, and a first horizontal driving mechanism provided on the first water driving mechanism. A second horizontal driving mechanism on the vertical driving mechanism; the driving directions of the first horizontal shifting driving mechanism and the second horizontal driving mechanism are vertical.
进一步的,所述第二水平驱动机构远离所述竖直驱动机构的一端设置有消化管放置平台固定机构。Further, an end of the second horizontal driving mechanism away from the vertical driving mechanism is provided with a digestive tube placement platform fixing mechanism.
进一步的,所述进样机内部底面上设置有滑轨,所述消化管放置平台底部上设置有能够与所述滑轨连接的滑槽。Further, a slide rail is provided on the internal bottom surface of the sample feeder, and a chute that can be connected to the slide rail is provided on the bottom of the digestive tube placement platform.
进一步的,所述定氮仪固定到所述进样机上;所述外罩上开设有消化管放置孔,所述消化管放置孔在所述定氮仪上的消化管安装位置处。Further, the nitrogen determiner is fixed to the sample introduction machine; a digestive tube placement hole is provided on the outer cover, and the digestive tube placement hole is at the installation position of the digestive tube on the nitrogen determiner.
进一步的,消化管安装位置上设置升降装置。Further, a lifting device is provided at the installation position of the digestive tube.
进一步的,所述取放机构为为六自由度机械臂。Furthermore, the pick-and-place mechanism is a six-degree-of-freedom robotic arm.
为了实现上述目的,第二方面,本发明还提供了一种全自动全流程凯氏法测定方法,采用如下技术方案:In order to achieve the above object, in the second aspect, the present invention also provides a fully automatic full-process Kjeldahl method for determination, adopting the following technical solution:
一种全自动全流程凯氏法测定方法,采用了如第一方面中所述的全自动全流程凯氏法测定系统,包括通过转运装置将带有消化管的消化管放置平台转运到进样机中,再通过取放机构将进样机中消化管放置平台上的消化管逐一运送到所述定氮仪上的消化管安装位置处,通过定氮仪进行实验。A fully automatic full-process Kjeldahl method for determination, using a fully automatic full-process Kjeldahl assay system as described in the first aspect, including transferring a digestive tube placement platform with a digestive tube to a sample inlet through a transfer device In the machine, the digestive tubes on the digestive tube placement platform in the sample introduction machine are transported one by one to the installation position of the digestive tubes on the nitrogen determiner through a pick-and-place mechanism, and the experiment is performed through the nitrogen determiner.
与现有技术相比,本发明的有益效果为:Compared with the prior art, the beneficial effects of the present invention are:
1、本发明在消解仪和定氮仪之间设置进样机,消解仪和进样机之间设置转运装置,进样机中设置有取放机构;进行实验时,首先通过转运装置将消解仪中的消化管放置平台送入进样机中,然后再通过进样机中的取放机构逐一的将消化管送到定氮仪上进行实验,代替了人为取放消化管的试验方式,在提高实验效率的基础上,解决了采用机械夹头夹持吸收管对消解仪中的多个消化管内的样品进行逐一吸收需要共用一个吸收管的问题,避免了多次输送样品会在吸收管内产生残留的问题,提高了实验精度;1. In the present invention, a sample feeder is provided between the digester and the nitrogen analyzer, a transfer device is provided between the digester and the sample feeder, and a pick-and-place mechanism is provided in the sample feeder; when conducting the experiment, the digester is first transferred to the sample feeder through the transfer device. The digestive tube placement platform in the instrument is fed into the sample injector, and then the digestive tubes are sent to the nitrogen analyzer one by one through the pick-and-place mechanism in the sample injector for experiments, replacing the test method of manually picking and placing the digestive tubes. On the basis of improving the experimental efficiency, it solves the problem of using a mechanical chuck to clamp the absorption tube to absorb the samples in multiple digestion tubes in the digestion instrument one by one, and needs to share one absorption tube, avoiding the possibility that samples transported multiple times will be in the absorption tube. Eliminates residual problems and improves experimental accuracy;
2、本发明在进样机上设置了外罩,降低了转运过程中外界环境对消化管的污染,在保证实验精度的基础上,代替了人为取放消化管的试验方式,提高了实验效率;2. The present invention provides an outer cover on the sample feeder, which reduces the pollution of the digestive tube from the external environment during the transfer process. On the basis of ensuring the accuracy of the experiment, it replaces the test method of manually picking and placing the digestive tube and improves the experimental efficiency;
3、因在消解仪中进行消解,以及在定氮仪中进行实验时,均需要一定的时间;而进样机中取放机构的添加,可以提高对消化管的操作灵活性,为了提高单批次实验时对更多的消化管数量进行实现,以及保证批量实验时,因消解时间造成后续实验停滞而影响批量实验下来的问题,本发明中,在消解仪中设置有多个消化管放置平台,提高了一次消解的消化管数量,保证了后续实验的连续性;同时,为了避免消解后试管一直在消解仪中,影响对消解仪的使用效率,本本发明中,在进样机内设置有多个消化管放置平台放置位,可以及时将消解仪中的消化管放置平台取出,保证了对消解仪的连续性使用;3. Digestion in the digestion instrument and experiments in the nitrogen analyzer require a certain amount of time; and the addition of a pick-and-place mechanism in the sample introduction machine can improve the operational flexibility of the digestive tube. In order to improve the single To implement a larger number of digestive tubes during batch experiments, and to ensure that during batch experiments, subsequent experiments will stagnate due to digestion time and affect the batch experiments. In the present invention, multiple digestive tubes are provided in the digestion instrument. The platform increases the number of digestive tubes digested at one time and ensures the continuity of subsequent experiments; at the same time, in order to avoid that the test tubes after digestion are always in the digestion instrument and affect the use efficiency of the digestion instrument, in the present invention, a sample introduction machine is installed There are multiple digestive tube placement platforms, and the digestive tube placement platform in the digestion instrument can be taken out in time, ensuring the continuous use of the digestion instrument;
4、本发明中通过两个水平驱动机构和一个竖直驱动机构实现了将消化管放置平台进行转运的目的,转运装置稳定性好,避免了消化管放置平台转运过程中倾斜和振动等问题,解决了消化管放置平台转运过程中消化管内样品摇晃后黏贴在消化管内壁以及溅出消化管的问题,保证了实验精度;4. In the present invention, two horizontal driving mechanisms and one vertical driving mechanism are used to realize the purpose of transferring the digestive tube placement platform. The transfer device has good stability and avoids problems such as tilt and vibration during the transfer process of the digestive tube placement platform. It solves the problem of samples in the digestive tube shaking and sticking to the inner wall of the digestive tube and splashing out of the digestive tube during the transfer process of the digestive tube placement platform, ensuring experimental accuracy;
5、本发明中在进样机内部底面上设置滑轨,对应的,在消化管放置平台底部上设置有能够与滑轨连接的滑槽,消化管放置平台通过滑轨和滑槽方式在进样机内移动,提高了消化管放置平台在进样机内移动时的稳定性,进一步避免了消化管内样品摇晃后黏贴在消化管内壁以及溅出消化管等问题;5. In the present invention, a slide rail is provided on the internal bottom surface of the sample feeder. Correspondingly, a slide rail that can be connected to the slide rail is provided on the bottom of the digestive tube placement platform. The digestive tube placement platform is moved in by the slide rail and slide groove. Movement within the sample machine improves the stability of the digestive tube placement platform when moving within the sample injector, further avoiding problems such as shaking the sample in the digestive tube and sticking to the inner wall of the digestive tube and splashing out of the digestive tube;
6、本发明中在消化管安装位置上设置升降装置,安装时,升降装置将消化管安装位置下移,蒸馏管放入到消化管后再通过升降装置将消化管安装位置上升托住消化管,避免了对每次放置消化管时需要将蒸馏管进行倾斜操作的问题,解决了对蒸馏管倾斜操作时造成蒸馏管内残留样品溅出造成污染等问题;6. In the present invention, a lifting device is provided at the installation position of the digestive tube. During installation, the lifting device moves the installation position of the digestive tube downward. After the distillation tube is put into the digestive tube, the lifting device raises the installation position of the digestive tube to support the digestive tube. , avoids the problem of tilting the distillation tube every time the digestion tube is placed, and solves the problem of contamination caused by residual samples in the distillation tube splashing out when tilting the distillation tube;
7、本发明中,将定氮仪固定到进样机上,以及将进样机和消解仪进行固定,提高了装置整体的稳定性,进样机的外罩上开设有消化管放置孔,消化管放置孔在定氮仪上的消化管安装位置处,方便对消化管的运送。7. In the present invention, the nitrogen determiner is fixed to the sample introduction machine, and the sample introduction machine and the digestion instrument are fixed, which improves the overall stability of the device. The outer cover of the sample introduction machine is provided with a hole for placing the digestive tube. Place the hole at the installation position of the digestive tube on the nitrogen analyzer to facilitate the transportation of the digestive tube.
附图说明Description of the drawings
构成本实施例的一部分的说明书附图用来提供对本实施例的进一步理解,本实施例的示意性实施例及其说明用于解释本实施例,并不构成对本实施例的不当限定。The description drawings that form a part of this embodiment are used to provide further understanding of this embodiment. The schematic embodiments and their descriptions of this embodiment are used to explain this embodiment and do not constitute an improper limitation of this embodiment.
图1为本发明实施例1的结构示意图;Figure 1 is a schematic structural diagram of Embodiment 1 of the present invention;
图2为本发明实施例1的取放机构示意图;Figure 2 is a schematic diagram of the pick-and-place mechanism in Embodiment 1 of the present invention;
图3为本发明实施例1的消化管放置平台放置位示意图;Figure 3 is a schematic diagram of the placement position of the digestive tube placement platform in Embodiment 1 of the present invention;
图4为本发明实施例1的转运装置示意图;Figure 4 is a schematic diagram of the transfer device according to Embodiment 1 of the present invention;
其中,1、消解仪;11、消化管放置平台;12、消化管放置位;13、消化管;2、进样机;21、取放机构;22、外罩;23、滑轨;24、消化管放置平台放置位;3、定氮仪;31、消化管安装位置;32、透明罩;4、转运装置;41、第一水平移驱动构;42、竖直驱动机构;43、第二水平驱动机构;44、消化管放置平台固定机构。Among them, 1. Digestion instrument; 11. Digestive tube placement platform; 12. Digestive tube placement position; 13. Digestive tube; 2. Sample feeder; 21. Pick and place mechanism; 22. Outer cover; 23. Slide rail; 24. Digestion Tube placement platform placement position; 3. Nitrogen determiner; 31. Digestive tube installation position; 32. Transparent cover; 4. Transfer device; 41. First horizontal shift driving mechanism; 42. Vertical driving mechanism; 43. Second horizontal Driving mechanism; 44. Digestive tube placement platform fixing mechanism.
具体实施方式Detailed ways
下面结合附图与实施例对本发明作进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and examples.
应该指出,以下详细说明都是示例性的,旨在对本申请提供进一步的说明。除非另有指明,本文使用的所有技术和科学术语具有与本申请所属技术领域的普通技术人员通常理解的相同含义。It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the present application. Unless otherwise defined, all technical and scientific terms used herein have the same meanings commonly understood by one of ordinary skill in the art to which this application belongs.
实施例1:Example 1:
采用现有的凯氏定氮仪进行凯氏定氮实验时,其过程为将多个带有样品的消化管在消解仪中进行消解,然后对所有消化管按照一定的顺序逐一的放到定氮仪上进行蒸馏、吸收和滴定等过程,此种方式需要人为取放消化管,整个实验过程效率较低;而采用机械夹头夹持吸收管的方式,对消解仪中的多个消化管内的样品进行逐一吸收后送到定氮仪中的消化管中,虽然避免了人为取放消化管,但是,样品的多次输送需要共用一个吸收管,多次输送样品会在吸收管内产生残留,残留样品会对后续实验产生影响,影响了实验精度;为了解决上述问题,如图1、图2、图3和图4所示,本实施例提供了一种全自动全流程凯氏法测定系统,包括包括用于向消化管进样的前处理机构、消解仪1、进样机2和定氮仪3;When using the existing Kjeldahl nitrogen analyzer to perform a Kjeldahl nitrogen determination experiment, the process is to digest multiple digestion tubes with samples in the digestion instrument, and then place all the digestion tubes one by one in a certain order. Processes such as distillation, absorption, and titration are carried out on a nitrogen analyzer. This method requires manual handling of the digestive tubes, and the entire experimental process is inefficient. However, the mechanical chuck is used to clamp the absorption tubes, and the multiple digestion tubes in the digestion instrument are The samples are absorbed one by one and sent to the digestion tube in the nitrogen analyzer. Although manual picking and placing of the digestion tube is avoided, the same absorption tube needs to be shared for multiple transportation of the sample. Multiple transportation of the sample will produce residues in the absorption tube. The residual sample will have an impact on subsequent experiments and affect the experimental accuracy; in order to solve the above problems, as shown in Figure 1, Figure 2, Figure 3 and Figure 4, this embodiment provides a fully automatic and full-process Kjeldahl method measurement system , including a pre-treatment mechanism for injecting samples into the digestive tube, digestion instrument 1, sample injector 2 and nitrogen determiner 3;
所述消解仪1中设置有消化管放置平台11,所述消化管放置平台11上设置有多个消化管放置位12;所述消解仪1和所述进样机2之间设置转运装置4,所述转运装置4能够将所述消化管放置平台11转运到所述进样机2中;The digestion instrument 1 is provided with a digestive tube placement platform 11, and a plurality of digestive tube placement positions 12 are provided on the digestive tube placement platform 11; a transfer device 4 is provided between the digestion instrument 1 and the sample introduction machine 2 , the transfer device 4 can transfer the digestive tube placement platform 11 to the sample introduction machine 2;
所述进样机2中设置有取放机构21,能够将所述消化管放置平台11上的消化管13逐一的运送到所述定氮仪3上的消化管安装位置31处;所述进样机2上设置有外罩22。The sample introduction machine 2 is provided with a pick-and-place mechanism 21, which can transport the digestive tubes 13 on the digestive tube placement platform 11 one by one to the digestive tube installation position 31 on the nitrogen determiner 3; The prototype 2 is provided with an outer cover 22 .
可以理解的,本实施例中的所述消解仪1和所述定氮仪3可以通过现有设备或对现有设备的改进实现;所述消化管放置平台11可以理解为设置有多个试管放置孔的试管架等机构,消化管放置位12可以理解为放置孔等结构;可选的,为了方便利用所述转运装置4对所述消化管放置平台11的转运,可以在所述消解仪1的侧面上开设操作孔,方便所述转运装置4的工作;为了保证消化管可以顺利的放到所述定氮仪3上的消化管安装位置31,在一些实施例中,可以将定氮仪上的蒸馏管的长度适当减小,使得蒸馏管的下端与消化管安装位置存在一定的距离,保证蒸馏管的下端可以放到消化管内;在另外一些实施例中,还可以在消化管安装位置31上设置液压升降装置、气压升降装置或电升降装置等升降装置,安装时,升降装置将消化管安装位置下移,蒸馏管放入到消化管后再通过升降装置将消化管安装位置上升托住消化管;或者在其他一些实施例中,通过在蒸馏装置上设置液压升降装置或气压升降装置等,安装时,升降装置将蒸馏装置提升,蒸馏管上升,取放机构21将消化管安装到消化管安装位置后,升降装置将蒸馏装置下移,蒸馏管下移到消化管内,完成消化管的运送;为了方便对定氮仪3内的观察,本实施例中,在所述定氮仪3上设置了透明罩32。It can be understood that the digester 1 and the nitrogen determiner 3 in this embodiment can be implemented by existing equipment or improvements to existing equipment; the digestive tube placement platform 11 can be understood as being provided with multiple test tubes. Mechanisms such as test tube racks that place holes, the digestive tube placement position 12 can be understood as placement holes and other structures; optionally, in order to facilitate the transfer of the digestive tube placement platform 11 by the transfer device 4, the digestive tube placement position 12 can be placed in the digestion instrument An operating hole is provided on the side of 1 to facilitate the work of the transfer device 4; in order to ensure that the digestive tube can be smoothly placed in the digestive tube installation position 31 on the nitrogen determiner 3, in some embodiments, the nitrogen determiner can be The length of the distillation tube on the instrument is appropriately reduced, so that there is a certain distance between the lower end of the distillation tube and the installation position of the digestive tube, ensuring that the lower end of the distillation tube can be placed in the digestive tube; in other embodiments, the lower end of the distillation tube can also be installed in the digestive tube. Position 31 is provided with lifting devices such as a hydraulic lifting device, a pneumatic lifting device or an electric lifting device. During installation, the lifting device moves the installation position of the digestive tube downwards. After the distillation tube is placed in the digestive tube, the lifting device raises the installation position of the digestive tube. Hold the digestive tube; or in some other embodiments, a hydraulic lifting device or a pneumatic lifting device is provided on the distillation device. During installation, the lifting device lifts the distillation device, the distillation tube rises, and the pick-and-place mechanism 21 installs the digestive tube. After arriving at the installation position of the digestive tube, the lifting device moves the distillation device downward, and the distillation tube moves downward into the digestive tube to complete the transportation of the digestive tube; in order to facilitate the observation in the nitrogen determiner 3, in this embodiment, in the nitrogen determination A transparent cover 32 is provided on the instrument 3.
可选的,所述前处理机构可以采用机器人或自动进样机等设备实现,首先将样品加入消化管,然后将催化剂和酸加入消化管,最后将消化管放置到消化管放置平台11上;比如,采用带有多自由度机械手的多个机器人,一个或多个机械手可以分别将盛放样品、催化剂和酸的容器抓取到消化管口处,并将样品、催化剂和酸倒入消化管内;消化管也可以由一个机械手抓取,消化管被倒入样品、催化剂和酸后,再通过机械手将消化管放置到消化管放置平台11上的相应位置,整个过程为自动化过程。Optionally, the pretreatment mechanism can be implemented using equipment such as a robot or an automatic sample feeder. First, the sample is added to the digestive tube, then the catalyst and acid are added to the digestive tube, and finally the digestive tube is placed on the digestive tube placement platform 11; For example, using multiple robots with multi-degree-of-freedom manipulators, one or more manipulators can grab containers containing samples, catalysts, and acids to the mouth of the digestion tube, and pour the samples, catalysts, and acids into the digestion tube. The digestive tube can also be grabbed by a robot. After the sample, catalyst and acid are poured into the digestive tube, the robot then places the digestive tube into the corresponding position on the digestive tube placement platform 11. The entire process is an automated process.
具体的,在所述消解仪1和所述定氮仪3之间设置所述进样机2,所述消解仪1和所述进样机2之间设置所述转运装置4,所述进样机2中设置有所述取放机构21;进行实验时,首先通过所述转运装置4将所述消解仪1中的消化管放置平台11送入所述进样机2中,然后再通过所述进样机2中的所述取放机构21逐一的将消化管13送到所述定氮仪3上进行实验,代替了人为取放消化管的试验方式,在提高实验效率的基础上,解决了采用机械夹头夹持吸收管对消解仪中的多个消化管内的样品进行逐一吸收需要共用一个吸收管的问题,避免了多次输送样品会在吸收管内产生残留的问题,提高了实验精度;同时,在所述进样机2上设置了所述外罩22,降低了转运过程中外界环境对消化管13内样品的污染,在保证实验精度的基础上,代替了人为取放消化管的试验方式,提高了实验效率。Specifically, the sample feeder 2 is disposed between the digestion instrument 1 and the nitrogen determiner 3, and the transfer device 4 is disposed between the digestion instrument 1 and the sample feeder 2. The sample machine 2 is provided with the pick-and-place mechanism 21; when performing an experiment, the digestive tube placing platform 11 in the digestion apparatus 1 is first sent to the sample introduction machine 2 through the transfer device 4, and then through The pick-and-place mechanism 21 in the sample introduction machine 2 sends the digestive tubes 13 to the nitrogen determiner 3 one by one for experiments, replacing the test method of manually picking and placing the digestive tubes, and on the basis of improving the experimental efficiency. , which solves the problem of using a mechanical chuck to clamp the absorption tube to absorb the samples in multiple digestion tubes in the digestion instrument one by one and requiring a shared absorption tube. It avoids the problem of residuals in the absorption tube due to multiple transports of samples, and improves efficiency. Experimental accuracy; at the same time, the outer cover 22 is provided on the sample introduction machine 2, which reduces the contamination of the samples in the digestive tube 13 by the external environment during the transfer process. On the basis of ensuring the experimental accuracy, it replaces manual picking and placing of digestion. The tube test method improves the experimental efficiency.
因在所述消解仪1中进行消解,以及在所述定氮仪3中进行实验时,均需要一定的时间;而在所述进样机2中取放机构21的添加,可以提高对消化管13的操作灵活性,为了提高单批次实验时对更多的消化管数量进行实现,以及保证批量实验时,因消解时间造成后续实验停滞而影响批量实验下来的问题,本实施例中,在所述消解仪1中设置有多个消化管放置平台11,提高了一次消解的消化管数量,保证了后续实验的连续性。可选的,将所述消解仪1设置为多层结构,不同消化管放置平台位于不同层上,当然,也可以在单层或多层的消解仪1中水平放置多个消化管放置平台来实现多消化管放置平台的设置。同时,为了避免消解后试管一直在所述消解仪1中,影响对消解仪1的使用效率,本实施例中,在所述进样机2内设置有多个消化管放置平台放置位24,可以及时将所述消解仪1中的消化管放置平台11取出,保证了对所述消解仪的连续性使用。Because digestion in the digestion instrument 1 and experiments in the nitrogen determiner 3 require a certain amount of time; and the addition of the pick-and-place mechanism 21 in the sample introduction machine 2 can improve the digestion efficiency. In order to improve the operational flexibility of the tube 13, more digestive tubes can be used in a single batch experiment, and to ensure that in batch experiments, subsequent experiments will be stagnated due to digestion time and affect the batch experiments. In this embodiment, Multiple digestive tube placement platforms 11 are provided in the digestion apparatus 1, which increases the number of digestive tubes digested at one time and ensures the continuity of subsequent experiments. Optionally, the digestion apparatus 1 is configured as a multi-layer structure, with different digestive tube placement platforms located on different layers. Of course, multiple digestive tube placement platforms can also be placed horizontally in a single-layer or multi-layer digestion apparatus 1. Realize the setting of multiple digestive tube placement platforms. At the same time, in order to avoid that the test tubes after digestion are always in the digestion apparatus 1 and affect the use efficiency of the digestion apparatus 1, in this embodiment, a plurality of digestive tube placement platforms 24 are provided in the sample introduction machine 2. The digestive tube placing platform 11 in the digestion apparatus 1 can be taken out in time, ensuring the continuous use of the digestion apparatus.
本实施例中,所述转运装置4可以包括设置在所述消解仪1和所述进样机2之间的第一水平移驱动构41、设置在所述第一水驱动机构41上的竖直驱动机构42以及设置在所述竖直驱动机构42上的第二水平驱动机构43;所述第一水平移驱动构41和所述第二水平驱动机构42的驱动方向垂直。所述第二水平驱动机构43远离所述竖直驱动机构42的一端设置有消化管放置平台固定机构44。In this embodiment, the transfer device 4 may include a first horizontal shift drive mechanism 41 disposed between the digestion instrument 1 and the sample feeder 2 , and a vertical shift drive mechanism disposed on the first water drive mechanism 41 . The straight driving mechanism 42 and the second horizontal driving mechanism 43 provided on the vertical driving mechanism 42; the driving directions of the first horizontal driving mechanism 41 and the second horizontal driving mechanism 42 are vertical. An end of the second horizontal driving mechanism 43 away from the vertical driving mechanism 42 is provided with a digestive tube placement platform fixing mechanism 44 .
可选的,所述第一水平移驱动构41和所述第二水平驱动机构43可以采用直线电机等装置实现,所述第一水平移驱动构41可以驱动所述竖直驱动机构42和所述第二水平驱动机构43在所述消解仪1和所述进样机2之间做水平运动;所述竖直驱动机构42固定到所述第一水平移驱动构41的移动部件上,比如固定到直线电机中皮带驱动的滑块上,所述竖直驱动机构42可以采用液压升降装置、气压升降装置或电动升降装置等,所述竖直驱动机构42可以驱动所述第二水平驱动机构43上下移动;所述第二水平驱动机构43固定到所述竖直驱动机构42的移动部件上,比如固定到升降装置的升降杆上;所述消化管放置平台固定机构44可以固定到所述第二水平驱动机构43的移动部件上,比如固定到直线电机中皮带驱动的滑块上,所述第二水平驱动机构43可以带动所述消化管放置平台固定机构44穿过所述消解仪1侧面上的操作孔后,在所述消解仪1中前后移动。通过所述第一水平移驱动构41、所述竖直驱动机构42和所述第二水平驱动机构43的设置,可以实现所述消化管放置平台固定机构44在水平位置和竖直位置上的任意移动,从而实现对消化管放置平台11的运送;所述消化管放置平台固定机构44可以采用夹爪和插板等结构实现,比如采用夹爪时,可以直接对所述消化管放置平台11进行夹持,采用插板时,可以插入所述消化管放置平台11的底部后将所述消化管放置平台11托起。Optionally, the first horizontal driving mechanism 41 and the second horizontal driving mechanism 43 can be implemented by linear motors and other devices, and the first horizontal driving mechanism 41 can drive the vertical driving mechanism 42 and the vertical driving mechanism 42 . The second horizontal drive mechanism 43 moves horizontally between the digestion instrument 1 and the sample feeder 2; the vertical drive mechanism 42 is fixed to the moving part of the first horizontal shift drive mechanism 41, such as Fixed to the belt-driven slide block in the linear motor, the vertical driving mechanism 42 can adopt a hydraulic lifting device, a pneumatic lifting device or an electric lifting device, etc. The vertical driving mechanism 42 can drive the second horizontal driving mechanism 43 moves up and down; the second horizontal driving mechanism 43 is fixed to the moving part of the vertical driving mechanism 42, such as to the lifting rod of the lifting device; the digestive tube placement platform fixing mechanism 44 can be fixed to the On the moving part of the second horizontal driving mechanism 43, such as being fixed to the belt-driven slider in the linear motor, the second horizontal driving mechanism 43 can drive the digestive tube placement platform fixing mechanism 44 to pass through the digestion instrument 1 After opening the operating hole on the side, move the digester 1 back and forth. Through the arrangement of the first horizontal driving mechanism 41 , the vertical driving mechanism 42 and the second horizontal driving mechanism 43 , the position of the digestive tube placement platform fixing mechanism 44 in the horizontal position and the vertical position can be realized. Move arbitrarily to realize the transportation of the digestive tube placement platform 11; the fixed mechanism 44 of the digestive tube placement platform can be implemented by using structures such as clamping claws and inserting plates. For example, when using clamping claws, the digestive tube placing platform 11 can be directly transported For clamping, when an inserting plate is used, the bottom of the digestive tube placement platform 11 can be inserted and the digestive tube placement platform 11 can be lifted up.
可以理解的,通过两个水平驱动机构和一个竖直驱动机构实现了将消化管放置平台11进行转运的目的,转运装置4工作稳定性好,避免了消化管放置平台11在转运过程中发生倾斜和振动等问题,解决了消化管放置平台11转运过程中消化管内样品摇晃后黏贴在消化管13内壁以及溅出消化管13的问题,保证了实验精度。It can be understood that the purpose of transferring the digestive tube placement platform 11 is achieved through two horizontal drive mechanisms and one vertical drive mechanism. The transfer device 4 has good working stability and avoids the digestive tube placement platform 11 from tilting during the transfer process. and vibration, which solves the problem of samples in the digestive tube shaking and then sticking to the inner wall of the digestive tube 13 and splashing out of the digestive tube 13 during the transfer process of the digestive tube placement platform 11, ensuring experimental accuracy.
在其他一些实施例中,所述转运装置4可以直接采用AGV小车等结构,消化管放置平台11可以直接通过螺栓或焊接等常规连接方式固定在AGV小车上,进行消解后,通过AGV小车将带有消化管13的化管放置平台11运送到进样机2中,再通过取放机构21进行后续操作;当然,在一些实施例中,还可以不设置进样机,进行消解后,通过AGV小车将带有消化管13的化管放置平台11运送到消解仪附近,直接利用机械臂等结构将消化管13放置到定氮仪上。In some other embodiments, the transfer device 4 can directly adopt a structure such as an AGV trolley, and the digestive tube placement platform 11 can be directly fixed on the AGV trolley through conventional connection methods such as bolts or welding. After digestion, the AGV trolley will The digestion tube placement platform 11 with the digestive tube 13 is transported to the sample introduction machine 2, and then the subsequent operations are performed through the pick-and-place mechanism 21; of course, in some embodiments, the sample introduction machine may not be provided, and after digestion, the digestion is carried out through the AGV The trolley transports the chemical tube placement platform 11 with the digestive tube 13 to the vicinity of the digestion instrument, and directly uses a mechanical arm or other structures to place the digestive tube 13 on the nitrogen analyzer.
所述消化管放置平台11送入所述进样机2后,在所述取放机构21夹持消化管13时,所述消化管放置平台11需要稳定,才能保证对消化管13夹持动作的顺利实现;因此,本实施例中,在所述进样机2内部底面上设置有滑轨23,在所述消化管放置平台11底部上设置有能够与所述滑轨23连接的滑槽;在所述转运装置4将所述消化管放置平台11送入到所述进样机2的过程中,可以将所述滑槽插入所述滑轨23内,所述滑槽和所述滑轨23的配合,在一定程度上提高了所述消化管放置平台11在所述进样机2底部的稳定性,避免了所述取放机构21夹持消化管13时发生过度摇晃或所述消化管放置平台11发生较大偏移的问题,提高了稳定性,使得所述取放机构21可以顺利夹持消化管13。After the digestive tube placement platform 11 is sent into the sample introduction machine 2, when the pick-and-place mechanism 21 clamps the digestive tube 13, the digestive tube placement platform 11 needs to be stable to ensure the clamping action of the digestive tube 13. Therefore, in this embodiment, a slide rail 23 is provided on the internal bottom surface of the sample feeder 2, and a chute capable of connecting with the slide rail 23 is provided on the bottom of the digestive tube placement platform 11. ; In the process of the transfer device 4 sending the digestive tube placement platform 11 to the sample feeder 2, the chute can be inserted into the slide rail 23, and the chute and the slide The cooperation of the rails 23 improves the stability of the digestive tube placement platform 11 at the bottom of the sample feeder 2 to a certain extent, and avoids excessive shaking or the occurrence of the digestive tube 13 when the pick-and-place mechanism 21 clamps the digestive tube 13. The problem of large deviation of the digestive tube placement platform 11 is improved, so that the pick-and-place mechanism 21 can smoothly clamp the digestive tube 13.
为了提高装置整体的稳定性,可以将所述定氮仪3通过焊接或螺栓连接等方式固定到所述进样机2上,以及将所述进样机2通过焊接或螺栓连接等方式和所述消解仪1进行固定;所述外罩22上开设有消化管放置孔,所述消化管放置孔在所述定氮仪上的消化管安装位置处,方便对所述消化管13的运送。为了方便观察所述消化管13的运送情况,以及实时查看所述送样机内消化管放置平台11和消化管13的整体情况,本实施例中,将所述外罩22设置为透明罩。In order to improve the overall stability of the device, the nitrogen determiner 3 can be fixed to the sample feeder 2 by welding or bolting, and the sample feeder 2 can be connected to the sample feeder 2 by welding or bolting. The digestion instrument 1 is fixed; the outer cover 22 is provided with a hole for placing the digestive tube, and the hole for placing the digestive tube is at the installation position of the digestive tube on the nitrogen analyzer to facilitate the transportation of the digestive tube 13. In order to facilitate observation of the transportation of the digestive tube 13 and to view the overall situation of the digestive tube placement platform 11 and the digestive tube 13 in the sample delivery machine in real time, in this embodiment, the outer cover 22 is set as a transparent cover.
可以理解的,所述定氮仪的消化管安装位置是指消解位,在放置消化管3时,对消化管13的放入角度、高度等位姿均有要求,所以,本实施例中,所述取放机构21设置为六自由度机械臂,保证了对消化管13运送和安装的灵活性;可以理解的,在所述取放机构21的端部设置夹持消化管的夹爪,所述夹爪的设置为常规设置,在此不再详述。It can be understood that the installation position of the digestive tube of the nitrogen analyzer refers to the digestion position. When placing the digestive tube 3, there are requirements for the angle, height and other postures of the digestive tube 13. Therefore, in this embodiment, The pick-and-place mechanism 21 is configured as a six-degree-of-freedom mechanical arm, ensuring flexibility in transporting and installing the digestive tube 13; it can be understood that a clamping claw for holding the digestive tube is provided at the end of the pick-and-place mechanism 21. The settings of the clamping jaws are conventional settings and will not be described in detail here.
实施例2:Example 2:
本实施例提供了一种全自动全流程凯氏法测定方法,采用了如实施例1中所述的全自动全流程凯氏法测定系统,包括通过转运装置4将带有消化管13的消化管放置平台11转运到进样机2中,再通过取放机构21将进样机2中消化管放置平台11上的消化管13逐一运送到所述定氮仪3上的消化管安装位置处,通过定氮仪3进行实验。This embodiment provides a fully automatic and full-process Kjeldahl method, which adopts the fully automatic and full-flow Kjeldahl method as described in Example 1, including transferring the digestion tube with the digestive tube 13 through the transfer device 4. The tube placement platform 11 is transferred to the sample feeder 2, and then the digestive tubes 13 on the digester tube placement platform 11 in the sample feeder 2 are transported one by one to the digestive tube installation position on the nitrogen determiner 3 through the pick-and-place mechanism 21. , conduct experiments through nitrogen analyzer 3.
以上所述仅为本实施例的优选实施例而已,并不用于限制本实施例,对于本领域的技术人员来说,本实施例可以有各种更改和变化。凡在本实施例的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本实施例的保护范围之内。The above descriptions are only preferred embodiments of this embodiment and are not intended to limit this embodiment. For those skilled in the art, this embodiment may have various modifications and changes. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of this embodiment shall be included in the protection scope of this embodiment.
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