CN116678875B - Alcohol degree detection method and device based on gold nanoparticle self-assembly system - Google Patents
Alcohol degree detection method and device based on gold nanoparticle self-assembly system Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 83
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 83
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 82
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000001338 self-assembly Methods 0.000 title claims abstract description 19
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 11
- 159000000001 potassium salts Chemical class 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
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- 239000002077 nanosphere Substances 0.000 description 1
- IRPDISVJRAYFBI-UHFFFAOYSA-N nitric acid;potassium Chemical compound [K].O[N+]([O-])=O IRPDISVJRAYFBI-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域Technical field
本发明涉及酒精度检测领域,具体涉及基于金纳米粒子自组装体系的酒精度检测方法及装置。The invention relates to the field of alcohol content detection, and specifically relates to an alcohol content detection method and device based on a gold nanoparticle self-assembly system.
背景技术Background technique
白酒是市场上一种主流的蒸馏酒,其以曲类、酒母为糖化发酵剂,利用淀粉质或糖质为原料,经蒸煮、糖化、发酵、蒸馏、陈酿、勾兑等步骤酿制而成。酒精度是白酒生产和销售过程中的一项重要指标,其代表了白酒中乙醇的体积百分比。目前市售的白酒酒精度主要在18~78度,依据酒精度大致可分为低度、中度、高度、特高度。Liquor is a mainstream distilled liquor on the market. It uses koji and distiller's sake as saccharification fermentation agents, starch or sugar as raw materials, and is brewed through cooking, saccharification, fermentation, distillation, aging, blending and other steps. Alcohol content is an important indicator in the production and sales process of liquor, which represents the volume percentage of ethanol in liquor. The alcohol content of currently commercially available liquor is mainly between 18 and 78 degrees. According to the alcohol content, it can be roughly divided into low, medium, high and extra high.
白酒的酒精度影响着白酒的口感,白酒的酒精度检测在生产销售、市场监管中十分重要。传统的白酒酒精度的检测方法主要有比重法、色谱法、红外光谱法等。近年来,一些新的酒精度检测方法也逐渐普及,包括利用荧光纳米的酒精度检测试纸等等。但是,这些白酒酒精度的检测方法检测步骤繁琐,检测结果等待时间长,难以实现高效、大量地区分。The alcohol content of liquor affects the taste of liquor. The alcohol content detection of liquor is very important in production, sales and market supervision. The traditional detection methods of liquor alcohol content mainly include specific gravity method, chromatography, infrared spectroscopy, etc. In recent years, some new alcohol detection methods have gradually become popular, including alcohol detection test strips using fluorescent nanometers. However, these liquor alcohol detection methods have cumbersome detection steps and long waiting times for detection results, making it difficult to achieve efficient and large-scale differentiation.
发明内容Contents of the invention
本发明的一个目的在于提供一种基于金纳米粒子自组装体系的酒精度检测方法,该方法基于发明人团队对金纳米粒子选择性自组装的研究,利用金纳米粒子在不同含量的乙醇、盐中一维线性组装的量不同而产生不同的颜色的特点,能够将特定酒精度的白酒与金纳米粒子、盐混合后,快速地检测出当前白酒的酒精度范围,进而实现高效、快速、大量地确定待检测白酒的酒精度。One object of the present invention is to provide an alcohol content detection method based on a gold nanoparticle self-assembly system. This method is based on the inventor's team's research on the selective self-assembly of gold nanoparticles, using gold nanoparticles in different contents of ethanol and salt. Different amounts of one-dimensional linear assembly produce different colors. After mixing liquor with a specific alcohol content with gold nanoparticles and salt, the current alcohol content range of the liquor can be quickly detected, thereby achieving efficient, rapid and large-scale testing. Determine the alcohol content of the liquor to be tested.
本发明通过下述技术方案实现:The present invention is realized through the following technical solutions:
基于金纳米粒子自组装体系的酒精度检测方法,包括以下步骤:The alcohol content detection method based on the self-assembly system of gold nanoparticles includes the following steps:
将待检测白酒分别加入至若干份检测体系中,所述若干份检测体系中的各份检测体系均包括金纳米粒子和钾盐,且各份检测体系中的钾盐的质量不同;The liquor to be detected is added to several detection systems respectively, each detection system in the several detection systems includes gold nanoparticles and potassium salt, and the potassium salt in each detection system has different qualities;
待检测白酒与检测体系接触后,基于若干份检测体系的颜色变化,判断待检测白酒的酒精度;After the liquor to be tested comes into contact with the detection system, the alcohol content of the liquor to be detected is determined based on the color changes of several portions of the detection system;
其中,所述金纳米粒子采用柠檬酸还原法合成。Wherein, the gold nanoparticles are synthesized by citric acid reduction method.
本技术方案中,金纳米粒子为采用现有的柠檬酸还原法合成的球形金纳米颗粒。具体地,可以在沸腾的纯水中加入氯金酸,之后快速加入柠檬酸钠,通过调节加热温度使其始终保持沸腾搅拌状态并反应一段时间,例如20~30分钟,至溶液颜色变为酒红色时,表明溶液中已经生成了金纳米球颗粒,反应完成,降温后得到金纳米粒子的初产物。随后进行离心处理,将含有多余的副产物的上清液倒掉,底部的金纳米粒子置于新的离心管中,加纯水定容即得到金纳米粒子。In this technical solution, the gold nanoparticles are spherical gold nanoparticles synthesized using the existing citric acid reduction method. Specifically, chloroauric acid can be added to boiling pure water, and then sodium citrate can be quickly added, and the heating temperature can be adjusted to keep it in a boiling and stirring state and react for a period of time, such as 20 to 30 minutes, until the color of the solution changes to wine. When red, it indicates that gold nanosphere particles have been generated in the solution, the reaction is completed, and the primary product of gold nanoparticles is obtained after cooling. Subsequently, centrifugation is performed, and the supernatant containing excess by-products is poured out. The gold nanoparticles at the bottom are placed in a new centrifuge tube, and pure water is added to the volume to obtain gold nanoparticles.
本技术方案中,各检测体系中均包括一定量的金纳米粒子和钾盐。所述钾盐可以是硝酸钾、氯化钾等钾盐,优选地,所述钾盐为硝酸钾。金纳米粒子的自组装的机理为:金纳米粒子在以不同乙醇含量为溶剂时,在静电作用力的驱动下,单个金纳米粒子出现一维线性组装。当处于组装态下的金纳米粒子的数量较少、链长度短时,混合物整体呈现出红色,随着单个金纳米粒子数量减少、组装态下的金纳米粒子数量增加、链长度增长,混合物整体颜色由红色向酒红色、紫色、蓝色、深蓝色转变。In this technical solution, each detection system includes a certain amount of gold nanoparticles and potassium salt. The potassium salt may be potassium nitrate, potassium chloride or other potassium salts. Preferably, the potassium salt is potassium nitrate. The mechanism of self-assembly of gold nanoparticles is as follows: When gold nanoparticles use different ethanol contents as solvents, driven by electrostatic forces, single gold nanoparticles appear in one-dimensional linear assembly. When the number of gold nanoparticles in the assembled state is small and the chain length is short, the entire mixture appears red. As the number of individual gold nanoparticles decreases, the number of gold nanoparticles in the assembled state increases, and the chain length increases, the overall mixture appears red. The color changes from red to burgundy, purple, blue, and dark blue.
影响金纳米粒子组装态数量的因素包括酒精中乙醇含量和体系中钾盐含量。因此,本技术方案中,当待检测白酒中的乙醇含量未知时,将白酒加入至一份或多份检测体系中,由于各检测体系中的金纳米粒子含量相同、钾盐含量不同,在白酒加入后,各检测体系中钾盐的质量不同将造成同一待检测白酒在不同的检测体系中呈现出特定的颜色。Factors that affect the number of gold nanoparticle assembly states include the ethanol content in the alcohol and the potassium salt content in the system. Therefore, in this technical solution, when the ethanol content in the liquor to be detected is unknown, the liquor is added to one or more detection systems. Since the gold nanoparticle content in each detection system is the same and the potassium salt content is different, in the liquor After addition, the different qualities of potassium salt in each detection system will cause the same liquor to be tested to show a specific color in different detection systems.
例如,38度的白酒在加入至300μL金纳米粒子和80μL硝酸钾、浓度为0.5mol/L的检测体系中时,白酒与检测体系充分接触后,检测体系呈红色;当38度的白酒在加入的检测体系中硝酸钾的体积为100μL时,检测体系呈紫色;当38度的白酒在加入的检测体系中硝酸钾的体积为120μL时,检测体系呈蓝色For example, when 38-degree liquor is added to a detection system with 300 μL gold nanoparticles and 80 μL potassium nitrate at a concentration of 0.5 mol/L, the detection system will turn red after the liquor is fully in contact with the detection system; when 38-degree liquor is added When the volume of potassium nitrate in the detection system is 100 μL, the detection system appears purple; when the volume of potassium nitrate in the detection system of 38-degree liquor is 120 μL, the detection system appears blue.
类似地,56度的白酒在加入至300μL金纳米粒子和80μL硝酸钾、浓度为0.5mol/L的检测体系中时,白酒与检测体系充分接触后,检测体系呈紫色;而当56度的白酒在加入的检测体系中硝酸钾的体积为100μL和120μL时,检测体系呈蓝色。Similarly, when 56-degree liquor is added to a detection system with 300 μL gold nanoparticles and 80 μL potassium nitrate at a concentration of 0.5 mol/L, the detection system turns purple after the liquor fully contacts the detection system; and when 56-degree liquor When the volume of potassium nitrate added to the detection system is 100 μL and 120 μL, the detection system turns blue.
基于显色的特点,本技术方案中,可以采用一份检测体系进行判断,例如可以通过300μL金纳米粒子、80μL硝酸钾、浓度为0.5mol/L的检测体系,在加入白酒后是否呈现红色来判断其是否为低度白酒,是否呈现紫色来判断其是否为中度白酒,以及是否呈现蓝色来判断其是否为高度白酒。Based on the characteristics of color development, in this technical solution, a detection system can be used for judgment. For example, it can be judged by whether a detection system with 300 μL gold nanoparticles, 80 μL potassium nitrate, and a concentration of 0.5 mol/L appears red after adding white wine. Determine whether it is a low-alcohol liquor, whether it is purple to determine whether it is a medium-alcohol liquor, and whether it is blue to determine whether it is a high-alcohol liquor.
本技术方案中,也可以采用多份检测体系相结合来进一步提高判断的准确性。例如,可以设置两份或者多份检测体系,各检测体系的钾盐质量不同,从而使待检测白酒加入后,以三份检测体系为例,检测体系组能够呈现出红-紫-蓝,紫-蓝-蓝,蓝-蓝-蓝的区分,从而允许检测人员能够快速、高效地对当前白酒酒精度数做出判断。In this technical solution, multiple detection systems can also be combined to further improve the accuracy of judgment. For example, two or more detection systems can be set up. The potassium salt quality of each detection system is different, so that after the liquor to be tested is added, taking three detection systems as an example, the detection system group can show red-purple-blue, purple -Blue-blue, blue-blue-blue distinction, allowing inspectors to quickly and efficiently judge the current alcohol content of liquor.
通过上述检测方法,能够根据一份或多份检测体系在加入待检测白酒后所呈现的颜色,快速地识别出白酒的酒精度范围,检测的时间通常在半分钟左右,且其灵敏度高、操作简单、制备成本低,在白酒的市场监管上具有广泛的应用价值。Through the above detection method, the alcohol content range of liquor can be quickly identified based on the color of one or more detection systems after adding the liquor to be detected. The detection time is usually about half a minute, and its sensitivity is high and the operation is It is simple, has low preparation cost and has wide application value in the market supervision of liquor.
进一步地,所述金纳米粒子与钾盐的摩尔比为0.04~0.02。本技术方案中,若金纳米粒子与钾盐的配比过高,不仅提高了检测成本,而且导致体系中的钾盐将不足使金纳米粒子进行组装,从而体系中颜色变化不够明显;相反地,若金纳米粒子与钾盐的配比过低,则体系中金纳米粒子更易组装,检测体系容易呈现蓝色或深蓝色,不利于通过颜色区分酒精度范围。因此,本技术方案中,金纳米粒子与钾盐的摩尔比为0.04~0.02,优选地,金纳米粒子与钾盐的摩尔比为0.0375~0.025。Further, the molar ratio of the gold nanoparticles to the potassium salt is 0.04 to 0.02. In this technical solution, if the ratio of gold nanoparticles to potassium salt is too high, it will not only increase the detection cost, but also result in insufficient potassium salt in the system to assemble the gold nanoparticles, so the color change in the system will not be obvious enough; conversely, , if the ratio of gold nanoparticles to potassium salt is too low, the gold nanoparticles in the system will be easier to assemble, and the detection system will easily appear blue or dark blue, which is not conducive to distinguishing the alcohol content range by color. Therefore, in this technical solution, the molar ratio of gold nanoparticles to potassium salt is 0.04 to 0.02. Preferably, the molar ratio of gold nanoparticles to potassium salt is 0.0375 to 0.025.
进一步地,所述若干份检测体系中,钾盐质量最大的检测体系与钾盐质量最小的检测体系的钾盐的摩尔比为1.2~2.0。当设置有至少两份检测体系时,两份检测体系的钾盐含量不宜过于接近,否则通过肉眼难以判断出检测体系颜色的差异。Further, among the several detection systems, the molar ratio of potassium salts in the detection system with the largest potassium salt mass and the detection system with the smallest potassium salt mass is 1.2 to 2.0. When there are at least two detection systems, the potassium salt content of the two detection systems should not be too close, otherwise it will be difficult to judge the color difference of the detection systems with the naked eye.
作为本发明中检测体系组的一种优选设置方式,所述若干份检测体系包括三份检测体系,所述三份检测体系中的钾盐的摩尔比为4:5:6。本技术方案中,检测体系组包括三份检测体系,三份检测体系的金纳米粒子含量相同,钾盐的摩尔比为4:5:6。As a preferred arrangement of the detection system group in the present invention, the several detection systems include three detection systems, and the molar ratio of potassium salts in the three detection systems is 4:5:6. In this technical solution, the detection system group includes three detection systems, the three detection systems have the same content of gold nanoparticles, and the molar ratio of potassium salt is 4:5:6.
进一步地,待检测白酒与检测体系接触后120秒内,基于若干份检测体系的颜色变化判断待检测白酒的酒精度。随着接触时间的增长,检测体系中单个的金纳米粒子向组装态转变的数量将增加,检测体系的整体颜色将更趋向于深蓝色,影响对颜色的判断。因此,本技术方案中,优选地,检测在两分钟以内完成,进一步优选地,检测在一分钟内完成。Furthermore, within 120 seconds after the liquor to be detected comes into contact with the detection system, the alcohol content of the liquor to be detected is determined based on the color changes of several portions of the detection system. As the contact time increases, the number of individual gold nanoparticles in the detection system that transition to the assembled state will increase, and the overall color of the detection system will tend to be darker blue, affecting the judgment of color. Therefore, in this technical solution, preferably, the detection is completed within two minutes, and further preferably, the detection is completed within one minute.
进一步地,加入至每份检测体系中的待检测白酒的体积为0.05~4.00mL。Further, the volume of the liquor to be detected added to each detection system is 0.05-4.00 mL.
本发明的另一个目的在于基于前述任一种基于金纳米粒子自组装体系的酒精度检测方法提供一种检测装置。Another object of the present invention is to provide a detection device based on any of the aforementioned alcohol content detection methods based on a gold nanoparticle self-assembly system.
具体地,所述检测装置包括一个或多个检测单元,所述一个或多个检测单元包括金纳米粒子和钾盐,且各检测单元中的钾盐的质量不同。Specifically, the detection device includes one or more detection units, the one or more detection units include gold nanoparticles and potassium salts, and the potassium salts in each detection unit have different qualities.
本技术方案中,检测装置包括的一个或多个检测单元即形成了检测方法中的一个或多个检测体系,各检测单元均包括金纳米粒子和钾盐,不同的检测单元中的钾盐质量不同。在使用时,将待检测白酒分别加入至各检测单元中观察检测单元中检测体系的变色情况即可识别待检测白酒的酒精度范围。In this technical solution, one or more detection units included in the detection device form one or more detection systems in the detection method. Each detection unit includes gold nanoparticles and potassium salt. The quality of potassium salt in different detection units different. When in use, add the liquor to be detected into each detection unit respectively and observe the discoloration of the detection system in the detection unit to identify the alcohol content range of the liquor to be detected.
在实际应用中,检测装置有多种设置方式,在部分优选的实施例中,检测装置被设置为测试板的形式。具体地,检测装置包括底板,所述底板上设置有若干容纳腔,所述容纳腔内用于放置检测单元,所述检测单元包括负载有金纳米粒子和钾盐的样品垫。In practical applications, the detection device can be arranged in various ways. In some preferred embodiments, the detection device is arranged in the form of a test board. Specifically, the detection device includes a bottom plate, and several accommodation cavities are provided on the bottom plate. The accommodation cavities are used to place detection units, and the detection units include sample pads loaded with gold nanoparticles and potassium salts.
本技术方案中,检测体系在加入白酒前为固体,携带更加方便。检测装置的底板上设置有一个或多个容纳腔,容纳腔内设置有样品垫。所述样品垫优选采用玻璃纤维素膜,玻璃纤维素膜浸泡于金纳米粒子溶液和钾盐溶液后烘干即可得到负载有金纳米粒子和钾盐的样品垫。In this technical solution, the detection system is solid before adding liquor, making it more convenient to carry. One or more receiving chambers are provided on the bottom plate of the detection device, and a sample pad is provided in the receiving chambers. The sample pad preferably uses a glass cellulose film. The glass cellulose film is soaked in a gold nanoparticle solution and a potassium salt solution and then dried to obtain a sample pad loaded with gold nanoparticles and potassium salt.
使用时,将待检测白酒滴加至各容纳腔中与样品垫上的金纳米粒子和钾盐溶解反应,通过观察样品垫的颜色变化判断待检测白酒的酒精度范围。During use, the liquor to be detected is added dropwise into each chamber to react with the dissolution of gold nanoparticles and potassium salts on the sample pad. The alcohol content range of the liquor to be detected is judged by observing the color change of the sample pad.
在部分优选的实施例中,检测装置包括放置架,所述放置架上设置有若干检测单元,所述检测单元包括离心管,所述离心管内放置有金纳米粒子和钾盐。In some preferred embodiments, the detection device includes a placement rack, and several detection units are provided on the placement rack. The detection units include centrifuge tubes, and gold nanoparticles and potassium salts are placed in the centrifuge tubes.
本技术方案中,检测体系在加入白酒前为液体,检测体系的接触、混匀更加充分。检测装置包括放置架,放置架上设置有一个或多个检测单元,检测单元即为装有金纳米粒子溶液和钾盐溶液的离心管。In this technical solution, the detection system is liquid before adding liquor, and the contact and mixing of the detection system are more complete. The detection device includes a placement rack, and one or more detection units are provided on the placement rack. The detection unit is a centrifuge tube containing gold nanoparticle solution and potassium salt solution.
使用时,将待检测白酒滴加至各离心管内,摇匀后记录检测体系的颜色,依靠一个或多个检测体系来判断待检测白酒的酒精度范围。When in use, dropwise add the liquor to be detected into each centrifuge tube, shake well and record the color of the detection system, and rely on one or more detection systems to determine the alcohol content range of the liquor to be detected.
在部分优选的实施例中,检测装置包括第一板和第二板,所述第一板和第二板共同构成若干用于放置检测单元的腔体,所述检测单元包括检测瓶,所述检测瓶内设置有分隔膜和穿刺件,所述分隔膜一侧用于装载金纳米粒子和钾盐、另一侧用于装载待检测白酒,所述穿刺件用于在第一板和第二板相向移动时刺穿所述分隔膜。In some preferred embodiments, the detection device includes a first plate and a second plate, and the first plate and the second plate together form a plurality of cavities for placing detection units, and the detection units include detection bottles, and the A separation film and a piercing member are provided in the detection bottle. One side of the separation film is used to load gold nanoparticles and potassium salts, and the other side is used to load the liquor to be detected. The piercing member is used to connect the first plate and the second plate. The plates pierce the separating membrane as they move toward each other.
本技术方案中,检测装置包括能够相向移动的第一板和第二板,第一板和第二板上均设置有一一对应的凹槽,当第一板和第二板扣合时,凹槽形成的腔体用于放置各检测单元。In this technical solution, the detection device includes a first plate and a second plate that can move toward each other. Each of the first plate and the second plate is provided with a one-to-one corresponding groove. When the first plate and the second plate are engaged, The cavity formed by the groove is used to place each detection unit.
本技术方案中,检测单元包括检测瓶,检测瓶内设置有分隔膜以将检测瓶的内部空间分为两部分,且两部分均可通过盖体与外部连通。例如,检测瓶的一端为第一盖体,第一盖体与分隔膜之间的内部空间用于放置金纳米粒子和钾盐溶液,检测瓶的另一端为第二盖体,第二盖体与分割膜之间的内部空间用于放置待检测白酒。In this technical solution, the detection unit includes a detection bottle, and a separation film is provided in the detection bottle to divide the internal space of the detection bottle into two parts, and both parts can be connected to the outside through the cover. For example, one end of the detection bottle is a first cover, and the internal space between the first cover and the separation film is used to place gold nanoparticles and potassium salt solution. The other end of the detection bottle is a second cover, and the second cover is The internal space between it and the dividing membrane is used to place the liquor to be detected.
第一盖体和/或第二盖体上设置有穿刺件,穿刺件能够在外力的作用下,例如,可以在第二板的凹槽内设置挤压件来推动穿刺件沿竖直方向移动,进而刺穿分隔膜,使得分隔膜两侧的空间连通,待检测白酒与金纳米粒子、钾盐溶液接触从而显色。The first cover body and/or the second cover body are provided with a piercing piece. The piercing piece can be acted upon by an external force. For example, a pressing piece can be provided in the groove of the second plate to push the piercing piece to move in the vertical direction. , and then pierce the separation film, making the spaces on both sides of the separation film connected, and the liquor to be detected comes into contact with gold nanoparticles and potassium salt solution to develop color.
在使用时,可以先将待检测白酒分别放置于多个检测瓶中,各检测瓶内的钾盐质量不同。在第二板和第一板相向移动的过程中,穿刺件在第二板的作用下刺穿分隔膜,使得分隔膜两侧的物质在同一时间开始接触并逐步显色。利用穿刺件实现的分隔膜同时穿刺,检测体系同时混合能够进一步提高检测结果的准确性。During use, the liquor to be tested can be placed in multiple testing bottles, and the potassium salts in each testing bottle have different qualities. In the process of the second plate and the first plate moving toward each other, the piercing member pierces the separation film under the action of the second plate, so that the substances on both sides of the separation film begin to contact at the same time and gradually develop color. The simultaneous puncture of the separator membrane and the simultaneous mixing of the detection system using the puncture piece can further improve the accuracy of the detection results.
本发明与现有技术相比,具有如下的优点和有益效果:Compared with the prior art, the present invention has the following advantages and beneficial effects:
1、本发明能够根据一份或多份检测体系在加入待检测白酒后所呈现的颜色,快速地识别出白酒的酒精度范围,检测的时间通常在半分钟左右,且其灵敏度高、操作简单、制备成本低,在白酒的市场监管上具有广泛的应用价值;1. The present invention can quickly identify the alcohol content range of liquor based on the color of one or more detection systems after adding the liquor to be detected. The detection time is usually about half a minute, and it has high sensitivity and simple operation. , low preparation cost, and has wide application value in the market supervision of liquor;
2、本发明通过将金纳米粒子与钾盐的摩尔比为0.04~0.02,不仅降低了检测成本,而且有利于提高呈色的差异,进一步提高酒精度范围判断的准确性;2. By setting the molar ratio of gold nanoparticles to potassium salt to 0.04-0.02, the present invention not only reduces the detection cost, but also helps to improve the difference in coloration and further improves the accuracy of judging the alcohol content range;
3、本发明通过设置三份检测体系且三份检测体系中的钾盐的摩尔比为4:5:6,使得检测体系组既能够有效地区分低度、中度和高度白酒,而且无需设置过多的检测体系,提高了检测效率和检测的准确度。3. The present invention sets up three detection systems and the molar ratio of potassium salts in the three detection systems is 4:5:6, so that the detection system group can effectively distinguish low-alcohol, medium-alcohol and high-alcohol liquor without setting up Excessive detection systems improve detection efficiency and detection accuracy.
附图说明Description of the drawings
此处所说明的附图用来提供对本发明实施例的进一步理解,构成本申请的一部分,并不构成对本发明实施例的限定。在附图中:The drawings described here are used to provide a further understanding of the embodiments of the present invention, constitute a part of this application, and do not constitute a limitation to the embodiments of the present invention. In the attached picture:
图1为本发明具体实施例中酒精度检测方法的流程框图;Figure 1 is a flow chart of an alcohol content detection method in a specific embodiment of the present invention;
图2为本发明具体实施例中三组不同的检测体系在加入白酒后的紫外线吸收图,其中横坐标为波长,纵坐标为吸光度;Figure 2 is an ultraviolet absorption diagram of three different groups of detection systems after adding liquor in a specific embodiment of the present invention, in which the abscissa is the wavelength and the ordinate is the absorbance;
图3为本发明具体实施例中一种酒精度检测装置的结构示意图;Figure 3 is a schematic structural diagram of an alcohol content detection device in a specific embodiment of the present invention;
图4为本发明具体实施例中另一种酒精度检测装置的结构示意图;Figure 4 is a schematic structural diagram of another alcohol content detection device in a specific embodiment of the present invention;
图5为本发明具体实施例中又一种酒精度检测装置的结构示意图;Figure 5 is a schematic structural diagram of another alcohol content detection device in a specific embodiment of the present invention;
图6为本发明具体实施例中又一种酒精度检测装置的检测瓶的结构示意图;Figure 6 is a schematic structural diagram of a detection bottle of another alcohol content detection device in a specific embodiment of the present invention;
图7示出了本发明具体实施例中各检测体系在加入不同酒精度的白酒后的显色情况。Figure 7 shows the color development of each detection system after adding liquor with different alcohol contents in the specific embodiment of the present invention.
附图中标记及对应的零部件名称:Marks and corresponding parts names in the attached drawings:
11-底板,12-容纳腔,13-样品垫,14-短柱,21-放置架,22-离心管,31-第一板,32-第二板,33-挤压件,4-检测瓶,41-瓶体,42-第一盖体,43-第二盖体,44-移动件,45-滑块,46-弹簧,47-穿刺件,48-分隔膜。11-Bottom plate, 12-Accommodating chamber, 13-Sample pad, 14-Short column, 21-Placement rack, 22-Centrifuge tube, 31-First plate, 32-Second plate, 33-Extrusion piece, 4-Detection Bottle, 41-bottle body, 42-first cover body, 43-second cover body, 44-moving part, 45-slider, 46-spring, 47-piercing part, 48-separating film.
具体实施方式Detailed ways
为使本发明的目的、技术方案和优点更加清楚明白,下面结合实施例和附图,对本发明作进一步的详细说明,本发明的示意性实施方式及其说明仅用于解释本发明,并不作为对本发明的限定。In order to make the purpose, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the examples and drawings. The schematic embodiments of the present invention and their descriptions are only used to explain the present invention and do not as a limitation of the invention.
本发明所有原料,对其来源没有特别限制,在市场上购买的或按照本领域技术人员熟知的常规方法即可制备。All raw materials of the present invention have no particular restrictions on their sources. They can be purchased in the market or prepared according to conventional methods well known to those skilled in the art.
本发明所有原料,对其纯度没有特别限制,本发明优选采用分析纯或酒精度检测领域常规的纯度要求。All raw materials in the present invention have no special restrictions on their purity. The present invention preferably adopts analytical purity or conventional purity requirements in the field of alcohol content detection.
本发明所有原料,其牌号和简称均属于本领域常规牌号和简称,每个牌号和简称在其相关用途的领域内均是清楚明确的,本领域技术人员根据牌号、简称以及相应的用途,能够从市售中购买得到或者通过常规方法制备得到。All raw materials of the present invention, their brands and abbreviations are conventional brands and abbreviations in this field. Each brand and abbreviation are clear and unambiguous in the field of its relevant use. Those skilled in the art can according to the brand names, abbreviations and corresponding uses. It is purchased from the market or prepared by conventional methods.
实施例1:Example 1:
如图1所示的基于金纳米粒子自组装体系的酒精度检测方法,包括以下步骤:The alcohol content detection method based on the gold nanoparticle self-assembly system shown in Figure 1 includes the following steps:
将待检测白酒分别加入至若干份检测体系中,所述若干份检测体系中的各份检测体系均包括金纳米粒子和钾盐,且各份检测体系中的钾盐的质量不同;The liquor to be detected is added to several detection systems respectively, each detection system in the several detection systems includes gold nanoparticles and potassium salt, and the potassium salt in each detection system has different qualities;
待检测白酒与检测体系接触后,基于若干份检测体系的颜色变化,判断待检测白酒的酒精度;After the liquor to be tested comes into contact with the detection system, the alcohol content of the liquor to be detected is determined based on the color changes of several portions of the detection system;
其中,所述金纳米粒子采用柠檬酸还原法合成。Wherein, the gold nanoparticles are synthesized by citric acid reduction method.
本技术方案中,如图2所示,520nm左右有一个尖锐的吸收峰,该峰为单个金纳米粒子的紫外吸收峰,当金纳米粒子开始出现一维线性组装时,会在650~700nm出现组装峰,组装峰的波长越小说明链越短。由此可见,对于38度的白酒,随着硝酸钾加入的含量增加,处于组装态的金纳米粒子的数量则会增加,检测体系则相应地呈现出红色(80μL硝酸钾)、紫色(100μL硝酸钾)和蓝色(120μL硝酸钾),从而实现快速地根据检测体系的颜色差异判断待检测白酒的酒精度范围。In this technical solution, as shown in Figure 2, there is a sharp absorption peak around 520nm. This peak is the ultraviolet absorption peak of a single gold nanoparticle. When the gold nanoparticles begin to appear in one-dimensional linear assembly, they will appear at 650-700nm. Assembly peak, the smaller the wavelength of the assembly peak, the shorter the chain. It can be seen that for 38-degree liquor, as the content of potassium nitrate added increases, the number of gold nanoparticles in the assembled state will increase, and the detection system will accordingly show red (80 μL potassium nitrate), purple (100 μL nitric acid Potassium) and blue (120μL potassium nitrate), thereby enabling the rapid determination of the alcohol content range of the liquor to be detected based on the color difference of the detection system.
在部分实施例中,可以采用一份检测体系进行判断,例如可以通过300μL金纳米粒子、80μL硝酸钾、浓度为0.5mol/L的检测体系,在加入白酒后是否呈现红色来判断其是否为低度白酒,是否呈现紫色来判断其是否为中度白酒,以及是否呈现蓝色来判断其是否为高度白酒。在一个或多个实施例中,可以通过设置比色卡,来更准确地判断白酒的酒精度。In some embodiments, a detection system can be used for judgment. For example, a detection system of 300 μL gold nanoparticles, 80 μL potassium nitrate, and a concentration of 0.5 mol/L can be used to determine whether it is low after adding white wine. For liquor with a high strength, whether it appears purple will determine whether it is a medium-strength liquor, and whether it will appear blue will determine whether it is a high-strength liquor. In one or more embodiments, the alcohol content of liquor can be judged more accurately by setting a color comparison card.
在部分实施例中,可以采用多份检测体系相结合来进一步提高判断的准确性。例如,可以设置三份检测体系,检测体系组能够呈现出红-紫-蓝,紫-蓝-蓝,蓝-蓝-蓝的区分,从而允许检测人员能够快速、高效地对当前白酒酒精度数做出判断。In some embodiments, multiple detection systems can be combined to further improve the accuracy of judgment. For example, three detection systems can be set up. The detection system group can show the distinction of red-purple-blue, purple-blue-blue, and blue-blue-blue, allowing the inspector to quickly and efficiently determine the alcohol content of the current liquor. make judgments.
在部分优选的实施例中,所述金纳米粒子与钾盐的摩尔比为0.04~0.02,优选地,金纳米粒子与钾盐的摩尔比为0.0375~0.025。In some preferred embodiments, the molar ratio of the gold nanoparticles to the potassium salt is 0.04-0.02. Preferably, the molar ratio of the gold nanoparticles to the potassium salt is 0.0375-0.025.
在部分实施例中,所述若干份检测体系中,钾盐质量最大的检测体系与钾盐质量最小的检测体系的钾盐的摩尔比为1.2~2.0。In some embodiments, among the several detection systems, the molar ratio of potassium salts in the detection system with the largest potassium salt mass and the detection system with the smallest potassium salt mass is 1.2 to 2.0.
在部分实施例中,述若干份检测体系包括三份检测体系,所述三份检测体系中的钾盐的摩尔比为4:5:6。例如,在浓度为0.5mol/L的检测体系中,三份检测体系的钾盐分别为80μL、100μL和120μL。该检测体系组既能够有效地区分低度、中度和高度白酒,而且无需设置过多的检测体系,提高了检测效率和检测的准确度。In some embodiments, the plurality of detection systems include three detection systems, and the molar ratio of potassium salts in the three detection systems is 4:5:6. For example, in a detection system with a concentration of 0.5 mol/L, the potassium salts of the three detection systems are 80 μL, 100 μL, and 120 μL respectively. This detection system set can effectively distinguish low-alcohol, medium-alcohol and high-alcohol liquor without setting up too many detection systems, improving detection efficiency and accuracy.
在部分实施例中,待检测白酒与检测体系接触后120秒内,基于若干份检测体系的颜色变化判断待检测白酒的酒精度。优选地,检测在60秒内完成。In some embodiments, within 120 seconds after the liquor to be detected comes into contact with the detection system, the alcohol content of the liquor to be detected is determined based on the color changes of several portions of the detection system. Preferably, detection is completed within 60 seconds.
在一个或多个实施例中,加入至每份检测体系中的待检测白酒的体积为0.05~4.00mL。In one or more embodiments, the volume of the liquor to be detected added to each detection system is 0.05-4.00 mL.
本实施例中,能够根据一份或多份检测体系在加入待检测白酒后所呈现的颜色,快速地识别出白酒的酒精度范围,检测的时间通常在半分钟左右,且其灵敏度高、操作简单、制备成本低,在白酒的市场监管上具有广泛的应用价值。In this embodiment, the alcohol content range of the liquor can be quickly identified based on the color of one or more detection systems after adding the liquor to be detected. The detection time is usually about half a minute, and its sensitivity is high and the operation is It is simple, has low preparation cost and has wide application value in the market supervision of liquor.
实施例2:Example 2:
在实施例1的基础上,如图3所示的基于金纳米粒子自组装体系的酒精度检测装置,包括三个检测单元,所述三检测单元均包括金纳米粒子和钾盐,且各检测单元中的钾盐的质量不同;检测装置包括底板11,所述底板11上设置有若干容纳腔12,所述容纳腔12内用于放置检测单元,所述检测单元包括负载有金纳米粒子和钾盐的样品垫13。On the basis of Example 1, the alcohol content detection device based on the self-assembly system of gold nanoparticles as shown in Figure 3 includes three detection units. The three detection units all include gold nanoparticles and potassium salt, and each detection unit The quality of the potassium salt in the unit is different; the detection device includes a bottom plate 11, which is provided with a number of accommodation chambers 12. The accommodation chambers 12 are used to place detection units. The detection units include gold nanoparticles loaded and Potassium salt sample pad 13.
使用时,将待检测白酒滴加至各容纳腔中与样品垫上的金纳米粒子和钾盐溶解反应,通过观察样品垫的颜色变化判断待检测白酒的酒精度范围。During use, the liquor to be detected is added dropwise into each chamber to react with the dissolution of gold nanoparticles and potassium salts on the sample pad. The alcohol content range of the liquor to be detected is judged by observing the color change of the sample pad.
在一个或多个实施例中,如图3所示,在容纳腔内还设置有若干支撑于样品垫下方的短柱,以使得样品垫下方具有足够的空间以容纳部分待检测白酒,不仅避免滴入白酒后溢出或溅射出容纳腔,允许白酒同检测体系充分接触,提高显色效果。In one or more embodiments, as shown in Figure 3, a number of short columns supported below the sample pad are also provided in the accommodation cavity, so that there is enough space below the sample pad to accommodate part of the liquor to be detected, which not only avoids After the liquor is dripped, it overflows or splashes out of the containing cavity, allowing the liquor to fully contact the detection system and improving the color development effect.
在部分优选的实施例中,还包括待检测白酒的滴加单元,滴加单元可以采用滴管、移液管等设备,尽量确保各检测单元中的白酒加入量相同,以提高结果的准确性。In some preferred embodiments, a dripping unit for the liquor to be detected is also included. The dripping unit can use droppers, pipettes and other equipment to ensure that the amount of liquor added in each detection unit is the same to improve the accuracy of the results. .
在部分优选的实施例中,还包括计时单元,所述计时单元用于提示在指定时间内完成对比。In some preferred embodiments, a timing unit is further included, and the timing unit is used to prompt that the comparison is completed within a specified time.
在部分优选的实施例中,还包括采集单元,所述采集单元用于采集检测结果的图片,用于后续的数据存储、比对。In some preferred embodiments, it also includes a collection unit, which is used to collect pictures of the detection results for subsequent data storage and comparison.
在部分实施例中,检测单元可以是一个或两个,也可以是四个以上,在一个或多个实施例中,可以以一个或多个检测单元作为一组,设置多组检测单元。In some embodiments, the number of detection units may be one or two, or there may be more than four. In one or more embodiments, one or more detection units may be used as a group, and multiple groups of detection units may be provided.
实施例3:Example 3:
在上述实施例的基础上,如图4所示的基于金纳米粒子自组装体系的酒精度检测装置,包括放置架21,所述放置架21上设置有三个检测单元,所述检测单元包括离心管22,所述离心管22内放置有金纳米粒子和钾盐。On the basis of the above embodiments, the alcohol content detection device based on the self-assembly system of gold nanoparticles as shown in Figure 4 includes a placement rack 21, and three detection units are provided on the placement rack 21. The detection unit includes a centrifugal Tube 22, gold nanoparticles and potassium salt are placed in the centrifuge tube 22.
使用时,将待检测白酒滴加至各离心管内,摇匀后记录检测体系的颜色,依靠一个或多个检测体系来判断待检测白酒的酒精度范围。When in use, dropwise add the liquor to be detected into each centrifuge tube, shake well and record the color of the detection system, and rely on one or more detection systems to determine the alcohol content range of the liquor to be detected.
在部分实施例中,检测单元可以是一个或两个,也可以是四个以上,在一个或多个实施例中,可以以一个或多个检测单元作为一组,设置多组检测单元。In some embodiments, the number of detection units may be one or two, or there may be more than four. In one or more embodiments, one or more detection units may be used as a group, and multiple groups of detection units may be provided.
实施例4:Example 4:
在上述实施例的基础上,如图5和图6所示的基于金纳米粒子自组装体系的酒精度检测装置,包括第一板31和第二板32,所述第一板31和第二板32共同构成三个用于放置检测单元的腔体,所述检测单元包括检测瓶4,所述检测瓶4内设置有分隔膜48和穿刺件47,所述分隔膜48一侧用于装载金纳米粒子和钾盐、另一侧用于装载待检测白酒,所述穿刺件47用于在第一板31和第二板32相向移动时刺穿所述分隔膜48。Based on the above embodiments, the alcohol content detection device based on the self-assembly system of gold nanoparticles as shown in Figures 5 and 6 includes a first plate 31 and a second plate 32. The plates 32 together constitute three cavities for placing detection units. The detection units include a detection bottle 4. A separation film 48 and a puncture member 47 are provided inside the detection bottle 4. One side of the separation film 48 is used for loading. Gold nanoparticles and potassium salt are used to load the liquor to be detected on the other side. The puncture member 47 is used to puncture the separation film 48 when the first plate 31 and the second plate 32 move toward each other.
在使用时,可以先将待检测白酒分别放置于多个检测瓶中,各检测瓶内的钾盐质量不同。在第二板和第一板相向移动的过程中,穿刺件在第二板的作用下刺穿分隔膜,使得分隔膜两侧的物质在同一时间开始接触并逐步显色。利用穿刺件实现的分隔膜同时穿刺,检测体系同时混合能够进一步提高检测结果的准确性。During use, the liquor to be tested can be placed in multiple testing bottles, and the potassium salts in each testing bottle have different qualities. In the process of the second plate and the first plate moving toward each other, the piercing member pierces the separation film under the action of the second plate, so that the substances on both sides of the separation film begin to contact at the same time and gradually develop color. The simultaneous puncture of the separator membrane and the simultaneous mixing of the detection system using the puncture piece can further improve the accuracy of the detection results.
在一个或多个实施例中,第一盖体或第二盖体上设置有移动件,所述移动件上连接有滑块45,滑块45位于第一盖体或第二盖体内壁上的滑槽中,因此,移动件能够沿盖体竖直上下移动。在滑块上还设置有弹簧,在未受第二板上的挤压件挤压时,移动件在弹簧的作用下保持初始位置,穿刺件未刺穿分隔膜,当第二板的挤压件挤压移动件时,移动件克服弹簧的作用力移动,从而使得穿刺件穿刺分隔膜。当挤压件不再继续向移动件施加挤压力后,移动件在弹簧的作用下复位,穿刺件从分隔膜上形成的穿刺孔中移除,有利于分隔膜两侧的液体充分接触。In one or more embodiments, a moving part is provided on the first cover or the second cover, and a slider 45 is connected to the moving part. The slider 45 is located on the inner wall of the first cover or the second cover. in the chute, so the moving part can move vertically up and down along the cover. A spring is also provided on the slider. When it is not squeezed by the extrusion part on the second plate, the moving part maintains its initial position under the action of the spring. The piercing part does not pierce the separation film. When the second plate is extruded When the moving part is pressed by the moving part, the moving part moves against the force of the spring, so that the piercing part pierces the separation film. When the extrusion part no longer continues to exert extrusion force on the moving part, the moving part is reset under the action of the spring, and the puncture part is removed from the puncture hole formed on the separation film, which is conducive to full contact between the liquids on both sides of the separation film.
在部分实施例中,检测单元可以是一个或两个,也可以是四个以上,在一个或多个实施例中,可以以一个或多个检测单元作为一组,设置多组检测单元。In some embodiments, the number of detection units may be one or two, or there may be more than four. In one or more embodiments, one or more detection units may be used as a group, and multiple groups of detection units may be provided.
实施例5:Example 5:
采用实施例3中的检测装置,设置三组检测体系,其中,三组检测体系中金纳米粒子为1.5x 10-6mol,硝酸钾的浓度为0.5mol/L,体积分别为80μL、100μL和120μL,接触时间为15秒。Using the detection device in Example 3, three groups of detection systems were set up, wherein the gold nanoparticles in the three groups of detection systems were 1.5x 10 -6 mol, the concentration of potassium nitrate was 0.5 mol/L, and the volumes were respectively 80 μL, 100 μL and 120μL, contact time is 15 seconds.
如图7所示,在加入38度的白酒后,三组检测体系分别显示出红色(80μL硝酸钾)、紫色(100μL硝酸钾)和蓝色(120μL硝酸钾);在加入56度的白酒后,三组检测体系分别显示出紫色(80μL硝酸钾)、蓝色(100μL硝酸钾)和蓝色(120μL硝酸钾)。在加入68度的白酒后,三组检测体系均呈现出蓝色。由此可见,结合不同检测体系的显色,能够在15秒内判断出待检测白酒的酒精度范围,且其灵敏度高、操作简单,有利于市场监督部门对白酒酒精度进行快速实时检测。As shown in Figure 7, after adding 38-degree white wine, the three detection systems showed red (80 μL potassium nitrate), purple (100 μL potassium nitrate), and blue (120 μL potassium nitrate) respectively; after adding 56-degree white wine , the three groups of detection systems respectively show purple (80μL potassium nitrate), blue (100μL potassium nitrate) and blue (120μL potassium nitrate). After adding 68-degree liquor, all three groups of detection systems showed blue color. It can be seen that by combining the color development of different detection systems, the alcohol content range of the liquor to be detected can be determined within 15 seconds. Its high sensitivity and simple operation are conducive to the rapid real-time detection of liquor alcohol content by market supervision departments.
本文中所使用的“第一”、“第二”等(例如第一板、第二板,第一盖体、第二盖体等)只是为了描述清楚起见而对相应部件进行区别,不旨在限制任何次序或者强调重要性等。此外,在本文中使用的术语“连接”在不进行特别说明的情况下,可以是直接相连,也可以使经由其他部件间接相连。The terms "first", "second", etc. (such as the first plate, the second plate, the first cover, the second cover, etc.) used in this article are only used to distinguish the corresponding components for the sake of clarity of description, and do not intend to In limiting any order or emphasizing importance, etc. In addition, the term "connection" used herein may be a direct connection or an indirect connection through other components unless otherwise specified.
以上所述的具体实施方式,对本发明的目的、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施方式而已,并不用于限定本发明的保护范围,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above-mentioned specific embodiments further describe the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above-mentioned are only specific embodiments of the present invention and are not intended to limit the scope of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.
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