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CN103969258B - A kind of bore hole fast detecting Cd2+Test paper and method - Google Patents

A kind of bore hole fast detecting Cd2+Test paper and method Download PDF

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CN103969258B
CN103969258B CN201410217634.2A CN201410217634A CN103969258B CN 103969258 B CN103969258 B CN 103969258B CN 201410217634 A CN201410217634 A CN 201410217634A CN 103969258 B CN103969258 B CN 103969258B
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test paper
color
nbt
aqueous solution
cadmium
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CN103969258A (en
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温广明
刘斌
双少敏
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Shanxi University
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Abstract

本发明提供了一种裸眼快速检测Cd2+的试纸和方法,是利用量子点在可见光照射下产生光电子使染料变色的原理发明一种新的检测试纸和方法,所制得的试纸成本极低,其能定性或半定量检测食品或水中的镉,测定速度快,灵敏度高。检测方法简单,对操作人员技术要求低,非常适合现场检测。The invention provides a test paper and method for rapid detection of Cd 2+ with the naked eye. It uses the principle that quantum dots generate photoelectrons under the irradiation of visible light to change the color of the dye to invent a new detection test paper and method. The cost of the prepared test paper is extremely low , which can qualitatively or semi-quantitatively detect cadmium in food or water, with fast determination speed and high sensitivity. The detection method is simple and has low technical requirements for operators, which is very suitable for on-site detection.

Description

一种裸眼快速检测Cd2+的试纸和方法A test paper and method for rapid detection of Cd2+ with naked eyes

一、技术领域 1. Technical field

本发明涉及检测重金属离子的试纸和方法,具体是一种裸眼快速检测Cd2+的试纸和方法。 The invention relates to a test paper and a method for detecting heavy metal ions, in particular to a test paper and a method for rapidly detecting Cd2 + with naked eyes.

二、背景技术 2. Background technology

镉是我国重点控制的重金属污染物,属于第一类污染物。除了可造成急、慢性中毒,还有一定的致畸、致癌和致突变作用,其最主要的危害还是在体内蓄积造成的慢性中毒。机体摄入镉的最主要途径是食品,而食品中的镉主要来自环境污染。因此,监测环境中镉的含量,是控制人体镉摄入量,预防和减少镉对人体危害的重要措施。 Cadmium is a heavy metal pollutant under key control in my country and belongs to the first category of pollutants. In addition to causing acute and chronic poisoning, it also has certain teratogenic, carcinogenic and mutagenic effects. The main hazard is chronic poisoning caused by accumulation in the body. The most important way for the body to absorb cadmium is food, and cadmium in food mainly comes from environmental pollution. Therefore, monitoring the content of cadmium in the environment is an important measure to control the intake of cadmium in the human body, prevent and reduce the harm of cadmium to the human body.

镉的检测方法很多,如:分光光度法、原子吸收法、极谱催化波法、单扫描极谱法、溶出伏安法、电位溶出法、电感耦合等离子体发射光谱法、中子活化分析法、质谱法、色谱法、电化学生物传感器法以及各种方法的联用技术等,它们大多需要昂贵的仪器,并且操作复杂,需要专门的技术人员来完成。 There are many detection methods for cadmium, such as: spectrophotometry, atomic absorption method, polarographic catalytic wave method, single-scan polarographic method, stripping voltammetry, potential stripping method, inductively coupled plasma emission spectrometry, neutron activation analysis method , mass spectrometry, chromatography, electrochemical biosensor method, and the combination of various methods, etc., most of them require expensive instruments, and the operation is complicated, requiring specialized technicians to complete.

三、发明内容 3. Contents of the invention

本发明的目的在于提供一种裸眼快速检测Cd2+的试纸和方法,这种试纸和方应能定性或半定量检测食品或水中的镉,不仅可节约大量的人力物力和财力,且试纸携带方便,方法简单,非常适合现场检测。 The purpose of the present invention is to provide a test paper and method for rapid detection of Cd 2+ with naked eyes. This test paper and method should be able to qualitatively or semi-quantitatively detect cadmium in food or water, which can not only save a lot of manpower, material and financial resources, but also can be carried by the test paper. Convenient, simple method, very suitable for on-site detection.

本发明提供的一种裸眼快速检测Cd2+的试纸,通过如下方法制得: A kind of naked-eye rapid detection Cd 2+ test paper provided by the invention is made by the following method:

(1)以0.1MNa2S的乙醇水溶液和0.1M的Zn(Ac)2的乙醇水溶液按体积比1∶1合成ZnS量子点水溶液,所述的乙醇与水的体积比为1∶3;配置浓度为1mg/mL的硝基四氮唑蓝(NBT)水溶液; (1) Synthesize ZnS quantum dot aqueous solution with 0.1M Na 2 S ethanol aqueous solution and 0.1M Zn(Ac) 2 ethanol aqueous solution at a volume ratio of 1:1, and the volume ratio of ethanol to water is 1:3; configuration Concentration is the nitro blue tetrazolium blue (NBT) aqueous solution of 1mg/mL;

(2)将ZnS量子点水溶液涂布于玻璃纤维纸上,将NBT水溶液划刻在条状硝酸纤维膜上,置干; (2) ZnS quantum dot aqueous solution is coated on glass fiber paper, and NBT aqueous solution is scratched on strip nitrocellulose membrane, puts to dry;

(3)将划刻好的硝酸纤维膜、已涂布ZnS量子点的玻璃纤维纸依次粘贴于硬牛皮卡纸上,在玻璃纤维纸下方即卡纸末端粘贴聚酯纤维作为样品垫,之后将粘贴好的卡纸沿垂直于NBT划痕线的纵向方向裁剪成条状试纸,NBT划痕所在位置为指示区。 (3) Paste the scratched nitrocellulose membrane and the glass fiber paper coated with ZnS quantum dots on the hard kraft cardboard successively, and stick the polyester fiber under the glass fiber paper, that is, the end of the cardboard as a sample pad, and then place the The pasted cardboard is cut into strips of test paper along the longitudinal direction perpendicular to the NBT scratch line, and the location of the NBT scratch is the indicator area.

所述的玻璃纤维也可以是聚酯纤维、醋酸纤维、硝酸纤维。 Described glass fiber also can be polyester fiber, acetate fiber, nitrocellulose.

本发明提供的一种裸眼快速检测Cd2+的方法,步骤包括: A kind of naked-eye rapid detection method for Cd provided by the invention, the steps include:

(1)将上述制成的试纸条插入待测液中,虹吸30秒到10分钟,在阳光或其它可见光照射下读取指示区的颜色; (1) Insert the test strip made above into the liquid to be tested, siphon it for 30 seconds to 10 minutes, and read the color of the indicator area under sunlight or other visible light;

(2)根据指示区的颜色判断待测样镉离子的含量:若指示区颜色为深蓝色,表明待测溶液中不含镉离子或含量极微;若指示区颜色为浅蓝,表明镉离子含量在1×10-6M~1×10-4M之间;若颜色为黄色或无色,表明镉离子含量在1×10-4M至1×10-2M之间。 (2) Judging the content of cadmium ions in the sample to be tested according to the color of the indicator area: if the color of the indicator area is dark blue, it indicates that the solution to be tested does not contain cadmium ions or the content is very small; if the color of the indicator area is light blue, it indicates that cadmium ions The content is between 1×10 -6 M~1×10 -4 M; if the color is yellow or colorless, it indicates that the content of cadmium ion is between 1×10 -4 M and 1×10 -2 M.

本发明利用了镉离子对量子点具有特异性破坏作用从而抑制了其光电变色过程而进行测定。所制得的试纸成本极低,测定速度快,灵敏度高。同时操作十分简便,对操作人员技术要求低。适合于环境监测、现场测定等场合中镉离子的检测。 The invention utilizes that cadmium ions have a specific destruction effect on quantum dots so as to inhibit the photoelectric color change process for measurement. The prepared test paper has extremely low cost, high determination speed and high sensitivity. At the same time, the operation is very simple and has low technical requirements for operators. It is suitable for the detection of cadmium ions in environmental monitoring, on-site determination and other occasions.

四、附图说明 4. Description of drawings

图1本发明一种裸眼快速检测Cd2+的试纸结构示意图 Fig. 1 is a kind of naked-eye rapid detection Cd 2+ test paper structure schematic diagram of the present invention

五、具体实施方式 5. Specific implementation

实施例1. Example 1.

(1)以Na2S为硫源合成ZnS量子点。具体操作方法为,分別配制0.1M的Zn(Ac)2和0.1M的Na2S乙醇水溶液各50mL﹝其中水与乙醇体积比為3∶1﹞,用HAc调节Zn(Ac)2.水与乙醇溶液的pH=5。室溫搅拌下将Zn(Ac)2水与乙醇溶液逐滴加入Na2S水与醇溶液中(控制滴速为每分种2mL~3mL),滴毕继续搅拌反应30分种。离心分离,沉淀分別用水和无水乙醇洗涤3次,40℃真空干燥2小时可得ZnS量子点,在4℃条件下储存备用,可储存3个月。 (1) ZnS quantum dots were synthesized using Na 2 S as sulfur source. The specific operation method is to prepare 50 mL each of 0.1M Zn(Ac) 2 and 0.1M Na 2 S ethanol aqueous solution (the volume ratio of water and ethanol is 3:1), and adjust Zn(Ac) 2 with HAc. The pH=5 of the ethanol solution. Add the Zn(Ac) 2 water and ethanol solution dropwise to the Na 2 S water and alcohol solution under stirring at room temperature (control the dropping speed at 2 mL-3 mL per minute), and continue to stir for 30 minutes after the dropping. After centrifugation, the precipitate was washed three times with water and absolute ethanol, and vacuum-dried at 40°C for 2 hours to obtain ZnS quantum dots, which could be stored at 4°C for 3 months.

(2)将NBT粉末配成1mg/mL的水溶液。 (2) Make NBT powder into 1 mg/mL aqueous solution.

(3)将ZnS量子点水溶液涂布于玻璃纤维垫上,将NBT水溶液划刻在硝酸纤维膜上,置干; (3) The ZnS quantum dot aqueous solution is coated on the glass fiber mat, the NBT aqueous solution is scratched on the nitrocellulose membrane, and dried;

(4)将划刻好的硝酸纤维膜、已涂布ZnS量子点的玻璃纤维纸依次粘贴于硬牛皮卡纸上,在玻璃纤维纸下方即卡纸末端粘贴聚酯纤维作为样品垫。之后将粘贴好的卡纸沿垂直于NBT划痕线的纵向方向裁剪成条状试纸。NBT划痕所在位置为指示区(即图1中的指示线)。 (4) Paste the scored nitrocellulose membrane and the glass fiber paper coated with ZnS quantum dots on the hard kraft cardboard in sequence, and stick polyester fiber under the glass fiber paper, that is, the end of the cardboard, as a sample pad. Afterwards, the pasted cardboard was cut into strips of test paper along the longitudinal direction perpendicular to the NBT scratch line. The position where the NBT scratches are located is the indicator area (that is, the indicator line in Figure 1).

将所制得的试纸的样品垫区浸入浓度为1×10-4M的醋酸镉溶液中,虹吸3分钟后放置于日光下照射。光照下指示区颜色为无色,判断镉离子浓度在1×10-4M至1×10-2M之间。 The sample pad area of the prepared test paper was immersed in a cadmium acetate solution with a concentration of 1×10 -4 M, siphoned for 3 minutes, and then placed under sunlight. The color of the indicator area under light is colorless, and it is judged that the concentration of cadmium ions is between 1×10 -4 M and 1×10 -2 M.

实施例2.按实施例1制成试纸,将试纸样品区插入浓度为1×10-5M的配制镉离子溶液中,虹吸3分钟。在灯光下照射,指示线变为浅蓝色,判断镉离子含量在1×10-6M~1×10-4M之间。 Example 2. Prepare test paper according to Example 1, insert the sample area of the test paper into the prepared cadmium ion solution with a concentration of 1×10 −5 M, and siphon for 3 minutes. When illuminated by light, the indicator line turns light blue, and it is judged that the content of cadmium ions is between 1×10 -6 M and 1×10 -4 M.

实施例3 Example 3

(1)配制含有Zn2+、Mg2+、Ca2+、Al3+、SO4 2-、NO3 -、PO4 3-离子浓度各为0.01M的溶液(不含镉离子)一份。 (1) Prepare a solution containing Zn 2+ , Mg 2+ , Ca 2+ , Al 3+ , SO 4 2- , NO 3 - , and PO 4 3- ions at a concentration of 0.01M each (without cadmium ions). .

(2)按实施例1制成试纸,将试纸样品区插入配制好的溶液中,虹吸3分钟。在灯光下照射,指示线变为深蓝色,判断溶液中不含镉离子。 (2) Prepare a test paper according to Example 1, insert the sample area of the test paper into the prepared solution, and siphon for 3 minutes. When illuminated by light, the indicator line turns dark blue, indicating that the solution does not contain cadmium ions.

实施例4.按实施例1制成试纸,将试纸样品区插入自来水样品中,虹吸3分钟。在日光下照射,指示线变为深蓝色,判断此自来水样品中不含镉离子。 Embodiment 4. make test paper according to embodiment 1, insert the test paper sample area in the tap water sample, siphon 3 minutes. When exposed to sunlight, the indicator line turns dark blue, indicating that the tap water sample does not contain cadmium ions.

实施例5.取某工厂附近河水样品,初步判断此河水已被排放的镉污染。按实施例1中步骤1-4制成试纸,将试纸样品区插入被镉污染的河水样品中,虹吸3分钟。在日光下照射,指示区变为浅蓝色,判断此河水样品中镉离子含量在1×10-6M~1×10-4M之间,已被污染。 Embodiment 5. Take a river water sample near a certain factory, and preliminarily judge that the river water has been polluted by cadmium discharged. Test paper was made according to steps 1-4 in Example 1, and the sample area of the test paper was inserted into the river water sample polluted by cadmium, and siphoned for 3 minutes. When illuminated by sunlight, the indicator area turns light blue. It is judged that the cadmium ion content in the river water sample is between 1×10 -6 M and 1×10 -4 M, which means it has been polluted.

实施例6.按实施例1制成试纸,将试纸样品区插入不知是否被污染的河水样品中,虹吸5分钟。在日光下照射,指示线变为深蓝色,判断此河水样品中不含镉离子,未被污染。 Embodiment 6. make test paper by embodiment 1, the test paper sample area is inserted in the river water sample that does not know whether to be polluted, siphon 5 minutes. When exposed to sunlight, the indicator line turns dark blue, indicating that the river water sample does not contain cadmium ions and is not polluted.

实验证明本发明镉离子检测试纸及方法测定速度快,选择性强,灵敏可靠。与传统方法相比,降低了检测成本,提高了检测效率,非常适用于实际样品的快速测定。 Experiments have proved that the cadmium ion detection test paper and the method of the present invention have fast determination speed, strong selectivity, sensitivity and reliability. Compared with the traditional method, the detection cost is reduced, the detection efficiency is improved, and it is very suitable for the rapid determination of actual samples.

Claims (3)

1.一种裸眼快速检测Cd2+的试纸,其特征在于,通过如下步骤的方法制得: 1. a kind of naked-eye rapid detection Cd 2+ test paper, it is characterized in that, make by the method for following steps: (1)以0.1MNa2S的乙醇水溶液和0.1M的Zn(Ac)2的乙醇水溶液按体积比1∶1合成ZnS量子点溶液,所述的乙醇与水的体积比为1∶3;配置浓度为1mg/mL的NBT水溶液; (1) Synthesize ZnS quantum dot solution with 0.1M Na 2 S ethanol aqueous solution and 0.1M Zn(Ac) 2 ethanol aqueous solution at a volume ratio of 1:1, and the volume ratio of ethanol and water is 1:3; configuration NBT aqueous solution with a concentration of 1 mg/mL; (2)将ZnS量子点溶液涂布于玻璃纤维纸上,将NBT水溶液划刻在条状硝酸纤维膜上,置干; (2) the ZnS quantum dot solution is coated on the glass fiber paper, the NBT aqueous solution is scratched on the strip nitrocellulose membrane, and dried; (3)将划刻好的硝酸纤维膜、已涂布ZnS量子点的玻璃纤维纸依次粘贴于硬牛皮卡纸上,在玻璃纤维纸下方即卡纸末端粘贴聚酯纤维作为样品垫,之后将粘贴好的卡纸沿垂直于NBT划痕线的纵向方向裁剪成条状试纸,NBT划痕所在位置为指示线。 (3) Paste the scratched nitrocellulose membrane and the glass fiber paper coated with ZnS quantum dots on the hard kraft cardboard successively, and stick the polyester fiber under the glass fiber paper, that is, the end of the cardboard as a sample pad, and then place the The pasted cardboard is cut into strips of test paper along the longitudinal direction perpendicular to the NBT scratch line, and the position of the NBT scratch is the indicator line. 2.如权利要求1所述的一种裸眼快速检测Cd2+的试纸,其特征在于,所述的玻璃纤维用聚酯纤维、醋酸纤维或硝酸纤维替代。 2. the test paper of a kind of naked eye rapid detection Cd 2+ as claimed in claim 1, is characterized in that, described glass fiber is replaced with polyester fiber, acetate fiber or nitrocellulose. 3.一种裸眼快速检测Cd2+的方法,其特征在于,步骤包括: 3. A method for naked-eye rapid detection of Cd 2+ , characterized in that the steps comprise: (1)将上述权利要求1或2所述的试纸条插入待测液中,虹吸30秒到10分钟,在阳光或其它可见光照射下读取指示区的颜色; (1) Insert the test strip described in claim 1 or 2 into the liquid to be tested, siphon it for 30 seconds to 10 minutes, and read the color of the indicator area under sunlight or other visible light irradiation; (2)根据指示区的颜色判断待测样镉离子的含量:若指示区颜色为深蓝色,表明待测溶液中不含镉离子或含量极微;若指示区颜色为浅蓝,表明镉离子含量在1×10-6M~1×10-4M之间;若颜色为黄色或无色,表明镉离子含量在1×10-4M至1×10-2M之间。 (2) Judging the content of cadmium ions in the sample to be tested according to the color of the indicator area: if the color of the indicator area is dark blue, it indicates that the solution to be tested does not contain cadmium ions or the content is very small; if the color of the indicator area is light blue, it indicates that cadmium ions The content is between 1×10 -6 M~1×10 -4 M; if the color is yellow or colorless, it indicates that the content of cadmium ion is between 1×10 -4 M and 1×10 -2 M.
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