CN108195832B - Method for detecting inorganic arsenic content in water and detection kit - Google Patents
Method for detecting inorganic arsenic content in water and detection kit Download PDFInfo
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Abstract
The invention discloses a method for detecting inorganic arsenic content in water, which comprises the following steps of measuring a gold colloid solution and a rhodamine B solution, adding the gold colloid solution and the rhodamine B solution into an inorganic arsenic standard solution, uniformly mixing and standing, adding a sodium borohydride solution, uniformly mixing and reacting for 1min in a dark place, comparing an obtained system with a standard color gradation to determine the color gradation of the inorganic arsenic standard solution after reaction, and comparing the color of a water solution to be detected after reaction with the color gradation of the inorganic arsenic standard solution to obtain the concentration or concentration range of the inorganic arsenic in the water solution to be detected.
Description
Technical Field
The invention relates to inorganic arsenic detection, in particular to a method for visually detecting inorganic arsenic content in water and a detection kit.
Background
The invention relates to a method for detecting inorganic arsenic in drinking water by using inorganic acetylcholinesterase reaction, which is characterized in that water is a source of life, the safety of water affects various fields of society, and arsenic is taken as a toxic element, particularly, the water quality safety is threatened by the form of inorganic arsenic with the highest toxicity, the Chinese national standard GB 5749 provides that the limit of arsenic in drinking water is 10ng/m L, the most common method for detecting arsenic in water at present is an atomic fluorescence method and an inductively coupled plasma mass spectrometry used in the Chinese national standard GB/T5750.6-2006, meanwhile, the traditional diethylamino dithio-formic acid silver spectrophotometry, a zinc-sulfuric acid system new silver salt spectrophotometry and an arsenic spot method are gradually eliminated due to obvious defects, the methods are laboratory detection methods, and a quick detection method for detecting low-content inorganic arsenic in water is only reported at home and abroad, the document retrieval of the prior art finds that the invention, such as Chinese patent Z L02146437.5, the invention, namely an inorganic arsenic esterase reaction detection device in drinking water based on enzyme inhibition reaction, has the detection limit of inorganic arsenic in water, the detection limit of 20ng L, and the invention has significance for detecting the national standard for detecting inorganic arsenic in drinking water with no more, and the practical popularization value of the national standard 5749.
As arsenic in water is mainly inorganic arsenic, the determination of inorganic arsenic in water can represent total arsenic in water. In addition, even if the water contains part of organic arsenic, the organic arsenic dissolved in the water generated by natural biological metabolism has low toxicity and is negligible compared with inorganic arsenic.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problem of low detection limit in the existing inorganic arsenic rapid detection method, the invention provides a method for detecting the content of inorganic arsenic in water, and the invention further aims to provide a kit for detecting the content of inorganic arsenic in an aqueous solution.
The technical scheme is as follows: the invention relates to a method for detecting inorganic arsenic content in water, which comprises the following steps:
(1) sequentially measuring a gold colloid solution and a rhodamine B solution, adding the gold colloid solution and the rhodamine B solution into an inorganic arsenic standard solution, uniformly mixing and standing; then adding a sodium borohydride solution, uniformly mixing, and reacting for 1-5 min in a dark place;
(2) comparing the system obtained in the step (1) with a standard color level, and determining the color level after the inorganic arsenic standard solution reacts;
(3) and (3) replacing the inorganic arsenic standard solution with the aqueous solution to be detected, repeating the step (1), and comparing the color of the aqueous solution to be detected after reaction with the color gradation of the inorganic arsenic standard solution after reaction to obtain the concentration or concentration range of the inorganic arsenic in the aqueous solution to be detected.
The principle of the invention for measuring inorganic arsenic in water is as follows: rhodamine B is catalyzed on the surface of the gold colloid, the rhodamine B is reduced on the surface of the gold colloid after sodium borohydride is added, at the moment, the color of the solution is changed from red to colorless, but inorganic arsenic (including arsenite radical and arsenate radical) can inhibit the occurrence of the catalytic reaction, the inhibition degree is related to the concentration of the inorganic arsenic, the catalytic reaction cannot be carried out as the concentration of the inorganic arsenic is higher, and the color of the solution is redder.
The inorganic arsenic standard solution in the step (1) is a standard solution containing arsenite ions and/or arsenate ions, namely the standard solution containing the arsenite ions, which is obtained by dissolving sodium arsenite powder in a 10% (w/w) sodium hydroxide aqueous solution, or a standard solution containing the arsenite ions and the arsenate ions, which is obtained by dissolving sodium arsenite powder and sodium arsenate in a 10% (w/w) sodium hydroxide aqueous solution, wherein the color order results of the standard solutions of the arsenite ions and the arsenate ions after reaction are consistent.
The gold colloid solution in the step (1) is prepared by adding 0.5-1 m L trisodium citrate aqueous solution with the mass fraction of 1% into a 50m L boiling 0.01% chloroauric acid aqueous solution, boiling for 10-15 min, concentrating the mixed solution by 10-20 times by adopting a high-speed centrifugation method to obtain the gold colloid solution, wherein the concentration of the gold colloid solution is 25-50 nmol/L, the average diameter of gold particles in the gold colloid solution is 20-60 nm, and the high-speed centrifugation method comprises the following steps of measuring 1m L gold colloid solution by using a 1.5m L centrifugal tube, balancing by a balance, centrifuging for 10min at 10000rpm, discarding 900-950 mu L supernatant, and resuspending bottom precipitation.
The concentration of the rhodamine B aqueous solution in the step (1) is 0.5 mmol/L-5 mmol/L, and the concentration of the sodium borohydride aqueous solution is 5 mmol/L-20 mmol/L.
Preferably, the volume of the standard solution in the step (1) is 200 mu L, the concentration of the rhodamine B solution is 1 mmol/L, the volume of the rhodamine B solution is 5 mu L, the volume of the gold colloid solution is 5 mu L, the mixture is uniformly mixed and stands for 1min, the concentration of the sodium borohydride solution is 10 mmol/L, the volume of the sodium borohydride solution is 25 mu L, and the mixture is reacted for 1min in a dark place.
And (4) in the step (3), the aqueous solution to be detected is drinking water, surface water or shallow groundwater.
The kit comprises an inorganic arsenic standard solution with the arsenic concentration of 0-200 ng/m L, a 50 nmol/L concentrated gold colloid solution, a 1 mmol/L rhodamine B solution, a 10 mmol/L sodium borohydride solution and a standard color gradation diagram.
The method for visually and rapidly detecting the inorganic arsenic in the water has the advantages of simple operation, low cost, strong anti-interference capability and the like, can visually detect the inorganic arsenic more than 0.5ng/m L in the water, is far lower than the limit of arsenic in drinking water of 10ng/m L specified in GB 5749 and 2006, and can be used for field rapid detection.
Drawings
FIG. 1 is a Zeta potential diagram of gold colloid solution with different concentrations of inorganic arsenic, in which the concentration unit ppb is ng/m L;
FIG. 2 is a graph of the mean particle size of gold colloid solution and inorganic arsenic of various concentrations, in ppb as ng/m L;
FIG. 3 is a schematic diagram showing the states of components in a mixed solution of gold colloid particles, inorganic arsenic and rhodamine B;
FIG. 4 is a color scale obtained by reacting 0ng/m L-200 ng/m L inorganic arsenic standard solution;
FIG. 5 is a graph showing the effect of interfering ions on the determination of inorganic arsenic in an aqueous solution;
FIG. 6 is a comparison graph of the color levels of the sample in example 4, wherein the first row shows the color levels of the inorganic arsenic standard solution after reaction, and the second row shows the color levels of the solution to be measured after reaction;
FIG. 7 is a comparison graph of the color levels of the inorganic arsenic standard solution after reaction and the second color level of the solution to be measured after reaction in example 5;
FIG. 8 is a comparison graph of the color levels of the sample in example 6, wherein the first row is the color level of the inorganic arsenic standard solution after reaction, and the second row is the color level of the solution to be measured after reaction.
Detailed Description
Example 1
(1) Preparing arsenite standard solutions (the concentrations are 0ng/m L, 0.5ng/m L, 1ng/m L, 2ng/m L, 10ng/m L, 50ng/m L, 100ng/m L and 200ng/m L respectively), and measuring 200 mu L standard solutions respectively and adding the standard solutions into a porous colorimetric plate;
(2) sequentially measuring 5 mu L concentrated gold colloid solution and 5 mu L1 mmol/L rhodamine B solution, respectively adding the concentrated gold colloid solution and the rhodamine B solution into the system obtained in the step (1), uniformly mixing and standing for 1 min;
the preparation method of the concentrated gold colloid solution comprises adding 1m L mass percent of trisodium citrate aqueous solution into 50m L boiling 0.01 mass percent of chloroauric acid aqueous solution, boiling for 10min to obtain wine red gold colloid solution, and concentrating the gold colloid solution by high speed centrifugation for 20 times;
(3) weighing 25 mu L10 mmol/L sodium borohydride solution, respectively adding the sodium borohydride solution into the system obtained in the step (2), uniformly mixing, and reacting for 1min in a dark place;
(4) and (4) respectively comparing the systems obtained in the step (3) with standard color levels to determine the color levels of the inorganic arsenic standard solution after reaction, wherein the result is shown in figure 4, and the inorganic arsenic with the concentration of 0.5ng/m L in water has obvious catalytic inhibition effect and can be visually checked.
The inorganic arsenic in the water sample in the step (2) significantly changes the Zeta potential on the surface of the gold colloid and the particle size of the gold colloid, and the dynamic light scattering (DS L) results are respectively shown in fig. 1 and fig. 2. the trends in fig. 1 and fig. 2 show that the higher the content of the inorganic arsenic, the more negative the Zeta potential on the surface of the gold colloid, and the smaller the particle size of the gold particle, the particle size obtained by DS L is not the physical particle size of the gold particle, but the physical particle size of the gold particle + the thickness of the hydrated layer.
Example 2
The method is the same as example 1, except that in step (1), the standard solutions of arsenate (the concentrations are 0ng/m L, 0.5ng/m L, 1ng/m L, 2ng/m L, 10ng/m L, 50ng/m L, 100ng/m L and 200ng/m L respectively) are adopted, and the color gradation results after the reaction of the standard solutions of arsenite ions and arsenate ions are consistent.
Example 3
The procedure is as in example 1, except that 1000ng/m L K are used respectively+、Na+、Li+、Fe2+、Mg2+、Ca2+、Fe3+、Al3 +、F-、Cl-、SO42-Replace inorganic arsenic (arsenite or arsenate) to carry out interference experimentAs shown in fig. 5, the analysis showed that these common anions and cations did not interfere with the determination of inorganic arsenic.
Example 4
Taking 200 mu L of municipal tap water from Nanjing city from the tail end of a pipe network, adding 5 mu L of concentrated gold colloid and 5 mu L of 1 mmol/L rhodamine B solution, uniformly mixing, standing for 1min, adding 25 mu L of 10 mmol/L sodium borohydride solution, uniformly mixing, placing the mixture in a dark place for reaction for 1min, and carrying out visual observation to find that the solution is nearly colorless, so that the inorganic arsenic content in the water sample is less than 0.5ng/m L.
Example 5
The determination of inorganic arsenic in surface water, namely taking 1 part of Yangtze river water, and carrying out early purification treatment due to the fact that more organic matters and solid particles in the Yangtze river water are needed, wherein the purification treatment process is that 10m L of the Yangtze river water is taken, after centrifugation, 5m L of supernatant is taken, the 5m L of clear water is filtered through a carbon 18 columella to absorb the organic matters in the clear water, 5m L of purified water is obtained, inorganic arsenic is not lost in the purification process, the purified water is detected according to the determination step of the inorganic arsenic in tap water in the embodiment 3, the result is compared with the color gradation of the image 4, the inorganic arsenic concentration of the water sample is 2ng/m L-10 ng/m L but is closer to 2ng/m L, ICP-MS is used for verifying the arsenic content in the water sample to be 3.1ng/m L, and after simple pretreatment, the method used by the invention can realize the visual rapid detection of the inorganic arsenic in the surface water.
Example 6
The determination of inorganic arsenic in shallow groundwater comprises the steps of taking 1 part of rural household well water in Jiangning district of Nanjing, carrying out pretreatment the well water in the same way as in example 4, detecting the inorganic arsenic by the method of example 3, comparing the result with the color gradation shown in figure 4 to obtain that the inorganic arsenic content in the water sample is between 1ng/m L and 2ng/m L, verifying the water sample by ICP-MS to determine the arsenic content to be 1.2ng/m L, and showing that after simple pretreatment, the method can realize visual rapid detection of the inorganic arsenic in the shallow groundwater.
Claims (8)
1. A method for detecting the content of inorganic arsenic in water is characterized by comprising the following steps:
(1) sequentially measuring a gold colloid solution and a rhodamine B solution, adding the gold colloid solution and the rhodamine B solution into an inorganic arsenic standard solution, uniformly mixing and standing; then adding a sodium borohydride solution, uniformly mixing, and reacting for 1-5 min in a dark place;
(2) comparing the system obtained in the step (1) with a standard color level, and determining the color level after the inorganic arsenic standard solution reacts;
(3) replacing the inorganic arsenic standard solution with the aqueous solution to be detected, repeating the step (1), and comparing the color of the aqueous solution to be detected after reaction with the color gradation of the inorganic arsenic standard solution after reaction to obtain the concentration or concentration range of the inorganic arsenic in the aqueous solution to be detected;
in the step (1), the concentration of the gold colloid solution is 25-50 nmol/L, the concentration of the rhodamine B solution is 0.5-5 mmol/L, and the concentration of the sodium borohydride solution is 5-20 mmol/L;
in the step (1), the volume of the standard solution is 200 mu L, the volumes of the gold colloid solution and the rhodamine B solution are 5 mu L respectively, and the volume of the sodium borohydride solution is 25 mu L.
2. The method of claim 1, wherein the inorganic arsenic standard solution in step (1) is a standard solution containing arsenite ions and/or arsenate ions.
3. The method according to claim 1, wherein the concentration of arsenic in the inorganic arsenic standard solution in the step (1) is 0-200 ng/m L.
4. The method of claim 3, wherein the concentration of arsenic in the standard inorganic arsenic solution in step (1) is 0ng/m L, 0.5ng/m L, 1ng/m L, 2ng/m L, 10ng/m L, 50ng/m L, 100ng/m L, or 200ng/m L.
5. The method of claim 1, wherein the gold sol solution in step (1) is prepared by the steps of: adding a trisodium citrate aqueous solution with the mass fraction of 1% into a boiling chloroauric acid aqueous solution with the mass fraction of 0.01%, boiling for 10-15 min, and concentrating the mixed solution by a high-speed centrifugation method for 10-20 times to obtain a gold colloid solution; the average diameter of gold particles in the gold colloid solution is 20-60 nm.
6. The method according to claim 1, wherein the gold colloid solution and the rhodamine B solution are uniformly mixed and left standing for 1-5 min in the step (1).
7. The method according to claim 1, wherein the aqueous solution to be tested in step (3) is drinking water, surface water or shallow groundwater.
8. A kit for detecting the content of inorganic arsenic in an aqueous solution is characterized by comprising an inorganic arsenic standard solution with the arsenic concentration of 0-200 ng/m L, a 50 nmol/L concentrated gold colloid solution, a 1 mmol/L rhodamine B solution, a 10 mmol/L sodium borohydride solution and a standard color gradation diagram.
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| CN1415967A (en) * | 2002-11-07 | 2003-05-07 | 中国科学院生态环境研究中心 | Device for detecting inorganic arsenic in drinking water based on enzyme inhibition reaction |
| CN102262087B (en) * | 2011-04-27 | 2013-01-16 | 杭州慕迪科技有限公司 | On-line monitoring device for total arsenic in water quality |
| CN103163127B (en) * | 2013-03-06 | 2014-12-31 | 上海交通大学 | Method for detecting trivalent arsenic by protoheme horseradish peroxidase catalytic colorimetry |
| CN103499575A (en) * | 2013-10-14 | 2014-01-08 | 无锡艾科瑞思产品设计与研究有限公司 | Reagent kit and method for quickly detecting arsenic content in I-III water bodies |
| CN103760148B (en) * | 2014-02-19 | 2016-03-23 | 中国科学院生态环境研究中心 | The method of Ionic Liquid Modified nm of gold optical probe and detection arsenic ion |
| CN106670495A (en) * | 2015-11-06 | 2017-05-17 | 南京大学 | Preparation method of network-state Ag-Au-Pd trimetal porous material |
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