CN109270152B - On-site visual detection method for heavy metal arsenic in environmental water sample - Google Patents
On-site visual detection method for heavy metal arsenic in environmental water sample Download PDFInfo
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- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
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- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
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Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/423—Coulometry
Abstract
The invention discloses a field visual detection method for heavy metal arsenic in an environmental water sample, which comprises the steps of firstly adsorbing the heavy metal arsenic in the environmental water sample by modified manganese dioxide, secondly adsorbing the environmental water sample subjected to primary adsorption by modified natural coral, and then measuring the content of the arsenic in each sample liquid by using a coulometric analyzer. According to the invention, the modified manganese dioxide and the modified natural coral are used for adsorbing pentavalent arsenic in an environmental water sample, so that the purpose of detecting heavy metal arsenic in the environmental water sample is achieved while the adsorption effect is measured, and a new direction is provided for detecting and removing arsenic in a water body.
Description
Technical Field
The invention belongs to the technical field of environmental detection, and particularly relates to a field visual detection method for heavy metal arsenic in an environmental water sample.
Background
Arsenic, commonly known as arsenic, is a kind of metal element, arsenic element widely exists in nature, hundreds of arsenic minerals are discovered, arsenic trioxide is called arsenic trioxide, arsenic trioxide is a substance with strong toxicity, year 2017, month 10, day 27, and a carcinogen list published by international cancer research institution of world health organization is initially prepared and referred, and arsenic and inorganic arsenic compounds are in a carcinogen list.
Arsenic and compounds thereof are applied to pesticides, herbicides, insecticides and a plurality of alloys, and the application range of arsenic is wider and wider, so that the content of arsenic substances in water and soil is increased year by year, the arsenic is greatly harmful to human bodies, and the detection of arsenic in environmental water is particularly important.
The commonly used detection methods for arsenic content in water mainly include spectrophotometry, arsenic spot method, catalytic oscillography, hydride-atomic fluorescence method and the like, but the methods can only measure the arsenic content in the water, and can not research the removal method and removal effect of arsenic in the water while measuring, thereby limiting the development of the removal method of arsenic in the water.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a field visual detection method for heavy metal arsenic in an environmental water sample.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a field visual detection method for heavy metal arsenic in an environmental water sample comprises the following steps:
step 1, taking a water sample with the thickness of 100m L to be detected into a clean reaction container, adding 0.84g of manganese dioxide into the reaction container, adjusting the pH value of the water sample to be detected to 2-5, introducing oxygen into the water sample to be detected after the adjustment is finished, controlling the gas flow to be 5L/min, the aeration temperature to be 36 ℃, the aeration time to be 10min, and obtaining an oxidized water sample after the aeration is finished;
step 2: adjusting the pH value of the oxidized water sample to 2-5, after the adjustment is finished, adding 0.10g of modified manganese dioxide serving as an arsenic adsorbent into the oxidized water sample, wherein the adsorption time is 30min, the adsorption temperature is 25 ℃, and after the adsorption is finished, carrying out solid-liquid separation to obtain an arsenic adsorbate and a sample liquid after primary adsorption;
and step 3: adjusting the pH value of the sample liquid after primary adsorption to 2-5, performing secondary adsorption on the sample liquid after primary adsorption by using modified natural coral after the adjustment is finished, and obtaining adsorbed coral and sample liquid after secondary adsorption after the secondary adsorption is finished;
step 4, putting the arsenic adsorbate into a first clean container, adding 8 mol/L hydrochloric acid solution into the first clean container for dissolving to obtain a first sample solution, adjusting the pH value of the first sample solution to 2-5, setting the dissolving time to be 10min, and after dissolving, filtering the first sample solution to obtain a first measurement sample solution;
step 5, placing the adsorbed coral into a second clean container, adding 8 mol/L hydrochloric acid solution into the second clean container for dissolving to obtain a second sample solution, adjusting the pH value of the second sample solution to 2-5, setting the dissolving time to be 10min, and after the dissolving is finished, filtering the second sample solution to obtain a second measurement sample solution;
step 6, respectively transferring 50m L of the first adsorbed sample liquid, the second adsorbed sample liquid, the first measurement sample liquid and the second measurement sample liquid, sequentially placing the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, adding 1m L of 40% acidic stannous oxide and 5m L of 15% potassium iodide solution into the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, fully shaking the mixture, and placing the mixture for 10min to obtain first measurement sample liquid, second measurement sample liquid, third measurement sample liquid and fourth measurement sample liquid;
and 7: measuring the arsenic content in the first measuring sample liquid, the second measuring sample liquid, the third measuring sample liquid and the fourth measuring sample liquid by using a coulometric analyzer to obtain a first arsenic concentration, a second arsenic concentration, a third arsenic concentration and a fourth arsenic concentration;
and 8: obtaining the concentration of heavy metal arsenic in the environmental water sample through the concentration of arsenic in the second determination sample liquid, the concentration of arsenic in the third determination sample liquid and the concentration of arsenic in the fourth determination sample liquid through analysis and conversion;
and step 9: the adsorption rate of the modified manganese dioxide is obtained by comparing the third arsenic concentration with the concentration of heavy metal arsenic in the environmental water sample through analysis and calculation; and (4) comparing the first arsenic concentration with the fourth arsenic concentration, and analyzing and calculating to obtain the adsorption rate of the modified natural coral.
Further, the preparation of the modified manganese dioxide comprises the following steps:
1) taking a first reaction container, and adding 30m L manganese nitrate solution and a certain amount of bismuth nitrate solution into the first reaction container to obtain mixed manganese solution, wherein the molar ratio of manganese ions to bismuth ions in the mixed manganese solution is 10;
2) diluting the mixed manganese solution by a dilution multiple of 5, cooling the mixed manganese solution after the dilution is finished, continuously introducing oxygen into the first reaction container after the cooling is finished, setting the gas flow to be 10L/min, the aeration temperature to be 5 ℃, dropwise adding a sodium hydroxide solution into the mixed manganese solution during the aeration process, wherein the concentration of the sodium hydroxide solution is 6 mol/L, the dropwise adding time is 10min, the dropwise adding amount is 100m L, and filtering after the dropwise adding is finished to obtain a mixture;
3) and (3) washing the mixture by using a sulfuric acid solution, drying the mixture in a vacuum freeze dryer after washing, setting the drying time to be 24h, and obtaining the modified manganese dioxide after drying.
Further, the preparation of the modified natural coral comprises the following steps:
1) taking 100g of coral sample, grinding by a grinder, and sieving by a 100-mesh sieve to obtain a granular coral sample;
2) taking 50g of a granular coral sample, placing the sample in a beaker, and adding 20m L1.0.0% ferric chloride solution into the beaker to obtain a semi-solid mixture;
3) drying the semi-solid mixture in a vacuum freeze dryer for 24 hours, grinding the semi-solid mixture after drying, and sieving with a 100-mesh sieve to obtain mixed particles;
4) and (3) taking 10g of the mixed particles into a crucible, moving the crucible into a muffle furnace, setting the sintering temperature to be 400 ℃, setting the sintering time to be 30min, obtaining a high-temperature sample after sintering, and standing the high-temperature sample to normal temperature to obtain the modified natural coral.
The invention has the beneficial effects that:
the modified manganese dioxide and the modified natural coral are used for adsorbing pentavalent arsenic in an environmental water sample, and the purpose of detecting heavy metal arsenic in the environmental water sample is achieved while the adsorption effect is measured by arranging the two novel adsorbents, namely the modified manganese dioxide and the modified natural coral, so that a new direction is provided for detecting and removing arsenic in a water body.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a flow chart of the detection of heavy metal arsenic in an environmental water sample provided by the invention;
FIG. 2 is a flow chart of the preparation of modified manganese dioxide provided by the present invention;
FIG. 3 is a flow chart of the preparation of the modified natural coral according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "opening," "upper," "lower," "thickness," "top," "middle," "length," "inner," "peripheral," and the like are used in an orientation or positional relationship that is merely for convenience in describing and simplifying the description, and do not indicate or imply that the referenced component or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be considered as limiting the present invention.
Examples
The on-site visual detection method for the heavy metal arsenic in the environmental water sample as shown in fig. 1 comprises the following steps:
step 1, taking 100m L water sample to be detected into a clean reaction container, adding 0.84g of manganese dioxide into the reaction container, adjusting the pH value of the water sample to be detected to 2-5, introducing oxygen into the water sample to be detected after the adjustment is finished, controlling the gas flow to be 5L/min, the aeration temperature to be 36 ℃, the aeration time to be 10min, and obtaining an oxidized water sample after the aeration is finished;
step 2: adjusting the pH value of the oxidized water sample to 2-5, adding 0.10g of modified manganese dioxide serving as an arsenic adsorbent into the oxidized water sample after the adjustment is finished, wherein the adsorption time is 30min, the adsorption temperature is 25 ℃, and after the adsorption is finished, carrying out solid-liquid separation to obtain an arsenic adsorbate and a sample liquid after primary adsorption;
and step 3: adjusting the pH value of the sample liquid after primary adsorption to 2-5, performing secondary adsorption on the sample liquid after primary adsorption by using modified natural coral after the adjustment is finished, and obtaining adsorbed coral and sample liquid after secondary adsorption after the secondary adsorption is finished;
step 4, putting the arsenic adsorbate into a first clean container, adding 8 mol/L hydrochloric acid solution into the first clean container for dissolving to obtain a first sample solution, adjusting the pH value of the first sample solution to 2-5, setting the dissolving time to be 10min, and after the dissolving is finished, filtering the first sample solution to obtain a first measurement sample solution;
step 5, placing the adsorbed coral into a second clean container, adding 8 mol/L hydrochloric acid solution into the second clean container for dissolving to obtain a second sample solution, adjusting the pH value of the second sample solution to 2-5, setting the dissolving time to be 10min, and after the dissolving is finished, filtering the second sample solution to obtain a second measurement sample solution;
step 6, respectively transferring 50m L of primary adsorbed sample liquid, secondary adsorbed sample liquid, first measurement sample liquid and second measurement sample liquid, sequentially placing the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, adding 1m L of 40% acidic stannous oxide and 5m L of 15% potassium iodide solution into the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, fully shaking, and placing for 10min to obtain first measurement sample liquid, second measurement sample liquid, third measurement sample liquid and fourth measurement sample liquid;
and 7: measuring the arsenic content in the first measuring sample liquid, the second measuring sample liquid, the third measuring sample liquid and the fourth measuring sample liquid by using a coulometric analyzer to obtain a first arsenic concentration, a second arsenic concentration, a third arsenic concentration and a fourth arsenic concentration;
and 8: and obtaining the concentration of the heavy metal arsenic in the environmental water sample through the concentrations of the arsenic in the second determination sample liquid, the third determination sample liquid and the fourth determination sample liquid through analysis and conversion, wherein in the process, the sum of the contents of the heavy metals in the three determination sample liquids is the content of the heavy metal arsenic in the environmental water sample.
And step 9: the adsorption rate of the modified manganese dioxide is obtained by comparing the third arsenic concentration with the concentration of heavy metal arsenic in the environmental water sample through analysis and calculation; through comparing first arsenic concentration and fourth arsenic concentration, through the analysis calculation, get the adsorption rate of modified natural coral, through this kind of design, when detecting the content of heavy metal arsenic in the environment water sample, more can be through the calculation of the adsorption rate of two kinds of different modified adsorbent heavy metal arsenic, research is chooseed for use the heavy metal arsenic that suitable adsorbent got rid of in the environment water sample, provides new direction when detecting and getting rid of heavy metal arsenic in the environment water sample.
The adsorption rate is calculated as follows:
r(％)＝(c1-c2)/c1*100％
wherein c1 is the concentration (mu g/L) of heavy metal arsenic in the environmental water sample before adsorption, and c2 is the concentration (mu g/L) of heavy metal arsenic in the solution after adsorption.
As shown in fig. 2, the preparation of modified manganese dioxide comprises the following steps:
1) taking a first reaction container, and adding 30m L manganese nitrate solution and a certain amount of bismuth nitrate solution into the first reaction container to obtain mixed manganese solution, wherein the molar ratio of manganese ions to bismuth ions in the mixed manganese solution is 10;
2) diluting the mixed manganese solution by a dilution multiple of 5, cooling the mixed manganese solution after the dilution is finished, continuously introducing oxygen into the first reaction container after the cooling is finished, setting the gas flow rate to be 10L/min, the aeration temperature to be 5 ℃, dropwise adding a sodium hydroxide solution into the mixed manganese solution during the aeration process, wherein the concentration of the sodium hydroxide solution is 6 mol/L, the dropwise adding time is 10min, and the dropwise adding amount is 100m L, and filtering to obtain a mixture after the dropwise adding is finished;
3) and (3) washing the mixture by using a sulfuric acid solution, drying the mixture in a vacuum freeze dryer after washing is finished, setting the drying time to be 8h, and obtaining the modified manganese dioxide after drying is finished.
As shown in FIG. 3, the preparation of the modified natural coral comprises the following steps:
1) taking 100g of coral sample, grinding by a grinder, and sieving by a 100-mesh sieve to obtain a granular coral sample;
2) taking 50g of a granular coral sample, placing the sample in a beaker, and adding 20m of L1.0.0% ferric chloride solution into the beaker to obtain a semisolid mixture;
3) drying the semi-solid mixture in a vacuum freeze dryer for 24h, grinding the semi-solid mixture after drying, and sieving with a 100-mesh sieve to obtain mixed particles;
4) and (3) taking 10g of mixed particles into a crucible, moving the crucible into a muffle furnace, setting the sintering temperature to be 400 ℃, setting the sintering time to be 30min, obtaining a high-temperature sample after sintering, and standing the high-temperature sample to normal temperature to obtain the modified natural coral.
In the invention, the modified manganese dioxide and the modified natural coral are used for adsorbing pentavalent arsenic in an environmental water sample, and the purpose of detecting heavy metal arsenic in the environmental water sample is achieved by setting two novel adsorbents, namely the modified manganese dioxide and the modified natural coral, while the adsorption effect is measured, so that a new direction is provided for detecting and removing arsenic in a water body.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (1)
1. The on-site visual detection method for heavy metal arsenic in an environmental water sample is characterized by comprising the following steps: the method comprises the following steps:
step 1, taking a water sample with the volume of 100m L to be detected into a clean reaction container, adding 0.84g of manganese dioxide into the reaction container, adjusting the pH value of the water sample to be detected to 2-5, introducing oxygen into the water sample to be detected after the adjustment is finished, controlling the gas flow to be 5L/min, the aeration temperature to be 36 ℃, the aeration time to be 10min, and obtaining an oxidized water sample after the aeration is finished;
step 2, adjusting the pH value of the oxidized water sample to 2-5, after the adjustment is finished, adding 0.10g of modified manganese dioxide serving as an arsenic adsorbent into the oxidized water sample, wherein the adsorption time is 30min, the adsorption temperature is 25 ℃, and after the adsorption is finished, performing solid-liquid separation to obtain an arsenic adsorbate and a sample liquid after primary adsorption;
step 3, adjusting the pH value of the sample liquid after primary adsorption to 2-5, performing secondary adsorption on the sample liquid after primary adsorption by using modified natural coral after adjustment, and obtaining coral after adsorption and sample liquid after secondary adsorption;
step 4, putting the arsenic adsorbate into a first clean container, adding 8 mol/L hydrochloric acid solution into the first clean container for dissolving to obtain a first sample solution, adjusting the pH value of the first sample solution to 2-5, setting the dissolving time to be 10min, and after dissolving, filtering the first sample solution to obtain a first measurement sample solution;
step 5, placing the adsorbed coral into a second clean container, adding 8 mol/L hydrochloric acid solution into the second clean container for dissolving to obtain a second sample solution, adjusting the pH value of the second sample solution to 2-5, setting the dissolving time to be 10min, and after the dissolving is finished, filtering the second sample solution to obtain a second measurement sample solution;
step 6, respectively transferring 50m L of the first adsorbed sample liquid, the second adsorbed sample liquid, the first measurement sample liquid and the second measurement sample liquid, sequentially placing the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, adding 1m L of 40% acidic stannous oxide and 5m L of 15% potassium iodide solution into the first measurement container, the second measurement container, the third measurement container and the fourth measurement container, fully shaking the mixture, and placing the mixture for 10min to obtain first measurement sample liquid, second measurement sample liquid, third measurement sample liquid and fourth measurement sample liquid;
step 7, measuring the arsenic content in the first measuring sample liquid, the second measuring sample liquid, the third measuring sample liquid and the fourth measuring sample liquid by using a coulometric analyzer to obtain a first arsenic concentration, a second arsenic concentration, a third arsenic concentration and a fourth arsenic concentration;
8, obtaining the concentration of heavy metal arsenic in the environmental water sample through analysis and conversion according to the concentrations of arsenic in the second determination sample liquid, the third determination sample liquid and the fourth determination sample liquid;
step 9, comparing the third arsenic concentration with the concentration of heavy metal arsenic in the environmental water sample, and analyzing and calculating to obtain the adsorption rate of the modified manganese dioxide; the adsorption rate of the modified natural coral is obtained by comparing the first arsenic concentration with the fourth arsenic concentration and analyzing and calculating;
wherein the preparation of the modified manganese dioxide comprises the following steps:
a1, taking a first reaction container, and adding a manganese nitrate solution with the molar ratio of 30m L and a certain amount of bismuth nitrate solution into the first reaction container to obtain a mixed manganese solution, wherein the molar ratio of manganese ions to bismuth ions in the mixed manganese solution is 10;
a2, diluting the mixed manganese solution by a dilution multiple of 5, cooling the mixed manganese solution after the dilution is finished, continuously introducing oxygen into the first reaction container after the cooling is finished, setting the gas flow rate to be 10L/min and the gas introduction temperature to be 5 ℃, dropwise adding a sodium hydroxide solution into the mixed manganese solution during the gas introduction process, wherein the concentration of the sodium hydroxide solution is 6 mol/L, the dropwise adding time is 10min, the dropwise adding amount is 100m L, and filtering after the dropwise adding is finished to obtain a mixture;
a3, washing the mixture by using a sulfuric acid solution, drying the mixture in a vacuum freeze dryer after washing, setting the drying time to be 24 hours, and obtaining modified manganese dioxide after drying;
wherein, the preparation of the modified natural coral comprises the following steps:
b1, taking 100g of coral sample, grinding by a grinder, and sieving by a 100-mesh sieve to obtain a granular coral sample;
b2, placing 50g of a granular coral sample into a beaker, and adding a 20m L1.0% ferric chloride solution into the beaker to obtain a semi-solid mixture;
b3, drying the semi-solid mixture in a vacuum freeze dryer for 24 hours, grinding the semi-solid mixture after drying, and sieving with a 100-mesh sieve to obtain mixed particles;
and B4, taking 10g of the mixed particles into a crucible, moving the crucible into a muffle furnace, setting the sintering temperature at 400 ℃ and the sintering time at 30min, obtaining a high-temperature sample after sintering, and standing the high-temperature sample to normal temperature to obtain the modified natural coral.
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| CN201811215014.XA CN109270152B (en) | 2018-10-18 | 2018-10-18 | On-site visual detection method for heavy metal arsenic in environmental water sample |
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| CN1751783A (en) * | 2005-07-20 | 2006-03-29 | 上海自来水市北科技有限公司 | Composite absorption material for removing arsenic from water and its prepn. method |
| CN103708587A (en) * | 2014-01-03 | 2014-04-09 | 长沙皓龙环保科技有限公司 | Preparation method of composite electrode for removing arsenic in water based on electro-adsorption and method for removing arsenic |
| CN107983300A (en) * | 2016-10-27 | 2018-05-04 | 湖南大学 | Biological carbon composite of manganese dioxide modification and its preparation method and application |
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| CN1751783A (en) * | 2005-07-20 | 2006-03-29 | 上海自来水市北科技有限公司 | Composite absorption material for removing arsenic from water and its prepn. method |
| CN103708587A (en) * | 2014-01-03 | 2014-04-09 | 长沙皓龙环保科技有限公司 | Preparation method of composite electrode for removing arsenic in water based on electro-adsorption and method for removing arsenic |
| CN107983300A (en) * | 2016-10-27 | 2018-05-04 | 湖南大学 | Biological carbon composite of manganese dioxide modification and its preparation method and application |
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| Selective Adsorption of Arsenic(V)Ion by Use of Iron(III) Hydroxide-Loaded Coral Limestone;SHIGERU MAEDA et.al;《SEPARATION SCIENCE AND TECHNOLOGY》;20061023;第25卷(第5期);第547-555页 * |
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