CN112326571A - Quantitative detection method for pentavalent arsenic in water sample - Google Patents
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Abstract
The invention relates to a quantitative detection method of pentavalent arsenic in a water sample, belonging to the field of analytical chemistry and comprising the following steps: preparing a monothio-arsenic acid standard solution with gradient concentration, measuring the absorbance of the monothio-arsenic acid standard solution at a characteristic wavelength, and drawing a standard curve based on the corresponding pentavalent arsenic concentration and absorbance in the monothio-arsenic acid standard solution; adjusting a water sample to be detected to be acidic, adding excessive negative divalent sulfide for mixing and reacting, and performing nitrogen stripping and constant volume on the water sample to be detected after the reaction is finished to obtain a solution to be detected; and testing the absorbance of the solution to be tested under the characteristic wavelength and bringing the absorbance into a standard curve to obtain the concentration of the pentavalent arsenic in the solution to be tested. The method can directly determine the content of pentavalent arsenic in the water sample, has simple sample pretreatment process and short required time, can realize the rapid detection of the pentavalent arsenic in the water sample, is not interfered by trivalent arsenic and other coexisting ions contained in the water sample in the analysis process, and has high accuracy and precision of the determination result.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to a quantitative detection method for pentavalent arsenic in a water sample.
Background
The industries of non-ferrous metal smelting, pharmacy, tanning, mining and the like can generate arsenic-containing waste water, and the environmental health is harmed.
Inorganic arsenic in aqueous solution is mainly arsenite (As (III), AsO3 3-) And arsenate (As (V), AsO4 3-) The two forms exist, and the chemical property, the environmental behavior and the biological toxicity of the two forms are greatly different. For example, trivalent arsenic is more toxic than pentavalent arsenic, and less mobile than pentavalent arsenic; in addition, in environmental pollution treatment, pentavalent arsenic is easy to adsorb and remove compared with trivalent arsenic. Therefore, in order to select a proper method for treating the arsenic-containing wastewater, quantitative detection of arsenic with different forms in the wastewater is particularly important.
The inorganic arsenic in water sample is measured by atomic fluorescence spectrometry, inductively coupled plasma spectrometry, arsenic-molybdenum blue spectrophotometry and silver diethyldithiocarbamate spectrophotometry. But the method is suitable for measuring the total arsenic content in the water sample.
Although the atomic fluorescence spectrometry can use a difference method to measure trivalent arsenic and pentavalent arsenic in wastewater, the measurement needs to be performed twice on a sample, and the operation is complex and long.
In addition, the arsenic form analysis method can be realized by methods such as ion chromatography, ion chromatography-atomic fluorescence spectrometry, high performance liquid chromatography-inductively coupled plasma mass spectrometry and the like, but the analysis methods have the defects of complex pretreatment, long detection time and the like.
At present, trivalent arsenic in a water sample can be directly measured by adopting an atomic fluorescence spectrometry, and a simple and effective quantitative detection method for pentavalent arsenic in the water sample is not available. The above problems are technical problems to be solved in the art.
Disclosure of Invention
The invention provides a quantitative detection method for pentavalent arsenic in a water sample to solve the technical problems.
The technical scheme for solving the technical problems is as follows: a quantitative detection method for pentavalent arsenic in a water sample comprises the following steps:
preparing a monothio-arsenic acid standard solution with gradient concentration, measuring the absorbance of the monothio-arsenic acid standard solution with each concentration at a characteristic wavelength, and drawing a standard curve based on the corresponding pentavalent arsenic concentration and the corresponding absorbance in the monothio-arsenic acid standard solution;
adjusting a water sample to be detected to be acidic, adding excessive negative divalent sulfide for mixing and reacting, and performing nitrogen stripping and constant volume on the water sample to be detected after the reaction is finished to obtain a solution to be detected;
and measuring the absorbance of the solution to be detected under the characteristic wavelength and bringing the absorbance into the standard curve to obtain the concentration of pentavalent arsenic in the water sample to be detected.
The principle of the method is that under an acidic condition, pentavalent arsenic in a water sample to be detected can react with negative divalent sulfur to generate dissolved monothio-arsenic acid, and trivalent arsenic can react with the negative divalent sulfur immediately to generate arsenic sulfide precipitate. Monothioarsenic acid is relatively stable under acidic conditions and has an absorption peak at a particular wavelength. After vulcanization, the influence of trivalent arsenic in a water sample can be eliminated, and the amount of pentavalent arsenic in the water sample is the same as the amount of arsenic contained in the monosulfuric arsenic acid generated by vulcanization. Therefore, the method utilizes the characteristic that the monothio-arsenic acid has an absorption peak at a specific wavelength to quantitatively detect the pentavalent arsenic in the water sample by adopting a spectrophotometry method.
The invention has the beneficial effects that: the method can directly measure the content of pentavalent arsenic in the water sample, has simple sample pretreatment process and short required time, can realize the rapid detection of the pentavalent arsenic in the water sample, is not interfered by trivalent arsenic and other coexisting ions contained in the water sample in the analysis process, and has high precision and accuracy of the measured result.
Further, the concentration of the standard solution of the mono-sulfur arsenic acid is 0-50 mg/L. In the embodiment disclosed by the invention, the monothio-arsenic acid standard solution is prepared by dissolving monothio-arsenate in acid solutions with different volumes, wherein the monothio-arsenate is prepared by adopting the following method: 1.44g of sulfur was added to 20mL of a solution containing 5.00g of As 203And 6.00g of NaOH aqueous solution, heating the solution to 100 ℃, filtering out excessive sulfur after 2 hours, slowly cooling the solution to 4 ℃, separating out colorless needle crystals, and performing vacuum filtration and drying to obtain the sodium monosulfoarsenate.
Further, the characteristic wavelength is 220-275 nm. The monothio-arsenic acid has an absorption peak in the wavelength range of 220-275 nm.
Further, the characteristic wavelength is 233 nm. In the embodiment disclosed by the invention, the solution of the monothio-arsenic acid has the maximum absorption peak lambda max at 233nm, so that the characteristic wavelength of the monothio-arsenic acid is analyzed by adopting a spectrophotometric method of 233 nm.
Further, the method for adjusting the acidity is as follows: and adjusting the water sample to be detected to be acidic by adding acid liquor into the water sample to be detected, wherein the concentration of hydrogen ions added into the water sample to be detected by the acid liquor is 0.1-2 mol/L. The acid solution used in the embodiment disclosed by the invention is any one of sulfuric acid, hydrochloric acid and nitric acid, and the hydrogen ion concentration can be 1mol/L by taking the water sample volume as 2mL as an example
Further, the amount of the divalent negative sulfide added is 0.05mmol or more. The embodiment of the invention tests that when the concentration ratio of the negative divalent sulfur to the pentavalent arsenic is more than or equal to 7.5, the pentavalent arsenic can be completely converted into the monothio-arsenic acid within 10 min. Because the concentration of pentavalent arsenic in a water sample is limited, 2mL of the water sample is diluted to 10mL according to the calculation that the upper limit of the determination of the pentavalent arsenic is 50mg/L, the maximum allowable concentration in the water sample is 250mg/L, and the volume of the added solution is more than or equal to 0.5mL when the negative divalent sulfide with the concentration of 0.1mol/L is added to react with the pentavalent arsenic.
Further, the negative divalent sulfide is one or more of sodium sulfide, potassium sulfide, ammonium sulfide, sodium hydrosulfide, potassium hydrosulfide and ammonium hydrosulfide.
Further, in the step of adding the divalent negative sulfide for mixing and reacting, the mixing and reacting are carried out under the ultrasonic condition, the ultrasonic power is 100W, and the ultrasonic time is more than 10 min.
Further, in the step of performing nitrogen stripping and constant volume on the water sample to be detected, the flow rate of the adopted nitrogen is 10mL/min, the stripping time is more than 10min, and the constant volume is performed in a 10mL colorimetric tube by adopting deionized water or ultrapure water. The excessive negative divalent sulfur can generate hydrogen sulfide in the acidic solution, the hydrogen sulfide has an absorption peak in the wavelength range of 190-400 nm, the absorption peak is partially overlapped with the absorption peak of monothio-arsenic acid, the hydrogen sulfide in the solution can be removed by a stripping method under the acidic condition, the absorbance of the solution at 233nm is reduced along with the stripping time through the test of the embodiment of the invention, and the absorbance is reduced to the minimum and is kept unchanged when the stripping time is more than 9 min. In order to ensure complete stripping, the stripping time needs to be over 10 min.
Further, the step of testing the absorbance of the solution to be tested at the characteristic wavelength and bringing the absorbance into the standard curve comprises the steps of:
and obtaining a standard curve equation of absorbance-concentration based on the standard curve, bringing the absorbance of the solution to be detected under the characteristic wavelength into the standard curve equation, calculating to obtain the concentration of the pentavalent arsenic in the solution to be detected, and calculating to obtain the concentration of the pentavalent arsenic in the water sample to be detected based on the dilution multiple of the solution to be detected compared with the water sample to be detected. When the characteristic wavelength is 233nm, the standard curve equation is that y is 0.0217x +0.0619, R20.9992, where x represents the concentration of pentavalent arsenic and y represents the absorbance, the formula of the concentration of pentavalent arsenic in the solution to be tested is C1(y-0.0619)/0.0217. When the volume is fixed to 10mL, the dilution factor kappa of the water sample to be detected is 10/V, wherein V is the volume/mL of the taken water sample to be detected, and the quinquevalent arsenic concentration C in the water sample to be detected can be calculated2＝κC1
Drawings
FIG. 1 is an absorption spectrum of a standard solution of mono-sulfurous arsenic acid at different wavelengths;
FIG. 2 is a pentavalent arsenic concentration-absorbance standard curve obtained by fitting based on absorption spectra of different concentrations of monothio-arsenic acid standard solutions at characteristic wavelengths;
FIG. 3 is the absorbance of monothioarsenic acid at a wavelength of 233nm for different hydrogen ion concentrations;
FIG. 4 is a graph of the reaction time of monothioarsenic acid with different concentration ratios of negative divalent sulfur to pentavalent arsenic;
FIG. 5 is an absorption spectrum at different wavelengths before and after stripping of hydrogen sulfide contained in a solution;
FIG. 6 shows the change of absorbance of the solution at 233nm wavelength, when the ratio of S to As is 7.5, the hydrogen ion concentration is 1mol/L, the solution is blown off for 10min and the volume is 10 mL.
Detailed Description
The principles and features of this invention are described below in conjunction with the accompanying drawings and examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
In the description of the present specification, it is to be understood that the terms "center", "length", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "inner", "outer", "peripheral side", "circumferential", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present specification.
In the description of the present specification, "a plurality" means at least two, e.g., two, three, etc., unless explicitly defined otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., 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 are not necessarily intended to 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. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The terms used in the present specification are those general terms currently widely used in the art in consideration of functions related to the present disclosure, but they may be changed according to the intention of a person having ordinary skill in the art, precedent, or new technology in the art. Also, specific terms may be selected by the inventor, and in this case, their detailed meanings will be described in the detailed description of the present disclosure. Therefore, the terms used in the specification should not be construed as simple names but based on the meanings of the terms and the overall description of the present disclosure.
Flowcharts or text are used in the present invention to illustrate the operational steps performed according to embodiments of the present invention. It should be understood that the operational steps in the embodiments of the present invention are not necessarily performed in the exact order recited. Rather, the various steps may be processed in reverse order or simultaneously, as desired. Meanwhile, other operations may be added to the processes, or a certain step or several steps of operations may be removed from the processes.
The following discloses many different embodiments or examples for implementing the subject technology described. While specific examples of one or more arrangements of features are described below to simplify the disclosure, the examples should not be construed as limiting the present disclosure, and a first feature described later in the specification in conjunction with a second feature can include embodiments that are directly related, can also include embodiments that form additional features, and further can include embodiments in which one or more additional intervening features are used to indirectly connect or combine the first and second features to each other so that the first and second features may not be directly related.
Preparing a standard solution:
in the embodiment disclosed by the invention, the pentavalent arsenic standard solution with gradient concentration is prepared by diluting a sodium monothioarsenate stock solution (the pentavalent arsenic concentration is 1000mg/L), the concentration range is 0.5-50 mg/L, and the specifically selected concentration is as shown in figure 2.
In the embodiment disclosed by the invention, an ultraviolet-visible spectrophotometer is adopted to carry out wavelength scanning on a solution with the concentration of 3mmol/L monothio-arsenic acid to obtain an absorption spectrum, and the result is shown in figure 1. The result shows that the monothio-arsenic acid has an absorption peak in the wavelength range of 220-275 nm, and the maximum absorption peak lambda max is 233 nm.
Measuring and recording the absorbance of standard solutions with different concentrations by using 233nm wavelength as characteristic wavelength, and drawing a standard curve with fitting as shown in figure 2, wherein the equation of the standard curve is that y is 0.0217x +0.0619, and R is20.9992, where x represents the pentavalent arsenic concentration and y represents the absorbance.
In the following embodiments disclosed in the present invention, the characteristic wavelength is 233nm, the curve shown in fig. 2 is used as a standard curve for testing, and the water sample to be tested is any one of mine wastewater, non-ferrous metal smelting wastewater, pharmaceutical wastewater and tanning wastewater containing pentavalent arsenic.
Example 1
Taking 2mL of mine wastewater containing pentavalent arsenic as a first sample, adding the mine wastewater into a 10mL test tube with a plug, adding 0.27mL of concentrated sulfuric acid, adding 50 mu L of 1mol/L negative divalent sulfide solution, sealing, carrying out ultrasonic mixing reaction for 10min, then blowing off the solution for 10min by nitrogen with the flow of 10mL/min, filtering all the solutions by using a 0.22 mu m filter membrane, transferring the solutions into a 10mL colorimetric tube, fixing the volume to 10mL by using deionized water, inverting the colorimetric tube for 2-3 times, uniformly mixing the components to obtain a solution to be detected, measuring the absorbance of the solution to be detected at the wavelength of 233nm, bringing the solution to a standard curve to obtain the concentration of the pentavalent arsenic in the solution to be detected, and calculating the concentration of the pentavalent arsenic in the mine wastewater according to the dilution multiple of the solution to the first sample.
Example 2
Taking arsenic-containing wastewater generated by smelting certain nonferrous metals as a second sample, wherein the total arsenic concentration in the wastewater is 1200mg/L, and the hydrogen ion concentration is 2.04 mol/L. Firstly, a water sample is diluted by 5 times by deionized water, 2mL of the diluted water sample is put into a 10mL test tube with a plug, and 0.84mL of concentrated hydrochloric acid is added. The other operating steps are the same as those described in example 1. The actual concentration of the pentavalent arsenic in the wastewater is obtained by multiplying the measured concentration of the pentavalent arsenic in the diluted water sample by the dilution factor.
Example 3
Taking 2mL of pentavalent arsenic-containing pharmaceutical wastewater as a third sample, adding the third sample into a 10mL test tube with a plug, and adding 0.27mL of concentrated sulfuric acid. The other operating steps are the same as those described in example 1.
The results of the measurement of the pentavalent arsenic concentrations in examples 1 to 3 are shown in Table 1:
TABLE 1 test results of pentavalent arsenic concentrations in examples 1-3
| Sample (I) | Pentavalent arsenic concentration (mg/L) |
| Sample No. 1 | 4.67 |
| Sample No. 2 | 46.87 |
| Sample No. 3 | 16.54 |
Example 4
The accuracy of the method for determining pentavalent arsenic in the water sample disclosed in the embodiments 1-3 of the invention is evaluated, and the specific method comprises the following steps: the accuracy of the detection of the present method was evaluated by performing 10 independent assays for each of examples 1 to 3, and statistically calculating the mean and Relative Standard Deviation (RSD) of 10 measurements, respectively, with the results shown in table 2:
table 2 accuracy evaluation test data table (n ═ 10)
| Sample (I) | Average of 10 measurements | RSD(％) |
| Sample No. 1 | 4.16 | 4.25 |
| Sample No. 2 | 46.02 | 2.89 |
| Sample No. 3 | 15.86 | 3.18 |
As can be seen from Table 2, the relative standard deviation RSD of the pentavalent arsenic in the water sample repeatedly measured under different concentration conditions is less than 5.0%, which shows that the repeated measurement results are consistent, the repeatability and reproducibility of the method are good, and the method has high accuracy.
Example 5
In this example, the standard recovery rate test of examples 1 to 3 was performed to verify the accuracy of the quantitative detection method for pentavalent arsenic in water samples according to the present invention, and the test results are shown in table 3:
TABLE 3 recovery test data sheet
As can be seen from Table 3, the recovery rate of the quantitative detection method for pentavalent arsenic in a water sample provided by the invention is 95.7% -98.5%, which shows that the method provided by the invention has high accuracy and reliable result.
In the disclosed embodiment of the present invention, the effect of the concentration of hydrogen ions on absorbance is shown in FIG. 3, which shows that hydrogen ions do not affect the absorbance of the solution.
The generation of monothio-arsenic acid along with the reaction time is shown in figure 4, which shows that when the concentration ratio of the negative divalent sulfur to the pentavalent arsenic is more than or equal to 7.5, the pentavalent arsenic can be completely converted into monothio-arsenic acid within 10 min. In the disclosed embodiment, according to the upper limit of the pentavalent arsenic measurement of 50mg/L, 2mL of water sample is diluted to 10mL, and the maximum allowable concentration in the water sample is 250mg/L, at least 0.05mmol of negative divalent sulfur needs to be added.
In the above embodiment of the present disclosure, the nitrogen stripping is performed on the reacted solution because the excessive negative divalent sulfur generates hydrogen sulfide in the acidic solution as shown in fig. 5, and the hydrogen sulfide has an absorption peak in the wavelength range of 190-400 nm, which partially overlaps with the absorption peak of monothioarsenic acid, and the hydrogen sulfide in the solution can be removed by the stripping method under the acidic condition. The flow rate of nitrogen gas during stripping was 10mL/min, and the relationship between the absorbance of the solution at 233nm and the stripping time during stripping is shown in FIG. 6, which indicates that the absorbance is minimized and maintained when the stripping time is greater than 9 min. In order to ensure complete stripping, the stripping time is at least 10 min.
The principle of the invention is that under the acidic condition, pentavalent arsenic in a water sample can react with negative divalent sulfur to generate dissolved monothio-arsenic acid, and trivalent arsenic can react with negative divalent sulfur ions to generate arsenic sulfide precipitate immediately. Monothioarsenic acid is relatively stable under acidic conditions and has an absorption peak at a particular wavelength. After vulcanization, the influence of trivalent arsenic in a water sample can be eliminated, and the amount of pentavalent arsenic in the water sample is the same as the amount of arsenic contained in the monosulfuric arsenic acid generated by vulcanization. Therefore, the method utilizes the characteristic that the monothio-arsenic acid has an absorption peak at a specific wavelength to quantitatively determine the pentavalent arsenic in the water sample by adopting a spectrophotometry method.
Compared with the existing method for determining the pentavalent arsenic in the water sample by the differential method, the method for quantitatively analyzing the pentavalent arsenic in the water sample provided by the invention converts the pentavalent arsenic in the water sample into monothio-arsenic acid by means of sulfurization, and the absorbance of the monothio-arsenic acid at a specific wavelength is determined, so that the concentration of the pentavalent arsenic in the water sample can be directly obtained.
The quantitative analysis method for pentavalent arsenic in the water sample provided by the invention has the advantages of simple sample pretreatment process and short required time, and can realize rapid detection of pentavalent arsenic in the water sample.
According to the quantitative analysis method for pentavalent arsenic in the water sample, provided by the invention, the analysis process is not interfered by trivalent arsenic and other coexisting ions in the water sample, and the accuracy and the precision of the measurement result are high
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A quantitative detection method for pentavalent arsenic in a water sample is characterized by comprising the following steps:
preparing a monothio-arsenic acid standard solution with gradient concentration, measuring the absorbance of the monothio-arsenic acid standard solution with each concentration at a characteristic wavelength, and drawing a standard curve based on the corresponding pentavalent arsenic concentration and the corresponding absorbance in the monothio-arsenic acid standard solution;
adjusting a water sample to be detected to be acidic, adding excessive negative divalent sulfide for mixing and reacting, and performing nitrogen stripping and constant volume on the water sample to be detected after the reaction is finished to obtain a solution to be detected;
and measuring the absorbance of the solution to be detected under the characteristic wavelength and bringing the absorbance into the standard curve, and calculating to obtain the concentration of pentavalent arsenic in the water sample to be detected.
2. The method for quantitatively detecting pentavalent arsenic in the water sample according to claim 1, wherein the concentration of the standard solution of monothioarsenic acid is 0-50 mg/L.
3. The method for quantitatively detecting pentavalent arsenic in water samples according to claim 1, wherein the characteristic wavelength is between 220 nm and 275 nm.
4. The method for quantitatively detecting pentavalent arsenic in water samples according to claim 1 or 3, wherein the characteristic wavelength is 233 nm.
5. The method for quantitatively detecting pentavalent arsenic in water samples according to claim 1, wherein the method for adjusting to acidity is: and adjusting the water sample to be detected to be acidic by adding acid liquor into the water sample to be detected, wherein the concentration of hydrogen ions added into the water sample to be detected by the acid liquor is 0.1-2 mol/L.
6. The method for quantitatively detecting pentavalent arsenic in a water sample according to claim 1, wherein the amount of the divalent negative sulfide added is 0.1mol/ml, and the volume of the added divalent negative sulfide is 0.5ml or more.
7. The method for quantitatively detecting pentavalent arsenic in a water sample according to claim 1, wherein the negative divalent sulfide is one or more of sodium sulfide, potassium sulfide, ammonium sulfide, sodium hydrosulfide, potassium hydrosulfide and ammonium hydrosulfide.
8. The method for quantitatively detecting pentavalent arsenic in a water sample according to claim 1, wherein in the step of adding the divalent negative sulfide for mixing and reacting, the mixing and reacting are performed under ultrasonic conditions, wherein the ultrasonic power is 100W, and the ultrasonic time is more than 10 min.
9. The method for quantitatively detecting the pentavalent arsenic in the water sample according to claim 1, wherein in the step of blowing off the water sample to be detected with nitrogen and fixing the volume, the flow of the nitrogen is 10mL/min, the blowing-off time is 10min or more, and the fixing the volume is performed in a 10mL colorimetric tube by using deionized water or ultrapure water.
10. The method for quantitatively detecting pentavalent arsenic in a water sample as claimed in claim 1, wherein said step of testing the absorbance of the solution to be tested at the characteristic wavelength and bringing the solution to the standard curve comprises the steps of:
and obtaining a standard curve equation of absorbance-concentration based on the standard curve, bringing the absorbance of the solution to be detected under the characteristic wavelength into the standard curve equation, calculating to obtain the concentration of the pentavalent arsenic in the solution to be detected, and calculating to obtain the concentration of the pentavalent arsenic in the water sample to be detected based on the dilution multiple of the solution to be detected compared with the water sample to be detected.
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