CN115436309B - Ultraviolet detection method for rapidly and accurately measuring lead concentration - Google Patents
Ultraviolet detection method for rapidly and accurately measuring lead concentration Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000000825 ultraviolet detection Methods 0.000 title claims abstract description 19
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
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- 238000002835 absorbance Methods 0.000 claims description 22
- 239000012086 standard solution Substances 0.000 claims description 18
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000007974 sodium acetate buffer Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention discloses an ultraviolet detection method for rapidly and accurately detecting lead concentration, and belongs to the technical field of online monitoring. Aiming at the problems that the volume of a solution to be measured is large and the measurement is inconvenient when heavy metals are measured by a xylenol orange chromogenic method, the invention provides an ultraviolet detection method for rapidly and accurately measuring the lead concentration. The method has the advantages of small volume of the liquid to be detected, low cost, simple and convenient instrument operation, high analysis speed, good accuracy in a certain concentration range and the like, can simply, quickly and accurately quantify the heavy metal lead in the water environment, can measure the adsorption effect of the micro-plastic on the lead, and can meet the quantitative test requirement of pollutants in the environmental field.
Description
Technical Field
The invention relates to an ultraviolet detection method for rapidly and accurately measuring lead concentration, and belongs to the technical field of online monitoring.
Background
Heavy metals are a common pollutant, have the characteristic of nondegradable and have great negative influence on water bodies. Lead is used as one of heavy metal elements, and is widely used in electroplating industry, steel industry, electric industry and the like, and industrial process wastewater discharged by each industry contains a large amount of lead and has potential toxicity to human beings and aquatic environments. For example, as the mining amount of lead zinc ores increases in recent years, the dumping of tailings causes different degrees of pollution to the environment. Research shows that the pollution can lead the content of surface water, sediment and soil near a lead-zinc mining area to exceed the standard. Lead contamination can have a certain impact on human health and ingestion of lead can lead to symptoms such as mental retardation, kidney and nervous system injury, cancer, poor pregnancy, etc. Therefore, the research of the environmental behavior of lead is of great importance.
The detection method of the lead concentration is the basis for researching the environmental behavior of lead. There are many methods for measuring lead, mainly inductively coupled plasma emission spectrometry (ICP-OES), plasma mass spectrometry (ICP-MS), spectrophotometry, atomic absorption spectrometry, polarography, atomic fluorescence spectrometry, stripping voltammetry, and the like. The spectrophotometry has the advantages of high sensitivity, simple operation, high analysis speed, low price and the like, and is a detection method commonly used by researchers. Spectrophotometry for determining lead content reported at present comprises xylenol orange chromogenic method and dithizone chromogenic method. The dithiozone color development method has the limitations of complicated operation, poor selectivity and the like, and limits the popularization of the method. When xylenol orange is used as a color developing agent for measuring the lead content, the relative standard deviation of the measurement result is smaller, the accuracy of the result is higher, and the method is widely applied, but when the method is used for measuring the lead concentration, the amount of the raw solution is more, and the measurement is more inconvenient.
Disclosure of Invention
Aiming at the problems that the volume of a solution to be measured is large and the measurement is inconvenient when heavy metals are measured by a xylenol orange chromogenic method, the invention provides an ultraviolet detection method for rapidly and accurately measuring the lead concentration.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides an ultraviolet detection method for rapidly and accurately measuring lead concentration, which comprises the following steps:
(1) Preparation of lead standard solution
Lead standard solutions with the concentration of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L are respectively prepared;
(2) Establishment of a Standard Curve
Respectively taking 1mL of the lead standard solution, sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate (HAC-NaAC) buffer solution, uniformly mixing, and then carrying out ultraviolet absorbance detection at 568nm wavelength to establish a standard curve between absorbance and lead concentration;
(3) Pretreatment of a sample to be tested
Diluting a sample to be tested containing lead with different concentration gradients, determining whether the sample is in the linear range of a regression equation or not by using the method of the step (4) of the invention, and if not, continuing to dilute;
(4) Lead concentration C pb Is measured by (a)
Taking 1mL of the lead-containing sample to be detected treated in the step (3), sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution, uniformly mixing, detecting ultraviolet absorbance at 568nm wavelength, and calculating the concentration of lead through the obtained absorbance and the standard curve obtained in the step (2).
Further, in the step (2), the usage ratio of the lead standard solution to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL, in the step (4), the dosage ratio of the lead sample to be tested to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL.
Further, the concentration of the xylenol orange solution was 1g/L, and the pH of the acetic acid-sodium acetate buffer solution was 6.
Further, in the step (3), the lead-containing sample to be measured is diluted with different concentration gradients, and the concentration of the lead in the diluted lead-containing sample to be measured is in the range of 0-10 mg/L and does not comprise 0.
The invention also provides application of the ultraviolet detection method in quantitative detection of the lead concentration in the water environment.
The invention also provides application of the ultraviolet detection method in measuring the adsorption effect of the micro plastic on lead.
The invention discloses the following technical effects:
(1) The invention discloses a method for analyzing and detecting lead concentration by an ultraviolet-spectrophotometry, which comprises the steps of sequentially adding reagents with a certain proportion into 1mL of diluted or concentrated lead-containing liquid to be detected by using a xylenol orange chromogenic method, testing the absorbance values of lead under the color development of xylenol orange with different concentrations by using an ultraviolet 2000 ultraviolet-visible light spectrophotometry, and then establishing a regression equation between the lead concentration and the absorbance values, wherein the equation can be used for calculating the lead concentration in a sample to be detected by using the ultraviolet spectrophotometry. The method has the advantages of small volume of the liquid to be measured, low cost, simple and convenient instrument operation, high analysis speed, good accuracy in a certain concentration range and the like, and has wide application prospect.
(2) Compared with the common quantitative method, the ultraviolet detection method has the advantages of simple operation, convenience, rapidness, lower cost, no need of using large-scale instruments and no need of complex pretreatment. The method can simply, rapidly and accurately quantify the heavy metal lead in the water environment, and can meet the quantitative test requirement of pollutants in the environmental field.
(3) Under the applicable concentration range of 0-10 mg/L, the method can accurately measure the lead concentration, and compared with the existing xylenol orange color development method, the method only uses 1mL of lead-containing solution to be measured, the dosage is about 20 times less than that of the existing xylenol orange color development method, the sample is saved, and the method is suitable for the research of less sampling quantity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the ultraviolet absorption spectrum of a lead standard solution at a partial concentration in example 1 of the present invention;
FIG. 2 is a graph showing the absorbance and lead concentration versus standard curve for example 1 of the present invention;
FIG. 3 is a graph showing the data of the adsorption result of the microplastic to lead at different ionic strengths.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The invention discloses a method for analyzing and detecting lead concentration by an ultraviolet-spectrophotometry, which comprises the steps of sequentially adding reagents with a certain proportion into 1mL of diluted or concentrated lead-containing liquid to be detected by using a xylenol orange chromogenic method, testing the absorbance values of lead under the color development of xylenol orange with different concentrations by using an ultraviolet 2000 ultraviolet-visible light spectrophotometry, and then establishing a regression equation between the lead concentration and the absorbance values, wherein the equation can be used for calculating the lead concentration in a sample to be detected by using the ultraviolet spectrophotometry. The method has the advantages of small volume of the liquid to be measured, low cost, simple and convenient instrument operation, high analysis speed, good accuracy in a certain concentration range and the like, and has wide application prospect.
The invention provides an ultraviolet detection method for rapidly and accurately measuring lead concentration, which comprises the following steps:
(1) Preparation of lead standard solution
Lead standard solutions with the concentration of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L are respectively prepared;
(2) Establishment of a Standard Curve
Respectively taking 1mL of the lead standard solution, sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate (HAC-NaAC) buffer solution, uniformly mixing, and then carrying out ultraviolet absorbance detection at 568nm wavelength to establish a standard curve between absorbance and lead concentration;
(3) Pretreatment of a sample to be tested
Diluting a sample to be tested containing lead with different concentration gradients, determining whether the sample is in the linear range of a regression equation or not by using the method of the step (4) of the invention, and if not, continuing to dilute;
(4) Lead concentration C pb Is measured by (a)
Taking 1mL of the lead-containing sample to be detected treated in the step (3), sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution, uniformly mixing, detecting ultraviolet absorbance at 568nm wavelength, and calculating the concentration of lead through the obtained absorbance and the standard curve obtained in the step (2).
Further, in the step (2), the usage ratio of the lead standard solution to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL, in the step (4), the dosage ratio of the lead sample to be tested to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL.
Further, the concentration of the xylenol orange solution was 1g/L, and the pH of the acetic acid-sodium acetate buffer solution was 6.
Further, in the step (3), the lead-containing sample to be measured is diluted with different concentration gradients, and the concentration of the lead in the diluted lead-containing sample to be measured is in the range of 0-10 mg/L and does not comprise 0.
The invention also provides application of the ultraviolet detection method in quantitative detection of the lead concentration in the water environment.
The technical scheme of the invention is further described by the following examples.
Example 1
The ultraviolet detection method for rapidly and accurately measuring the lead concentration comprises the following steps of:
(1) Preparation of lead standard solution
Lead standard solutions with the concentration of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L are respectively prepared;
(2) Establishment of a Standard Curve
Taking 1mL of the lead standard solution respectively, sequentially adding 1.5mL of deionized water, 0.1mL of 1g/L xylenol orange solution and 0.5mL of acetic acid-sodium acetate (HAC-NaAC) buffer solution with pH of 6, uniformly mixing, detecting ultraviolet absorbance at 568nm wavelength, wherein the ultraviolet absorption spectrum of the lead standard solution with partial concentration is shown in figure 1, the measurement result is shown in table 1, a standard curve is established according to the absorbance and the lead concentration, and the standard curve is shown in figure 2, and the regression equation is y=0.0228x+0.1506, R is shown in the formula 1 2 =0.999, demonstrating that the uv detection method of the present invention is feasible.
Table 1 record of absorbance values for lead standard solutions
(3) Pretreatment of a sample to be tested
Diluting a lead-containing sample to be detected with different concentration gradients, determining whether the lead-containing sample is in the linear range (0-10 mg/L and not including 0) of a regression equation by using the method of the step (4) of the embodiment, and if the lead-containing sample is not in the linear range, continuing to dilute;
(4) Lead concentration C pb Is measured by (a)
Taking 1mL of the lead-containing sample to be detected treated in the step (3), sequentially adding 1.5mL of deionized water, 0.1mL of 1g/L xylenol orange solution and 0.5mL of acetic acid-sodium acetate (HAC-NaAC) buffer solution with pH of 6, uniformly mixing, detecting ultraviolet absorbance at 568nm wavelength, and calculating the concentration of lead according to the obtained absorbance and the standard curve obtained in the step (2).
Example 2
The method for measuring the lead concentration by the ultraviolet spectrophotometry of the embodiment 1 is applied to practice, and in order to explore the migration rule of pollutants in a porous medium, the change of the concentration of free lead with time in a penetration experiment of a column migration test is tested. From one group of free lead column migration experiments, 6 experimental points at different moments are randomly taken, each experimental point is measured by adopting an inductively coupled plasma emission spectrum (ICP-OES) and the ultraviolet detection method of the invention, and the obtained measurement results are shown in Table 2.
Table 2 results of measuring lead concentration in examples and comparative examples
As can be seen from the data in Table 2, the results of the measurement of the lead concentration in the examples of the present invention are not much different from those of the measurement by the ICP-OES method, and thus, it is demonstrated that the ultraviolet detection method of the present invention is reliable.
Application example
The adsorption effect of three different microplastic on lead was tested by the method of example 1 of the present invention under different ionic strengths.
The first step: three microplastic materials (MS, CMS and SMS) were mixed with heavy metal lead to prepare 125mL mixed solutions with ionic strength of 1mM and 100mM, respectively, wherein the microplastic materials had a concentration of 15mg/L and a lead concentration of 10mg/L.
And a second step of: the above mixed solutions were placed in conical flasks, respectively, and pH was adjusted to 6.8.+ -. 0.2 with 0.02M HCl and 0.02M NaOH, sealed with sealing film, and placed in a constant temperature shaker, and subjected to constant temperature shaking at 25℃for 45min at 170 rpm.
And a third step of: 1mL of each sample to be measured was filtered through a 0.22 μm needle filter, and the concentration of free lead was measured in accordance with the method of example 1 of the present invention.
Fourth step: and calculating the adsorption rate under different ionic strengths according to the concentration of the free lead after adsorption and the initial lead concentration, namely the percentage of the total amount of the lead adsorbed by the microplastic in the adsorption time to the initial lead content, wherein the data graph of the adsorption result is shown in figure 3.
As can be seen from fig. 3, the detection method of the present invention can be used for measuring lead concentration before and after adsorption.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (4)
1. An ultraviolet detection method for rapidly and accurately measuring lead concentration is characterized by comprising the following steps:
(1) Preparation of lead standard solution
Lead standard solutions with the concentration of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L are respectively prepared;
(2) Establishment of a Standard Curve
Respectively taking 1mL of the lead standard solution, sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution, uniformly mixing, and then detecting ultraviolet absorbance at 568nm wavelength to establish a standard curve between absorbance and lead concentration;
(3) Pretreatment of a sample to be tested
Diluting a lead-containing sample to be tested with different concentration gradients;
(4) Measurement of lead concentration
Taking 1mL of the lead-containing sample to be detected treated in the step (3), sequentially adding deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution, uniformly mixing, detecting ultraviolet absorbance at 568nm wavelength, and calculating to obtain the concentration of lead through the obtained absorbance and the standard curve obtained in the step (2);
in the step (3), the lead-containing sample to be measured is diluted with different concentration gradients, and the concentration of the lead in the diluted lead-containing sample to be measured is within the range of 0-10 mg/L and does not comprise 0;
the concentration of the xylenol orange solution is 1g/L;
in the step (2), the dosage ratio of the lead standard solution to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL, in the step (4), the dosage ratio of the lead sample to be tested to deionized water, xylenol orange solution and acetic acid-sodium acetate buffer solution is 1mL:1.5mL:0.1mL:0.5mL.
2. The uv assay according to claim 1, wherein the pH of the acetic acid-sodium acetate buffer solution is 6.
3. Use of the ultraviolet detection method according to any one of claims 1-2 for quantitatively detecting lead concentration in an aqueous environment.
4. Use of the ultraviolet detection method according to any one of claims 1-2 for determining the adsorption effect of micro-plastics on lead.
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