CN113092457A - Online accurate detection method suitable for nitrite nitrogen in water body in complex environment - Google Patents
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- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 title claims abstract description 97
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000001514 detection method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 30
- ZCUQOPGIJRGJDA-UHFFFAOYSA-N 1-naphthalen-1-ylethane-1,2-diamine Chemical compound C1=CC=C2C(C(N)CN)=CC=CC2=C1 ZCUQOPGIJRGJDA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000013535 sea water Substances 0.000 claims abstract description 15
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 14
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- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 15
- 229940124530 sulfonamide Drugs 0.000 claims description 15
- 238000011161 development Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 6
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- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
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- G—PHYSICS
- 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
Abstract
The invention discloses an online accurate determination method for nitrite nitrogen content in a water body in a complex environment, belonging to the technical field of water quality monitoring. Nitrite nitrogen is used as a research object, a mathematical model for correcting the spectral absorption coefficient is combined on the basis of a naphthyl ethylenediamine spectrophotometry, and an online accurate detection method for nitrite nitrogen in seawater is established. The influence of the change of the environmental temperature, the pH, the salinity and the turbidity on the measurement result is inspected, and the compensation correction is carried out on the influence of the relevant parameters. The method is used for measuring the actual seawater sample, and is compared and analyzed with the detection result of the national standard method, and the relative error of the two is not more than 4.86 percent. The method is simple and convenient to operate, has good reproducibility, can eliminate the influence caused by environmental factors, and can be used for accurately measuring nitrite nitrogen in seawater on line.
Description
Technical Field
The invention belongs to the technical field of water quality monitoring, and particularly designs an online accurate determination method suitable for nitrite nitrogen content in a complex environment water body.
Background
Nitrite nitrogen is a naturally occurring chemical in the marine environment and is also an important component of the nitrogen cycle. Large amounts of nitrite nitrogen not only disrupt the balance of the nitrogen cycle, but also can be detrimental to human health, for example, leading to methemoglobinemia, congenital defects, and carcinogenesis. Therefore, the accurate detection of the nitrite nitrogen content in seawater is of great importance for environmental management, water quality monitoring and human health.
At present, the measuring methods of nitrite nitrogen reported at home and abroad mainly comprise spectrophotometry, chemiluminescence, chromatography and the like. Among them, the chemiluminescence method is poor in stability and reproducibility. The chromatography not only needs sample pretreatment, but also has complex instrument operation and wastes time and labor. The spectrophotometry has the characteristics of low cost and easy feasibility, thus the method still has a dominant position in a plurality of methods for detecting nitrite and is widely adopted. When measuring nitrite nitrogen in a water sample, Emilio (Emilio garci-Robledo, Alfonso corona, Sokratis paspaspalou. Marine Chemistry, 2014, 162: 30-36) and the like need to establish a standard curve by using a standard solution with similar salinity to the sample to be analyzed, so that accurate data can be obtained, and analysis of a large number of samples is not facilitated. Wang et al (Wang Huihui, Wan Nanwei, Ma Lin, et al. The analysis, 2018, 143(19): 4555-. Therefore, establishing a method for measuring the nitrite nitrogen content in seawater which can inhibit the influence of environmental factors is particularly important.
The method is based on the diazotization-coupling reaction of nitrite nitrogen and sulfanilamide and naphthyl ethylene diamine hydrochloride in a hydrochloric acid medium, and adopts a spectrophotometry to detect nitrite nitrogen in a water sample. The influence of the change of temperature, pH, salinity and turbidity of a water sample on the absorbance value is investigated, and the interference caused by the change of different parameters is compensated and corrected, so that the method for accurately detecting the nitrite nitrogen on line, which can inhibit the influence caused by environmental factors, is established and used for the measurement of actual seawater.
Disclosure of Invention
The invention aims to provide a naphthyl ethylenediamine hydrochloride spectrophotometry, which can eliminate the influence caused by environmental factors by adding a constant temperature device and compensating and correcting the influence of salinity and turbidity, can be used for accurately measuring nitrite nitrogen in seawater on line, has the advantages of simple and convenient operation, good reproducibility and the like, and provides a new method and thought for eliminating the influence of the environmental factors in the seawater on-line detection process.
The method of the invention comprises the following steps:
(1) drawing a nitrite nitrogen standard curve: respectively adding 0-1000 mu L of nitrite nitrogen standard solution into a colorimetric tube with a plug, the content of which in each colorimetric tube with a plug is 50mL, diluting the nitrite nitrogen standard solution in each colorimetric tube with a plug to 50mL by using deionized water, wherein the concentration of the nitrite nitrogen in each colorimetric tube with a plug is 0-100 mu g/L, sequentially adding a sulfanilamide solution and a naphthyl ethylenediamine hydrochloride solution into each colorimetric tube with a plug, oscillating and shaking uniformly to obtain a solution after color development, measuring the absorbance of the nitrite nitrogen at 540nm by adopting a spectrophotometry method, and drawing by taking the concentration as an abscissa and the absorbance as an ordinate to obtain a nitrite nitrogen standard curve.
(2) Taking 800 mu L of nitrite nitrogen standard solution in a 50mL colorimetric tube with a plug, using deionized water to fix the volume to 50mL to obtain nitrite nitrogen solution with the concentration of 80 mu g/L, then adding sulfanilamide solution and naphthyl ethylenediamine hydrochloride solution in sequence, shaking up uniformly to obtain solution after color development, and measuring the nitrite nitrogen absorbance at 540nm by adopting a spectrophotometry.
(3) Adding a constant temperature device in the experimental process according to the step (2), and inspecting the influence of the temperature of 5-30 ℃ on the absorbance of nitrite nitrogen under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L, the salinity is 0 per thousand and the turbidity is 0 NTU; the results show that the absorbance value changes little with increasing temperature and is stabilized at a substantially constant value, indicating that the method of the present invention can suppress the influence of temperature.
(4) According to the step (2), under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L, the salinity is 0 per thousand and the turbidity is 0NTU, the influence of the pH value between 6 and 10 on the nitrite nitrogen absorbance is investigated; the result shows that the absorbance is slightly influenced by the pH, which indicates that the color development system of the method is stable and is not influenced by the pH.
(5) According to the step (2), under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L and the turbidity is 0NTU, the influence of the salinity between 0 and 35 per thousand on the nitrite nitrogen absorbance is inspected; under the condition that the salinity is more than 20 per mill, combiningThe absorbance value and the salt error correction coefficient f =0.0003x at different salinity2-0.0211x +1.2515 and a standard curve model, compensating for the nitrite nitrogen concentration predicted by the model;
(6) according to the step (2), the influence of turbidity between 0 and 120NTU on the nitrite nitrogen absorbance is inspected; under the condition that the turbidity is more than 40NTU, combining absorbance values at different turbidities with a standard curve model, and performing turbidity compensation according to the relation y =0.1162x-2.94 that the variation between the nitrite nitrogen concentration predicted by the model and the real nitrite nitrogen concentration changes along with the turbidity;
(7) filtering an actual seawater sample to be detected by using a filter membrane to obtain a filtered water sample;
(8) taking the filtered water sample obtained in the step (7), and determining the nitrite nitrogen concentration according to the step (2) by adopting the method and the national standard method without adding a nitrite nitrogen standard solution to obtain the determination results of the two methods for comparative analysis; the result shows that the relative error of the two methods is not more than 4.86 percent at most, which shows that the method can well complete the measurement of the nitrite nitrogen content of the actual seawater sample.
In the steps (1) and (2), the concentration of the nitrite nitrogen standard solution is 5mg/L, the concentration of the sulfanilamide solution is 10g/L, and the concentration of the naphthyl ethylene diamine hydrochloride solution is 1 g/L; the addition amount of the sulfanilamide solution and the naphthyl ethylenediamine hydrochloride solution is 1 mL.
In step (7), the filter membrane is a 0.45 μm filter membrane.
The invention has the following remarkable advantages:
(1) the naphthyl ethylenediamine spectrophotometric method has the characteristics of low cost and easy feasibility.
(2) The method can eliminate the influence of environmental factors on the detection result, and can be used for accurately measuring the nitrite nitrogen in the seawater on line.
(3) The invention has simple and convenient operation, easy operation, low requirement on the skill of an analyst, relatively common used instruments and wide popularization and application.
Drawings
FIG. 1 is a graph showing absorption spectra of solutions of nitrite nitrogen of different concentrations in example 1 of the present invention.
FIG. 2 is a graph showing the effect of temperature on nitrite nitrogen absorbance in example 2 of the present invention.
FIG. 3 is a graph showing the effect of pH on nitrite nitrogen absorbance in example 3 of the present invention.
FIG. 4 is a graph showing the effect of salinity on nitrite nitrogen absorbance in example 4 of the present invention.
FIG. 5 shows the salinity compensation results of the nitrite nitrogen solution in example 4 of the present invention.
FIG. 6 is a graph showing the effect of turbidity on nitrite nitrogen solution and offset correction in example 5 of the present invention.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1
Spectrophotometric detection of nitrite nitrogen standard solution
Respectively adding 0, 100, 200, 300, 400, 500, 600, 700, 800, 900 and 1000 mu L of nitrite nitrogen standard solution with the concentration of 5mg/L into a colorimetric tube with a plug with the capacity of 50mL, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen standard solutions with different concentrations, sequentially adding 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L naphthylethylenediamine hydrochloride solution, shaking uniformly, detecting by a spectrophotometry method after the color development is completed to obtain a spectrum after the color development, wherein the product after the color development has the maximum light absorption value at the wavelength of 540nm as shown in figure 1. Measuring the light absorption value of the developed nitrite nitrogen standard solution at the 540nm wavelength by using an absorption spectrogram or by using deionized water as a reference to obtain the light absorption values corresponding to the nitrite nitrogen standard solutions with different concentrations, thereby obtaining a standard working curve of the nitrite nitrogen, wherein R of the standard working curve is2=0.9999。
Example 2
Investigating the influence of temperature on absorbance
Respectively adding 800 mu L of nitrite nitrogen standard solution with the concentration of 5mg/L into a colorimetric tube with a plug with the capacity of 50mL, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen standard solution with the concentration of 80 mu g/L, respectively controlling the temperature of the solution to be between 5 and 30 ℃, sequentially adding 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L of naphthyl ethylenediamine hydrochloride solution, shaking up by shaking, and measuring the absorbance after the color development is completed, wherein the result is shown in figure 2.
Example 3
Investigating the influence of pH on absorbance
Respectively adding 800 mu L of nitrite nitrogen standard solution with the concentration of 5mg/L into a colorimetric tube with a plug with the capacity of 50mL, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen standard solution with the concentration of 80 mu g/L, respectively controlling the pH of the solution to be 6-10, sequentially adding 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L naphthylenediamine hydrochloride solution, shaking up by shaking, and measuring the absorbance after the color development is completed, wherein the result is shown in figure 3.
Example 4
Influence of salinity on absorbance and compensation correction
Respectively adding 800 mu L of nitrite nitrogen standard solution with the concentration of 5mg/L into a colorimetric tube with a plug with the capacity of 50mL, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen standard solution with the concentration of 80 mu g/L, respectively controlling the salinity of the solution to be 0-35 per thousand, sequentially adding 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L naphthylenediamine hydrochloride solution, shaking up, and measuring the absorbance after the color development is completed, wherein the result is shown in figure 4 (a).
As can be seen from FIG. 4 (a), the absorbance change is small when the salinity is lower than 20, and is within the allowable error range; when the salinity is greater than 20, the absorbance value changes to a certain extent, so that the spectral data with the salinity in the range of 20-35 per mill are fitted, and the result is shown in fig. 4 (b).
For seawater sample, if a standard curve is drawn, deionized water is used, then the absorbance A of the water samplewAbsolute analysis of blank absorbance AbThen, the salinity of the measured water sample should be multiplied by the corresponding salt error correction coefficient f (see Table 1), according to f (A)w-Ab) And (4) checking the standard curve to calculate the concentration of nitrite nitrogen in the water sample.
And (4) compensating the nitrite nitrogen concentration predicted by the model by combining the absorbance value and the salt error correction coefficient at different salinity and the standard curve. Before and after the nitrite nitrogen solution with the concentration of 80 mug/L and the salinity of 20, 25, 30 and 35 is subjected to salinity compensation, the results of the real value of the nitrite nitrogen, the predicted value before compensation and the predicted value after compensation are shown in figure 5. As can be seen from the figure 5, the salinity compensation method can effectively inhibit the influence of the salinity of the water sample on the nitrite nitrogen prediction model, and the maximum relative error between the real value and the predicted value does not exceed 2.14%.
Example 5
Influence of turbidity on absorbance and compensation correction
Respectively adding 800 mu L of nitrite nitrogen standard solution with the concentration of 5mg/L into a colorimetric tube with a plug with the capacity of 50mL, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen standard solution with the concentration of 80 mu g/L, respectively controlling the turbidity of the solution to be 0-120 NTU, sequentially adding 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L naphthylenediamine hydrochloride solution, shaking up by shaking, and measuring the absorbance after the color development is completed, wherein the results are shown in Table 2.
As can be seen from Table 2, when the turbidity is less than 40NTU, the absorbance value is basically stabilized at about 0.2025, within the error tolerance range; when the turbidity is greater than 40NTU, the absorbance value changes more, which decreases from 0.2025 to 0.1783 with increasing turbidity, indicating that the effect of turbidity is not negligible. FIG. 6 (a) shows the relationship between the absorbance of a nitrite nitrogen solution having a concentration of 80. mu.g/L and the turbidity at 40 to 120 NTU.
In the experimental process, a nitrite nitrogen standard solution with the concentration of 80 mug/L is selected, an absorbance value with different turbidity is obtained by measuring by adopting a spectrophotometry method, and the relation between the variation of the nitrite nitrogen concentration and the real nitrite nitrogen concentration predicted by a model and the turbidity variation is y =0.1162x-2.94, and R = 0.9997. And then turbidity compensation can be carried out by combining the absorbance values at different turbidity levels and the standard curve model. The effect of the spectral data model of the nitrite nitrogen solution at a concentration of 80. mu.g/L after turbidity compensation is shown in FIG. 6 (b).
The calculation formula of the overall average deviation Bias is shown as the formula (1). Wherein
Is the predicted value of the model;
is a standard value; n is the number of correction samples.
The smaller the overall average deviation Bias value is, the better the compensation effect of the model is, according to fig. 6 (b), the Bias =0.056 μ g/L of the spectrum data model after turbidity compensation is obtained by calculation, and the maximum relative error between the true value and the predicted value is not more than 0.09%. Therefore, the influence of turbidity change on the detection of nitrite nitrogen in a water sample by a spectrophotometry can be well corrected by the turbidity compensation model.
Example 6
In the experiment, Jinjiang seawater is taken as a measuring solution, the volume is fixed to 50mL in a colorimetric tube with a stopper, 1mL of 10g/L sulfanilamide solution and 1mL of 1g/L naphthyl ethylenediamine hydrochloride solution are sequentially added, the mixture is shaken up, the absorbance of the mixture is measured after the mixture is completely developed, and the absorbance is measured in parallel for 6 times, so that the result shows that the detection limit of the method is 2.28 mug/L, and the relative standard deviation is 1.26% (n = 6).
The above description is an exemplary embodiment of the present invention, but the present invention should not be limited to the disclosure of the embodiment. Therefore, it is intended that all equivalents and modifications which do not depart from the spirit of the invention disclosed herein are deemed to be within the scope of the invention.
Claims (4)
1. An online accurate detection method for nitrite nitrogen in a water body in a complex environment is characterized by comprising the following steps: the nitrite nitrogen standard solution is used as a research object, a naphthylethylenediamine hydrochloride spectrophotometry is adopted, and a spectral absorption coefficient correction mathematical model is combined to establish the on-line accurate detection method for nitrite nitrogen in seawater, which can inhibit the influence of environmental factors.
2. The method of claim 1, wherein: the method comprises the following specific steps:
(1) drawing a nitrite nitrogen standard curve: respectively adding 0-1000 mu L of nitrite nitrogen standard solution into a colorimetric tube with a plug, the capacity of which is 50mL, diluting the nitrite nitrogen standard solution in each colorimetric tube with the plug to 50mL by using deionized water, enabling the nitrite nitrogen concentration in the colorimetric tube with the plug to be 0-100 mu g/L, sequentially adding a sulfanilamide solution and a naphthyl ethylenediamine hydrochloride solution into each colorimetric tube with the plug, shaking uniformly to obtain a solution after color development, measuring the absorbance of the nitrite nitrogen at 540nm by adopting a spectrophotometry method, and drawing a nitrite nitrogen standard curve by taking the concentration as an abscissa and the absorbance as an ordinate;
(2) putting 800 mu L of nitrite nitrogen standard solution into a 50mL colorimetric tube with a plug, fixing the volume to 50mL by using deionized water to obtain nitrite nitrogen solution with the concentration of 80 mu g/L, then sequentially adding sulfanilamide solution and naphthyl ethylenediamine hydrochloride solution, shaking uniformly to obtain solution after color development, and measuring the nitrite nitrogen absorbance at 540nm by adopting a spectrophotometry;
(3) adding a constant temperature device in the experimental process of the step (2), and inspecting the influence of the temperature between 5 and 30 ℃ on the absorbance of the nitrite nitrogen under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L, the salinity is 0 per thousand and the turbidity is 0 NTU;
(4) according to the step (2), under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L, the salinity is 0 per thousand and the turbidity is 0NTU, the influence of the pH value between 6 and 10 on the nitrite nitrogen absorbance is inspected;
(5) according to the step (2), under the conditions that the concentration of the nitrite nitrogen solution is 80 mug/L and the turbidity is 0NTU, the influence of the salinity between 0 and 35 per thousand on the nitrite nitrogen absorbance is inspected; under the condition that the salinity is more than 20 per mill, combiningThe absorbance value and the salt error correction coefficient f =0.0003x at different salinity2-0.0211x +1.2515 and a standard curve model, compensating for the nitrite nitrogen concentration predicted by the model;
(6) according to the step (2), the influence of turbidity between 0 and 120NTU on nitrite nitrogen absorbance is inspected; under the condition that the turbidity is more than 40NTU, combining absorbance values at different turbidities with a standard curve model, and performing turbidity compensation according to the relation y =0.1162x-2.94 that the variation between the nitrite nitrogen concentration predicted by the model and the real nitrite nitrogen concentration changes along with the turbidity;
(7) filtering an actual seawater sample to be detected by using a filter membrane to obtain a filtered water sample;
(8) and (3) taking the water sample filtered in the step (7), and determining the nitrite nitrogen concentration according to the step (2) without adding a nitrite nitrogen standard solution.
3. The method of claim 1, wherein: in the steps (1) and (2), the concentration of the nitrite nitrogen standard solution is 5mg/L, the concentration of the sulfanilamide solution is 10g/L, and the concentration of the naphthyl ethylene diamine hydrochloride solution is 1 g/L; the addition amount of the sulfanilamide solution and the naphthyl ethylenediamine hydrochloride solution is 1 mL.
4. The method of claim 1, wherein: in step (7), the filter membrane is a 0.45 μm filter membrane.
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| CN115452751A (en) * | 2022-10-26 | 2022-12-09 | 杭州泽天春来科技有限公司 | Residual chlorine detection method and device |
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| 中华人民共和国国家质量监督检验检疫总局中国国家标准化管理委员会: "《中华人民共和国国家标准 海洋监测规范 第4部分：海水分析》", 18 October 2007 * |
Cited By (4)
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| CN114235730A (en) * | 2022-02-21 | 2022-03-25 | 中国科学院烟台海岸带研究所 | Seawater nutrient salt online monitoring system and seawater nutrient salt detection method |
| CN115839925A (en) * | 2022-02-21 | 2023-03-24 | 中国科学院烟台海岸带研究所 | Seawater nutrient salt online monitoring system and seawater nutrient salt detection method |
| CN115452751A (en) * | 2022-10-26 | 2022-12-09 | 杭州泽天春来科技有限公司 | Residual chlorine detection method and device |
| CN115452751B (en) * | 2022-10-26 | 2023-03-10 | 杭州泽天春来科技有限公司 | Residual chlorine detection method and device |
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| CN113092457B (en) | 2022-03-22 |
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