CN120161001A - Method and application of quantification of free chlorine in water based on UV-visible absorption spectroscopy - Google Patents
Method and application of quantification of free chlorine in water based on UV-visible absorption spectroscopy Download PDFInfo
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Abstract
本发明公开了一种基于紫外‑可见吸收光谱定量水体中游离氯的方法及应用，属于水质检测技术领域，所述方法包括：采集目标水样，进行氯化处理后，检测获得pH值、游离氯浓度和氯化光谱数据；根据氯化光谱数据计算背景天然有机物的基线；根据背景天然有机物的基线计算获得氯化过程中次氯酸根离子的吸光度变化量；使用次氯酸根离子的吸光度变化量和光谱参数计算获得次氯酸根浓度；结合目标水样pH值与次氯酸根浓度计算获得水体中游离氯浓度。本发明能够弥补在线紫外光谱仪在游离氯浓度检测上的不足，并且显著提升了实时监测的便捷性。
The present invention discloses a method and application for quantitatively measuring free chlorine in water based on ultraviolet-visible absorption spectrum, which belongs to the technical field of water quality detection. The method comprises: collecting a target water sample, performing chlorination treatment, detecting and obtaining pH value, free chlorine concentration and chlorination spectrum data; calculating the baseline of background natural organic matter according to the chlorination spectrum data; calculating the absorbance change of hypochlorite ions during chlorination according to the baseline of background natural organic matter; calculating the hypochlorite concentration using the absorbance change of hypochlorite ions and spectral parameters; and calculating and obtaining the free chlorine concentration in the water body in combination with the target water sample pH value and hypochlorite concentration. The present invention can make up for the deficiency of online ultraviolet spectrometer in free chlorine concentration detection, and significantly improve the convenience of real-time monitoring.
Description
Technical Field
The application relates to the technical field of water quality detection, in particular to a method for quantifying free chlorine in a water body based on ultraviolet-visible absorption spectrum and application thereof.
Background
In the drinking water treatment process, the disinfection link is of great importance, the threat to health caused by the disease transmission of drinking water is obviously reduced by effectively inactivating pathogenic microorganisms in the water, and the chlorine disinfection is widely applied in the global scope due to the low cost and the continuous oxidation disinfection capability.
However, it should be noted that excessive addition of chlorine-containing disinfectant will cause the concentration of free chlorine in water to exceed the standard, and at the same time, the chlorine-containing disinfectant can react with natural organic matters (Natural organic matter, NOM) to generate Disinfection Byproducts (DBPs) such as Trihalomethanes (THMs), haloacetic acids (HAAs), haloacetonitrile (HANs) and the like with toxicological risks. According to the current sanitary standards for drinking water (GB 5749-2022), when liquid chlorine, sodium hypochlorite or calcium hypochlorite is used for disinfection, the free chlorine balance of the factory water should be controlled between 0.3 and 2 mg/L. Based on the method, a real-time monitoring system of the concentration of free chlorine is constructed in the disinfection process of the water purification plant, and the accurate regulation and control of the dosage of the disinfectant is a key control link for guaranteeing the chemical safety and biological safety of the drinking water.
The existing free chlorine detection method is mainly divided into an electrode method and a traditional chemical method. However, the electrode method requires frequent calibration, and electrodes of different materials are required for detecting different indexes. Traditional chemical methods include titration and spectrophotometry (N, N-diethyl-1, 4-phenylenediamine spectrophotometry, DPD), but both require the addition of buffer solution and DPD reagents to the sample to be tested, and the addition of chemical reagents breaks down the water sample and fails to allow in situ detection. The use of an ultraviolet spectrophotometer only realizes in-situ detection of pure substances of sodium hypochlorite, which cannot be realized in a complex system containing NOM such as a natural water sample.
Therefore, there is a need for a method that can detect free chlorine in natural water samples without the addition of chemical reagents.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the method for compensating the defects of the online ultraviolet spectrometer in free chlorine concentration detection, and the convenience of real-time monitoring is remarkably improved.
The invention adopts the following technical scheme.
The invention discloses a method for quantifying free chlorine in a water body based on ultraviolet-visible absorption spectrum, which comprises the following steps:
collecting a target water sample, performing chlorination treatment, and detecting to obtain pH value and spectrum data;
Calculating a baseline of NOM absorbance background in the water body according to the spectrum data;
obtaining the absorbance change quantity of hypochlorite ions in the chlorination process according to the baseline calculation of the background NOM;
Calculating to obtain hypochlorite concentration by using the absorbance variation of hypochlorite ions and spectral parameters;
And calculating the concentration of free chlorine in the water body by combining the pH value of the target water sample and the concentration of hypochlorite.
Preferably, the chlorination treatment is to add sodium hypochlorite to the target water sample, and when the amount of sodium hypochlorite added is zero, the measured spectrum data is the spectrum data of raw water.
Preferably, the detection wavelength range of the spectrum data is 200-600 nm.
Preferably, the spectral data comprises absorbance: A 200~A600;
And calculating the logarithmic absorbance corresponding to the set wavelength according to the obtained spectrum data, wherein the logarithmic absorbance is lnA 200~lnA600.
Preferably, the baseline for calculating NOM absorbance background in the water body according to the spectrum data is:
Calculation of NOM absorbance background Using (1) ;
The saidThe slope of any interval in the wave band of 250-500 nm.
Preferably, the set wavelength is calculated using equation (2)Logarithmic absorbance values for background NOM;
The set wavelengthIs any value within the interval of 250-380 nm;
In the formula, For the calculated NOMThe logarithmic absorbance value at which the light is absorbed,Is the log spectrum after chlorination~The slope between the two points is such that,AndRespectively isAndLog absorbance at two wavelengths.
Preferably, the absorbance change amount of hypochlorite ions in the chlorination process according to the baseline calculation of NOM absorbance background in the water body is:
calculation of hypochlorite ion in Chlorination Using (3) Absorbance change at;
In the formula,In the presence of hypochlorite ionsAbsorbance change at that point.
Preferably, the calculating the hypochlorite concentration using the absorbance variation and the spectral parameters of the hypochlorite ion includes:
The hypochlorite concentration was calculated using formula (4):
wherein: The concentration was calculated for the hypochlorite ion, Is of different water samplesAnd b is the intercept of different water samples after correction.
Preferably, the concentration of free chlorine in the water body obtained by combining the pH value of the target water sample with the hypochlorite concentration is calculated as follows:
the free chlorine concentration was calculated using formula (5):
In the formula, In order to calculate the concentration of free chlorine,The pH value of the water sample is set,Is the ionization constant of hypochlorous acid.
The second aspect of the invention discloses the application of the method for quantifying free chlorine in a water body based on ultraviolet-visible absorption spectrum in measuring the free chlorine in the water body.
Compared with the prior art, the invention has the beneficial effects that at least:
the method adopts ultraviolet-visible absorption spectrum technology, and can calculate the concentration of free chlorine through the spectrum analysis operation of ultraviolet-visible absorption spectrum by analyzing the chloridized spectrum of the water sample and combining the pH value without adding any chemical reagent.
Compared with an electrochemical method, the method has the advantages that the electrode passivation does not need to be worried about, the electrode does not need to be corrected frequently, and the interference of other substances capable of generating redox current on the electrode detection does not need to be considered.
For the titration method (and the HJ 586-2010 national standard DPD spectrophotometry), the method has the advantages that interference of other substances with oxidability on experimental results is not required to be considered, secondary pollution to a water sample is not required to be caused by using chemical reagents, and the detection speed is higher.
The method can be used for detecting whether the concentration of free chlorine in factory water after disinfection is in the national standard range or not in a water supply plant, and can also be used on an online ultraviolet water quality detector to supplement water quality indexes detectable by the existing online ultraviolet water quality detector, so as to realize in-situ detection of various water quality indexes integrated with one instrument.
Drawings
FIG. 1 logarithmic absorbance values for background NOM at 292 nm;
FIG. 2-ten water samples each with R2 greater than 0.98 calculated as the relationship between free chlorine concentration and actual free chlorine concentration.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. The described embodiments of the application are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art without inventive faculty, are within the scope of the application, based on the spirit of the application.
Due to interference of soluble organic matters (NOM) and inorganic ions (NO 3-、NO2- and the like) in natural water, the traditional free chlorine detection method (DPD spectrophotometry) needs to be added with chemical reagents for color development. The research provides a novel method for quantitatively detecting the concentration of free chlorine in water body by utilizing ultraviolet-visible absorption spectrum without a reagent. The inventors noted that the hypochlorite concentration in pure water has a significant linear relationship with the absorption intensity of the spectrum at 292 nm (R 2. Gtoreq.0.99), but the absorption intensity of the spectrum at 292 nm in natural water changes with both hypochlorite concentration and NOM oxidation.
In order to eliminate the spectral interference of NOM absorbance background in water to free chlorine, the inventor establishes a model for linearly calculating NOM absorbance background baseline in water based on 260 nm-360 nm logarithmic spectrum, and establishes a quantitative relation between spectral characteristics and free chlorine concentration by combining pH and hypochlorous acid ionization constant (Ka).
The result shows that the novel method realizes unified measurement of free chlorine after 10 water sources are disinfected, the correlation coefficient (R2) of the concentration of the free chlorine can reach 0.98, and the average absolute percentage error (MAPE) is 23.7%. The method provides a new means for water quality monitoring with no need of chemical reagent, high convenience and high reliability. In engineering application, the method can be used for detecting the free chlorine in factory water of an intelligent water plant, simplifies the step of detecting the free chlorine by the existing spectrophotometry, realizes in-situ detection without adding chemical reagents, and facilitates real-time on-line monitoring of the concentration index of the free chlorine. Meanwhile, in the aspect of instruments, the problem that the existing online ultraviolet-visible water spectrometer cannot directly measure the concentration of free chlorine in water is solved, so that the water quality detection index range of an online ultraviolet-visible absorption spectrum is further expanded, the integration level of equipment is higher, energy is saved, and one spectrum is further promoted to detect various data.
The embodiment 1 of the invention provides a method for quantifying free chlorine in a water body based on ultraviolet-visible absorption spectrum, which comprises the following steps:
Step 1, collecting water samples in different areas, detecting an absorption spectrum under a set wavelength after chloridizing treatment, and obtaining spectrum data;
Preferably, all water samples are transported to the laboratory in high density polyethylene or polypropylene containers, and after arrival, the samples are filtered through a 0.45 μm aqueous filter and then stored at 4 ℃.
Preparing free chlorine solution with the same volume according to the set concentration by the water sample, respectively adding 250 ml water samples into 8 brown glass bottles, sequentially adding sodium hypochlorite with different amounts to ensure that the initial free chlorine concentration of each bottle reaches 0, 1.1, 2.2, 3.3, 4.4, 5.5, 6.6 and 7.7 mg/L (calculated by Cl 2), and carrying out light-shielding reaction for 30 minutes under the condition of 20 ℃ and then carrying out the following measurement;
step 1.1, measuring the pH value, namely measuring the pH value of the chlorinated water sample by using a pH meter (Mettler Toledo S210 Seven Compact);
step 1.2, measuring the concentration of free chlorine, namely measuring the concentration of free chlorine in a water sample by adopting a method of measuring the free chlorine and the total chlorine of water quality by using an N, N-diethyl-1, 4-phenylenediamine spectrophotometry (HJ 586-2010);
And step 1.3, measuring a spectrum, namely taking a proper amount of chlorinated water sample, and scanning an ultraviolet-visible absorption spectrum of the chlorinated water sample within a wavelength range of 200-600 nm by using an ultraviolet-visible spectrophotometer (PERKINELMER LAMBDA and 950), so as to obtain spectrum data.
Step 2, according to the chlorination spectrum obtained in the step 1, the absorbance of the water sample can be obtained, and the corresponding logarithmic absorbance can be calculated;
Specifically, the required chlorination spectral data are:
absorbance A 200~A600;
logarithmic absorbance lnA 200~lnA600.
When the addition amount of sodium hypochlorite in step 1 was 0 mg/L (calculated as Cl 2), the absorbance was measured as the spectrum data of raw water.
Step 3, calculating a baseline of NOM absorbance background according to the chlorination spectrum data in the step 2;
NOM absorbance background baseline slope: ;
The said ~Is any interval of 250-500 nm wave bands.
Since there is no interference of inorganic ions after 250 nm, only the absorption of organic matters except hypochlorite is theoretically achieved, but when the wavelength is too large (more than 400 nm), spectrum calculation errors are easily caused due to the fact that the absorbance signal is relatively low, so that in the preferred but non-limiting embodiment of the invention,~The preferable range of (2) is 260-360 nm.
Background NOM at a set wavelengthAbsorbance of (c):
since the absorption peak center of hypochlorite is at A 292 and the band is affected by NOM absorbance only, the wavelength Preferably 292 nm.
Step 4, calculating the absorbance change amount of hypochlorite ions in the chlorination process according to the baseline of the NOM absorbance background in the step 3;
Hypochlorite ion in Absorbance change at;
Step 5, usingAnd spectral parameters calculate hypochlorite concentration;
The inventor carries out multiple linear regression analysis on the spectral parameters of water samples in different areas, obtains a correction parameter b after data fitting and screening, and the intercept correction coefficient b is caused by different water samples The intercept difference between the hypochlorite concentration and the corresponding hypochlorite concentration linear relation is large, so fitting correction is carried out, and a general formula for calculating the hypochlorite concentration is obtained, wherein the general formula is expressed by C ClO - =×+b;
Is of different water samplesAverage value of slope of linear relation between value and hypochlorite concentration of water sampleThe slope is similar to the slope of the linear relation of hypochlorite concentration, so the average value is taken.
And 6, calculating the concentration of free chlorine in the water body by combining the pH value.
Calculating a free chlorine concentration formula:。
wherein: In order to calculate the concentration of free chlorine, The pH value of the water sample is set,Is the ionization constant of hypochlorous acid.
Aiming at the problem that the absorbance of hypochlorite ions at 292 nm is interfered by the absorption spectrum of Natural Organic Matters (NOM) in an actual water body, the slope of a wave band of 260-360 nm of the logarithmic absorption spectrum is adopted to estimate the background absorbance of NOM in the chlorination process, and a ClO-concentration quantitative model (R2 is more than or equal to 0.99) based on an absorbance difference algorithm at 292 nm is constructed. And combining the pH value of the water sample, and finally realizing quantitative calculation of the concentration of free chlorine in the water body by utilizing an ultraviolet-visible absorption spectrometry.
When the detection is carried out on a single water sample, the concentration of free chlorine measured by a national standard method can be converted into the concentration of hypochlorite ions according to a free chlorine concentration formula, so that the slope k and intercept value b of the water sample are obtained. Meanwhile, for convenience of use, the inventor also uses a multi-linear fitting method to fit an intercept correction coefficient b according to spectrum parameters, gives an average slope value k according to experimental results, and calculates the free chlorine concentration.
The nest lake water sample is taken as a further explanation of the specific embodiment of the invention.
Step 1, respectively adding 250 ml water samples into 8 glass bottles, and then respectively adding a proper amount of sodium hypochlorite standard solution to ensure that the initial free chlorine concentration of each bottle reaches 0, 1.1, 2.2, 3.3, 4.4, 5.5, 6.6 and 7.7 mg/L (calculated by Cl 2);
after 30 minutes of chlorination, the water samples in each reaction bottle are sequentially subjected to detection of the following indexes:
Detecting the pH value by using a pH meter;
The concentration of free chlorine was measured using the method of "determination of free chlorine and total chlorine in Water quality" method of spectrophotometry of N, N-diethyl-1, 4-phenylenediamine (HJ 586-2010);
the chlorination spectrum (scanning range is 200-600 nm; step size 1 nm) is scanned by using an ultraviolet-visible spectrophotometer.
Step 2, calculating corresponding logarithmic absorbance (lnA 200~lnA600) according to the absorbance (A 200~A600) measured by each water sample;
Step 3, calculating three logarithmic spectrum slopes by using the formula (1): 、 S 260~360 represents the spectral parameters of raw water, i.e. the spectrum of a water sample without chlorination, i.e. the point where the chlorine addition is 0.
Wherein the method comprises the steps ofIs the logarithmic spectrum slope of 275-295 nm of the raw water,Is the logarithmic spectrum slope of the raw water at 380-443 nm, S260-360 is the absorbance of the background NOM, and the logarithmic value of the NOM absorbance background at 292 nm is calculated by using the formula (2)。
When determining the range of NOM absorbance background baselines in the logarithmic spectrum, in order to avoid the influence of inorganic ions such as nitrate, nitrite and the like with the wavelength less than 250 nm on the spectrum, and simultaneously ensure that the absorbance in the research range is dominated by background NOM, the starting wavelength is selected to be 260 nm, and in consideration of the fact that the absorbance of a water sample after chlorination can be greatly reduced, in order to ensure the reliability of the detection value of an instrument, the ending wavelength is taken to be 360 nm.
As shown in fig. 1, the log spectrum of the water sample from the nest lake after chlorination treatment is shown. As can be seen, during chlorination, the absorption peak formed by excess hypochlorite ions interferes with the linearity of the log spectrum, forming a distinct bulge at 292 nm. Therefore, to achieve direct determination of free chlorine based on uv-vis absorption spectroscopy, the interference of NOM on hypochlorite absorption spectrum needs to be subtracted.
The method comprises the following specific steps:
Firstly, calculating the slope of a wave band of 260-360 nm (S260-360) by adopting a formula (1), wherein the slope of the wave band represents the absorption characteristic of a background NOM in a specific wavelength interval and is used as a baseline of an NOM absorption spectrum, and then, calculating the logarithmic absorbance theoretical value of the NOM at 292 nm after chlorination by using a formula (2).
In the formula,For the calculated log absorbance of background NOM at 292 nm, S 260~360 is the slope between the two points of post-chlorination log spectra 260 nm and 360 nm, lnA 260 and lnA 360 are the log values of absorbance at two wavelengths 260 nm and 360 nm, respectively.
Step 4, calculating the absorbance change of hypochlorite ion at 292 nm in the chlorination process by using formula (3);
In the formula,Is the change in absorbance of hypochlorite ion at 292 nm.
Specifically, the inventors collected 10 regional water samples, respectively, a river water sample (Beijing city Kunying river; beijing city Change river), a canal water sample (Beijing city Yongding canal; beijing city Beijing dense canal), a lake water sample (Anhui province nest lake; beijing city sea lake; beijing city lotus pool), a subsurface water sample (Beijing city famous lake), a regenerated water sample (Beijing city Qinghai river; beijing city Mo Quanhe), measured its chlorination spectrum data, and calculated using (3)The absorbance change amount and the hypochlorite concentration have obvious positive correlation with the measured concentration relation of the hypochlorite.
Step 5, carrying out algorithm optimization value to obtain the calculated hypochlorite concentration;
Because of different water samples The intercept difference of the linear relation with the corresponding hypochlorite concentration is too large, so that the corrected intercept b needs to be corrected by fittingThe slope is similar to the slope of the linear relationship between the hypochlorite concentration and the slope of the linear relationship, so that the average value is taken.
Obtaining a correction intercept b using equation (4);
Calculating hypochlorite concentration by using a formula (5) (wherein the calculation result of the correction intercept b of the nest lake water sample is-1.41);
wherein: The concentration was calculated for the hypochlorite ion, 、、、All are raw water spectrum parameters, b is the corrected intercept of the nest lake water sample, 614.53 is 10 water samplesAverage value of slope values of linear relationship of value and hypochlorite concentration.
The algorithm is optimized because the intercept of the linear equation between hypochlorite concentration values and different water samples is different, so that the intercept is corrected by using spectral parameters for the universality of the formula. The method uses the general formula for obtaining the spectrum data of 10 water samples, and b is a correction parameter obtained by performing data fitting on the spectrum parameters.
Step 6, calculating the concentration of free chlorine by using the formula (6) in combination with the pH value;
wherein: In order to calculate the concentration of free chlorine, The pH value of the water sample is set,The ionization constant of hypochlorous acid (2.9X10 -8 at 20 ℃).
Notably, in aqueous solutions, free chlorine exists in the form of hypochlorous acid (HClO), hypochlorite ions (ClO -) and elemental chlorine in dissolved form (Cl 2), the three morphological distributions being affected by pH. Under the condition that the pH value of the natural water body is usually 6.5-8.5, hypochlorous acid and hypochlorite ions are the main existence forms of free chlorine, so that the concentration of the free chlorine (namely the sum of the concentration of HClO and the concentration of ClO -) can be calculated by using the concentration of ClO - according to the formula (6).
The detailed calculation data of the nest lake water sample are shown in the following table:
wherein for the point where the back calculated free chlorine concentration is less than zero, it is considered that the calculated free chlorine concentration is 0.
The relationship between the calculated free chlorine and the measured free chlorine of the final 10 water samples is shown in fig. 2, and it can be seen that the final calculated model of the ultraviolet-visible absorption spectrum free chlorine concentration has good fitting degree (R 2 =0.98, mape=23.7%).
Example 2 of the present invention provides the use of a method for quantifying free chlorine in a body of water based on ultraviolet-visible absorption spectroscopy according to the above.
Compared with the prior art, the invention has the beneficial effects that at least:
the method adopts ultraviolet-visible absorption spectrum technology, and can calculate the concentration of free chlorine through the spectrum analysis operation of ultraviolet-visible absorption spectrum by analyzing the chloridized spectrum of the water sample and combining the pH value without adding any chemical reagent.
Compared with an electrochemical method, the method has the advantages that the electrode passivation does not need to be worried about, the electrode does not need to be corrected frequently, and the interference of other substances capable of generating redox current on the electrode detection does not need to be considered.
For the titration method (and the HJ 586-2010 national standard DPD spectrophotometry), the method has the advantages that interference of other substances with oxidability on experimental results is not required to be considered, secondary pollution to a water sample is not required to be caused by using chemical reagents, and the detection speed is higher.
The method can be used for detecting whether the concentration of free chlorine in factory water after disinfection is in the national standard range or not in a water supply plant, and can also be used on an online ultraviolet water quality detector to supplement water quality indexes detectable by the existing online ultraviolet water quality detector, so as to realize in-situ detection of various water quality indexes integrated with one instrument.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made to the specific embodiments of the present invention without departing from the spirit and scope of the present invention, and any modifications and equivalents are intended to be included in the scope of the claims of the present invention.
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