CN110596024A - Turbidity compensation method for automatic online total nitrogen monitoring and total nitrogen monitoring method - Google Patents

Turbidity compensation method for automatic online total nitrogen monitoring and total nitrogen monitoring method Download PDF

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Publication number
CN110596024A
CN110596024A CN201910896364.5A CN201910896364A CN110596024A CN 110596024 A CN110596024 A CN 110596024A CN 201910896364 A CN201910896364 A CN 201910896364A CN 110596024 A CN110596024 A CN 110596024A
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China
Prior art keywords
absorbance
total nitrogen
water sample
turbidity
digestion treatment
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Inventor
李满园
戈燕红
谢广群
王青青
郭德音
王坤
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Guangdong Yingfeng Technology Co Ltd
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Guangdong Yingfeng Technology Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/12Circuits of general importance; Signal processing
    • G01N2201/127Calibration; base line adjustment; drift compensation

Abstract

The invention discloses a turbidity compensation method for automatic online monitoring of total nitrogen and a total nitrogen monitoring method, and relates to the technical field of water quality monitoring. The turbidity compensation method comprises the following steps: carrying out first digestion treatment on the water sample, and measuring the first absorbance of the water sample subjected to the first digestion treatment; judging whether the first absorbance meets the total nitrogen turbidity compensation condition, if so, performing second digestion treatment on the water sample, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample; and if not, taking the first absorbance as the absorbance of the water sample. The turbidity condition of the water sample can be automatically determined by judging whether the first absorbance meets the total nitrogen turbidity compensation condition or not, so that the turbidity compensation is performed pertinently, the interference of the water turbidity to the total nitrogen test is solved, the soluble organic matters in the water sample are reserved, and the test precision of the total nitrogen and the soluble organic matters of the water sample is ensured.

Description

Turbidity compensation method for automatic online total nitrogen monitoring and total nitrogen monitoring method
Technical Field
The invention relates to the technical field of water quality monitoring, in particular to a turbidity compensation method and a total nitrogen monitoring method for automatic online monitoring of total nitrogen.
Background
Total nitrogen refers to the sum of dissolved nitrogen in the sample and nitrogen in the suspended matter, including nitrite nitrogen, nitrate nitrogen, inorganic ammonium salts, dissolved ammonia and nitrogen in most organic nitrogen compounds. Total nitrogen is one of important indexes of water quality monitoring, and common testing methods of automatic online total nitrogen monitoring equipment mainly comprise an alkaline potassium persulfate digestion ultraviolet spectrophotometry, a gas phase molecular absorption spectrometry and the like at present. The most common on-line monitoring devices in the market are spectrophotometric methods, which are suitable for the determination of total nitrogen in surface water, groundwater, industrial wastewater and domestic sewage.
In recent years, the quality of surface water is more complex, and the influence of the turbidity of the water body on the testing precision of the automatic online total nitrogen monitoring equipment is more and more large, so that the research of the automatic online total nitrogen monitoring equipment with the turbidity interference resistance is urgently needed by the current market.
Aiming at a water sample with larger turbidity, the interference of turbidity is reduced by adopting standing and filtering means when the total nitrogen content is manually tested in a laboratory; the automatic on-line monitoring equipment for total nitrogen sold in the market mostly adopts the light path with the wavelength of 700nm added to compensate turbidity, and although the method can effectively solve the problem of turbidity interference, the method abandons the influence of soluble organic matters on the total nitrogen test and greatly reduces the test precision of water samples with more soluble organic matters.
Disclosure of Invention
The invention aims to solve the technical problems that the interference of the water turbidity on the total nitrogen test is solved, the water total nitrogen test precision with more soluble organic matter content is ensured, a turbidity compensation method for monitoring the total nitrogen is provided, and a monitoring method capable of automatically judging whether to carry out the total nitrogen turbidity compensation according to the condition of the water turbidity is provided.
In order to solve the above problems, the present invention proposes the following technical solutions:
in a first aspect, the present invention provides a turbidity compensation method for automatic online total nitrogen monitoring, comprising the following steps:
carrying out first digestion treatment on the water sample, and measuring the first absorbance of the water sample subjected to the first digestion treatment;
judging whether the first absorbance meets the total nitrogen turbidity compensation condition, if so, performing second digestion treatment on the water sample, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample;
and if not, taking the first absorbance as the absorbance of the water sample.
The method for judging whether the first absorbance meets the total nitrogen turbidity compensation condition specifically comprises the following steps:
determining A of the first absorbance275Whether the content is more than or equal to 0.1;
determining A of the first absorbance275/A220Whether the content is more than or equal to 15 percent or not;
if A of said first absorbance275Not less than 0.1 or A of the first absorbance275/A220And if the total nitrogen turbidity compensation condition is not less than 15%, judging that the first absorbance meets the total nitrogen turbidity compensation condition.
The further technical scheme is that the first digestion treatment step specifically comprises the following steps:
adding an oxidant and an alkali liquor with preset volumes into a water sample, fully and uniformly mixing, and digesting for 30-40min at the temperature of 120-; after digestion, adding acid liquor until the pH value of the water sample is less than 7, and fully and uniformly mixing.
The further technical scheme is that the oxidant is potassium persulfate solution with the concentration of 10-20 g/L;
the alkali liquor is sodium hydroxide solution, and the concentration is 10-25 g/L;
the acid solution is hydrochloric acid solution with the concentration of 1+ 9.
The further technical scheme is that the second digestion treatment step specifically comprises the following steps:
and heating and digesting the water sample subjected to the first digestion treatment at the temperature of 80-125 ℃ for 5-15 min.
In a second aspect, the present invention provides a total nitrogen automatic online monitoring method, including the turbidity compensation method for total nitrogen automatic online monitoring according to the first aspect, further including:
measuring the absorbance of the reference solution;
and determining the total nitrogen of the water sample according to the absorbance of the water sample and the absorbance of the reference solution.
The technical scheme is that the reference solution is distilled water.
Compared with the prior art, the invention can achieve the following technical effects:
the method determines the turbidity condition of the water sample by judging whether the first absorbance of the water sample subjected to the first digestion treatment meets the total nitrogen turbidity compensation condition or not, so as to judge whether the total nitrogen turbidity compensation is performed or not, can solve the interference of the water turbidity on the total nitrogen test for the water sample with high water turbidity through the previous and subsequent digestion treatments, reserves the soluble organic matters in the water sample, and ensures the test precision of the total nitrogen and the soluble organic matters in the water sample. The turbidity compensation method for automatic on-line monitoring of total nitrogen and the total nitrogen monitoring method provided by the invention can be used for monitoring the total nitrogen only by optimizing the test flow on the existing total nitrogen on-line monitoring equipment and ensuring that the equipment runs stably.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a flowchart of a total nitrogen monitoring method according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, wherein like reference numerals represent like elements in the drawings. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The embodiment of the invention provides a turbidity compensation method for automatic online monitoring of total nitrogen, which comprises the following steps:
carrying out first digestion treatment on the water sample, and measuring the first absorbance of the water sample subjected to the first digestion treatment;
judging whether the first absorbance meets the total nitrogen turbidity compensation condition, if so, performing second digestion treatment on the water sample, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample;
and if not, taking the first absorbance as the absorbance of the water sample.
For a water sample with high water turbidity, the interference of the water turbidity on the total nitrogen test can be effectively solved through the digestion treatment twice, and the soluble organic matters in the water sample are reserved, so that the test precision of the total nitrogen and the soluble organic matters of the water sample is ensured; for a water sample with low turbidity, only the first digestion treatment is needed.
The first absorbance refers to the absorbance A at the wavelengths of 220nm and 275nm after the water sample is subjected to the first digestion treatment220、A275
The second absorbance is the absorbance A 'at the wavelengths of 220nm and 275nm after the water sample is subjected to the second digestion treatment'220、A’275
In a specific implementation, the determining whether the first absorbance meets a total nitrogen turbidity compensation condition specifically includes:
determining A of the first absorbance275Whether the content is more than or equal to 0.1;
determining A of the first absorbance275/A220Whether the content is more than or equal to 15 percent or not;
if A of said first absorbance275Not less than 0.1 or A of the first absorbance275/A220And if the total nitrogen turbidity compensation condition is not less than 15%, judging that the first absorbance meets the total nitrogen turbidity compensation condition.
In the ultraviolet spectrophotometry measurement of the total nitrogen, the total nitrogen content is related to the absorbance of a water sample at the wavelengths of 220nm and 275nm, the absorbance value is related to the turbidity of the water sample, and the turbidity condition of the water sample can be determined by judging whether the first absorbance meets the total nitrogen turbidity compensation condition, so that whether the total nitrogen turbidity compensation is needed or not is judged.
In a specific implementation, the first digestion treatment step specifically includes:
adding an oxidant and an alkali liquor with preset volumes into a water sample, fully and uniformly mixing, and digesting for 30-40min at the temperature of 120-; after digestion, adding acid liquor until the pH value of the water sample is less than 7, and fully and uniformly mixing.
It can be understood that the corresponding oxidant and alkali liquor are added according to the volume of the water sample, so that the nitrogen element in the water sample is converted into nitrate.
Preferably, the digestion treatment is carried out by using alkaline potassium persulfate, and the oxidizing agent is potassium persulfate solution with the concentration of 10-20 g/L; the alkali liquor is sodium hydroxide solution, and the concentration is 10-25 g/L; the acid solution is hydrochloric acid solution with the concentration of 1+ 9.
It can be understood that the purpose of adding the hydrochloric acid solution is to neutralize the water sample, so that the water sample is acidic, and the pH value is less than 7, and those skilled in the art can determine the amount of the added hydrochloric acid according to the volume of the water sample and the pH value of the water after adding the alkali solution and the oxidant, which is not limited in the present invention.
In a specific implementation, the second digestion treatment step specifically includes:
and heating and digesting the water sample subjected to the first digestion treatment at the temperature of 80-125 ℃ for 5-15 min.
Most suspended matters are removed after the water sample is subjected to first digestion treatment, and the rest suspended matters are heated for the second time, so that the interference of turbidity can be effectively reduced.
The embodiment of the invention also provides a total nitrogen monitoring method, which comprises the following steps:
carrying out first digestion treatment on the water sample, and measuring the first absorbance of the water sample subjected to the first digestion treatment;
judging whether the first absorbance meets the total nitrogen turbidity compensation condition, if so, performing second digestion treatment on the water sample, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample;
if not, taking the first absorbance as the absorbance of the water sample;
measuring the absorbance of the reference solution;
and determining the total nitrogen of the water sample according to the absorbance of the water sample and the absorbance of the reference solution.
Preferably, the reference solution is distilled water.
The judging whether the first absorbance meets the total nitrogen turbidity compensation condition specifically comprises:
judging whether A275 of the first absorbance is more than or equal to 0.1;
judging whether the A275/A220 of the first absorbance is more than or equal to 15 percent;
and if the A275 of the first absorbance is more than or equal to 0.1 or the A275/A220 of the first absorbance is more than or equal to 15%, judging that the first absorbance meets the total nitrogen turbidity compensation condition.
The first digestion treatment step specifically comprises: adding an oxidant and an alkali liquor with preset volumes into a water sample, fully and uniformly mixing, and digesting for 30-40min at the temperature of 120-; after digestion, adding acid liquor until the pH value of the water sample is less than 7, and fully and uniformly mixing.
The oxidant is potassium persulfate solution with the concentration of 10-20 g/L; the alkali liquor is sodium hydroxide solution, and the concentration is 10-25 g/L; the acid solution is hydrochloric acid solution with the concentration of 1+ 9.
The second digestion treatment step specifically comprises: and heating and digesting the water sample subjected to the first digestion treatment at the temperature of 80-125 ℃ for 5-15 min.
Referring to fig. 1, in the total nitrogen automatic on-line monitoring device, the total nitrogen monitoring method provided by the embodiment of the invention can be perfectly executed by optimizing the test flow. The total nitrogen automatic on-line monitoring equipment comprises a sample introduction unit, a metering unit, a digestion colorimetric unit and a data processing unit.
The sample introduction unit and the metering unit measure a certain volume of oxidant, alkali liquor and a water sample to be measured, the oxidant, the alkali liquor and the water sample enter the digestion colorimetric unit, after heating and digestion are carried out for a period of time, a certain volume of acid liquor is measured through the sample introduction unit and the metering unit, the acid liquor enters the digestion colorimetric unit, and the first absorbance of the water sample is measured through the digestion colorimetric unit;
judging whether the first absorbance meets the total nitrogen turbidity compensation condition or not by the data processing unit, if so, performing second digestion treatment on the water sample by the digestion colorimetric unit, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample; if not, taking the first absorbance as the absorbance of the water sample;
then, liquid in the digestion colorimetric unit is emptied by the sample introduction unit and the metering unit, a certain volume of reference solution is taken to enter the digestion colorimetric unit, and the reference absorbance of the reference solution is measured by the digestion colorimetric unit;
and determining the total nitrogen of the water sample according to the absorbance of the water sample and the absorbance of the reference solution.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (7)

1. A turbidity compensation method for automatic online total nitrogen monitoring is characterized by comprising the following steps:
carrying out first digestion treatment on the water sample, and measuring the first absorbance of the water sample subjected to the first digestion treatment;
judging whether the first absorbance meets the total nitrogen turbidity compensation condition, if so, performing second digestion treatment on the water sample, determining second absorbance of the water sample subjected to the second digestion treatment, and taking the second absorbance as the absorbance of the water sample;
and if not, taking the first absorbance as the absorbance of the water sample.
2. The turbidity compensation method for automatic on-line total nitrogen monitoring as claimed in claim 1, wherein said determining whether said first absorbance satisfies a total nitrogen turbidity compensation condition specifically comprises:
determining A of the first absorbance275Whether the content is more than or equal to 0.1;
determining A of the first absorbance275/A220Whether the content is more than or equal to 15 percent or not;
if A of said first absorbance275Not less than 0.1 or A of the first absorbance275/A220And if the total nitrogen turbidity compensation condition is not less than 15%, judging that the first absorbance meets the total nitrogen turbidity compensation condition.
3. The turbidity compensation method for automatic on-line total nitrogen monitoring according to claim 1, wherein the first digestion treatment step specifically comprises:
adding an oxidant and an alkali liquor with preset volumes into a water sample, fully and uniformly mixing, and digesting for 30-40min at the temperature of 120-; after digestion, adding acid liquor until the pH value of the water sample is less than 7, and fully and uniformly mixing.
4. A turbidity compensating method for automatic on-line monitoring of total nitrogen according to claim 3, wherein said oxidizing agent is potassium persulfate solution with concentration of 10-20 g/L;
the alkali liquor is sodium hydroxide solution, and the concentration is 10-25 g/L;
the acid solution is hydrochloric acid solution with the concentration of 1+ 9.
5. The turbidity compensation method for automatic on-line total nitrogen monitoring according to claim 1, wherein said turbidity compensation method comprises,
the second digestion treatment step specifically comprises:
and heating and digesting the water sample subjected to the first digestion treatment at the temperature of 80-125 ℃ for 5-15 min.
6. A total nitrogen monitoring method comprising a turbidity compensation method of automatic on-line total nitrogen monitoring according to any one of claims 1 to 5, further comprising:
measuring the absorbance of the reference solution;
and determining the total nitrogen of the water sample according to the absorbance of the water sample and the absorbance of the reference solution.
7. The total nitrogen monitoring method of claim 6, wherein the reference liquid is distilled water.
CN201910896364.5A 2019-09-19 2019-09-19 Turbidity compensation method for automatic online total nitrogen monitoring and total nitrogen monitoring method Pending CN110596024A (en)

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CN113092457A (en) * 2021-04-07 2021-07-09 福州大学 Online accurate detection method suitable for nitrite nitrogen in water body in complex environment
CN114002168A (en) * 2021-08-04 2022-02-01 河北雄安华清宏远环境科技有限公司 Method and device for detecting liquid concentration by eliminating turbidity difference
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CN117517231A (en) * 2024-01-03 2024-02-06 杭州泽天春来科技股份有限公司 Analysis method, system and readable medium of total nitrogen water quality online analyzer

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Publication number Priority date Publication date Assignee Title
CN112098348A (en) * 2020-08-20 2020-12-18 厦门斯坦道科学仪器股份有限公司 Total phosphorus turbidity compensation method applied to high-turbidity water body online monitoring
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CN112924405A (en) * 2021-01-27 2021-06-08 华能(天津)煤气化发电有限公司 Concentrated seawater total nitrogen data continuous online monitoring system for seawater cooling power plant
CN113092457A (en) * 2021-04-07 2021-07-09 福州大学 Online accurate detection method suitable for nitrite nitrogen in water body in complex environment
CN113092457B (en) * 2021-04-07 2022-03-22 福州大学 Online accurate detection method suitable for nitrite nitrogen in water body in complex environment
CN114002168A (en) * 2021-08-04 2022-02-01 河北雄安华清宏远环境科技有限公司 Method and device for detecting liquid concentration by eliminating turbidity difference
CN114636694A (en) * 2022-05-17 2022-06-17 广东盈峰科技有限公司 Water environment on-line automatic detection device and detection method
CN117517231A (en) * 2024-01-03 2024-02-06 杭州泽天春来科技股份有限公司 Analysis method, system and readable medium of total nitrogen water quality online analyzer
CN117517231B (en) * 2024-01-03 2024-04-12 杭州泽天春来科技股份有限公司 Analysis method, system and readable medium of total nitrogen water quality online analyzer

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Application publication date: 20191220