CN113138170A - Method for measuring biodegradable soluble organic nitrogen of drinking water - Google Patents

Method for measuring biodegradable soluble organic nitrogen of drinking water Download PDF

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CN113138170A
CN113138170A CN202110282755.5A CN202110282755A CN113138170A CN 113138170 A CN113138170 A CN 113138170A CN 202110282755 A CN202110282755 A CN 202110282755A CN 113138170 A CN113138170 A CN 113138170A
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楚文海
张瑞华
肖融
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Tongji University
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    • G01MEASURING; TESTING
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    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

本发明公开了一种饮用水可生物降解溶解性有机氮的测定方法,包括以下步骤:S110、待测样品预处理,用滤膜过滤待测水样,并测定过滤后水样的DON浓度,记为DONi;S120、配置接种母液,配制接种活性污泥浓度为100~200mg/L的培养接种母液MLSS;S130、混合培养;S140、根据公式BDON=DONi‑DONf,计算待测水样的BDON值。有益效果在于:采用该方法,可测定饮用水和地表水等含氮水平较低的水样中生物可降解溶解性有机氮的含量,测量精度高;该方法操作简单,接种液廉价易得,操作成本低,且同时可进行批量测定;该方法可运用于饮用水、地表水等实际水体中生物可降解溶解性有机氮的测定。

Figure 202110282755

The invention discloses a method for determining the biodegradable dissolved organic nitrogen of drinking water, comprising the following steps: S110, pre-processing a sample to be tested, filtering the water sample to be tested with a filter membrane, and measuring the DON concentration of the filtered water sample, Denoted as DON i ; S120, configuration inoculation mother liquor, preparation inoculation activated sludge concentration is the culture inoculation mother liquor MLSS of 100~200mg/L; S130, mixed culture; S140, according to formula BDON=DON i -DON f , calculate the water to be tested the same BDON value. The beneficial effects are as follows: by adopting the method, the content of biodegradable dissolved organic nitrogen in water samples with low nitrogen levels such as drinking water and surface water can be measured, and the measurement accuracy is high; the method is simple to operate, the inoculation solution is cheap and easy to obtain, The operation cost is low, and batch determination can be performed at the same time; the method can be applied to the determination of biodegradable dissolved organic nitrogen in actual water bodies such as drinking water and surface water.

Figure 202110282755

Description

Method for measuring biodegradable soluble organic nitrogen of drinking water
Technical Field
The invention relates to the technical field of water treatment, in particular to a method for measuring biodegradable soluble organic nitrogen of drinking water.
Background
The soluble total nitrogen of the drinking water comprises three inorganic nitrogen of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen and soluble organic nitrogen (DON). Most of the inorganic nitrogen in the drinking water treatment plant can be removed by nitrification-denitrification, but DON is hardly removed completely, while Biodegradable Dissolved Organic Nitrogen (BDON) refers to the portion of DON in the water body that can be metabolized and utilized by heterotrophic bacteria, and is more difficult to remove by chemical oxidation. The BDON not only can be used as a nitrogen source for the growth of microorganisms in a water distribution system to bring about potential safety hazards of the microorganisms, but also is an important precursor of nitrogen-containing disinfection byproducts with cytotoxicity and genetic toxicity.
At present, no direct and perfect BDON measuring method exists at home and abroad. Generally, most researchers at home and abroad compare differences of DONs before and after culture to calculate BDON mainly through a static culture method. The method has simple operation, cheap and easily obtained inoculation liquid, and can simultaneously carry out batch determination. In general, the analysis of BDON values is susceptible to microbial inoculation and inoculation cycles. Higher inoculum size increases the error in final BDON value due to the increase in DON values resulting from release of endogenous species from the bacteria, and lower inoculum size underestimates BDON values due to insufficient degradation of organic matter by the microorganisms. Khan et al (Water environ. Res.,2009,81(8),779-787) invented a method for measuring factory Water BDON of a sewage plant by using a static culture method, taking bacteria in sewage to be measured as inoculation liquid, and accurately reflecting the outlet Water BDON of the sewage plant when the sludge concentration (MLSS) of the added inoculation liquid is determined to be 240mg/L through a preliminary experiment. The Chinese patent with the patent number CN107655842A determines a sewage sample BDON through a similar experiment, and shows that when the concentration of DOC in the sewage sample is less than or equal to 30mg/L, the concentration of inoculating liquid sludge is 240mg/L, when the concentration of DOC in the sewage sample is more than 30mg/L and less than or equal to 70mg/L, the concentration of inoculating liquid sludge is 350mg/L, when the concentration of DOC in the sewage sample is more than 70mg/L, the concentration of inoculating liquid sludge is 420mg/L, and the BDON can accurately reflect the effluent BDON of a sewage plant. However, for raw water of drinking water and drinking water in the treatment process, because the organic matter content of the raw water is very low (the DOC concentration is less than 10mg/L), the method for measuring the sewage sample has the problem of lack of accuracy and precision in measuring the water sample of the drinking water.
The previous method for measuring the biodegradable soluble organic nitrogen of the sewage comprises the following steps: the concentration of DON in the sewage is high (mg/L level), the concentration of the inoculation liquid sludge required for measuring BDON is high, and the required culture period is long. The concentration of DON in a drinking water sample is low (mu g/L level), and the accuracy and the precision of measuring the BDON of the drinking water by using a method for measuring the BDON of the sewage are lacked. And various DON's (e.g., unstable DON in fresh water and sea water) may not be degraded with the inoculum from river water. Based on this, the applicant proposed a method for determining the biodegradable solubility of drinking water with eggs.
Disclosure of Invention
The present invention is directed to solving the above problems and providing a method for measuring biodegradable soluble organic nitrogen in drinking water, and a preferred embodiment of the present invention includes: the method can be used for measuring the organic nitrogen content in drinking water and surface water, and has the technical effects of simple operation, low operation cost and the like, and the details are explained below.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for measuring biodegradable soluble organic nitrogen of drinking water, which comprises the following steps:
s110, pretreating a sample to be detected, filtering the sample to be detected by using a filter membrane, and determining the DON concentration of the filtered sample, and recording the DON concentration as DONi
S120, preparing an inoculation mother liquor, and preparing a culture inoculation mother liquor MLSS with inoculation activated sludge concentration of 100-200 mg/L;
s130, performing mixed culture, namely taking the water sample to be detected processed in the step S110 and the culture inoculation mother liquor prepared in the step S120 according to the material taking ratio of 50-150:1, fully shaking and uniformly mixing the water sample and the culture inoculation mother liquor in the step S120, placing the mixture in a reagent bottle, performing light-tight culture for 7-20 days, and measuring the DON concentration in the mixture after the culture is finished, wherein the DON concentration is marked as DONf
S140, according to the formula BDON DONi-DONfAnd calculating the BDON value of the water sample to be detected.
Preferably, in step S110, the filter membrane is an acetate membrane, and the pore size of the filter membrane is 0.22 μm.
Preferably, the step S120 includes the following operations:
s121, taking activated sludge in an aerobic section of a water plant;
s122, measuring the MLSS concentration of the activated sludge by using quantitative filter paper filtration, and marking as MLSS0
S123, diluting the activated sludge to 100-200 mg/L to obtain a culture inoculation mother liquor.
Preferably, in operation S123, the sludge concentration of the mother liquor for culture and inoculation is 150 g/L.
Preferably, in step S130, the ratio of the water sample to be tested to the culture inoculation mother liquor is 100: 1.
Preferably, in step S130, the reagent bottle is a brown glass reagent bottle.
Preferably, in step S130, the temperature in the incubator is 25 ± 0.5 ℃.
Preferably, in step S130, the culture time is 14 days.
In conclusion, the beneficial effects of the invention are as follows: 1. by adopting the method, the content of biodegradable soluble organic nitrogen in water samples with low nitrogen level, such as drinking water, surface water and the like, can be measured, and the measurement precision is high;
2. the method has the advantages of simple operation, cheap and easily obtained inoculation liquid, low operation cost and capability of carrying out batch determination;
3. the method can be applied to the determination of biodegradable soluble organic nitrogen in actual water bodies such as drinking water, surface water and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 shows BDON concentrations of 1 to 5 in water samples to be tested in examples 1 to 5 of the present invention.
Fig. 2 is an operational schematic of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The invention provides a method for measuring biodegradable soluble organic nitrogen of drinking water, which comprises the following steps as shown in figure 2:
s110, pretreating a sample to be detected, filtering the water sample to be detected by using a filter membrane, wherein the filter membrane is an acetate fiber membrane, the aperture of the filter membrane is 0.22 mu m, and determining the DON concentration of the filtered water sample and marking as DONi
S120, preparing an inoculation mother liquor, and preparing a culture inoculation mother liquor MLSS with inoculation activated sludge concentration of 100-200 mg/L, wherein the method specifically comprises the following operations:
s121, taking activated sludge in an aerobic section of a water plant;
s122, measuring the MLSS concentration of the activated sludge by using quantitative filter paper filtration, and marking as MLSS0
S123, diluting the activated sludge to 100-200 mg/L to obtain a culture inoculation mother liquor, wherein the preferable concentration is 150 g/L;
s130, performing mixed culture, namely taking the water sample to be detected processed in the step S110 and the culture inoculation mother liquor prepared in the step S120 according to the material taking ratio of 50-150:1, preferably 100:1, taking 200ml of the water sample to be detected, culturing 2ml of the inoculation mother liquor, sufficiently shaking, uniformly mixing in a 250ml brown glass reagent bottle, placing in a thermostat at the temperature of 25 +/-0.5 ℃ for 7-20 days, preferably 14 days in a dark place, and measuring the DON concentration after the culture is finished, wherein the DON concentration is recorded as DONf
S140, according to the formula BDON DONi-DONfAnd calculating the BDON value of the water sample to be detected.
Concentration of DON (DON) in the drinking water sample described in step S110 and step S130iAnd DONf) The ammonia nitrogen-containing nitrite nitrogen is calculated by the difference value of total soluble organic nitrogen (TDN) and ammonia nitrogen (NH3-N), nitrate nitrogen (NO3-N) and nitrite nitrogen (NO2-N), namely DON (mu g/L, counted by N) is TDN- (NH3-N + NO3-N + NO 2-N); the concentration of the total soluble organic nitrogen is measured by adopting a Hash total nitrogen reagent package (persulfate oxidation-ultraviolet spectrophotometry); the concentration of the ammonia nitrogen is measured by adopting a nano reagent-spectrophotometry method; the concentration of the nitrate nitrogen is measured by adopting a Hash nitrate reagent powder pillow bag (cadmium reduction method); the concentration of the nitrite nitrogen is measured by adopting a pillow bag (diazotization method) of a Hash nitrite reagent powder
The specific embodiment is as follows:
example 1:
taking raw water from a certain drinking water treatment plant, marking as a sample 1, immediately filtering the raw water by using a filter membrane with the diameter of 0.22 mu m, and measuring total soluble organic nitrogen (TDN) and ammonia Nitrogen (NH) in the filtered sample3-N), nitrate Nitrogen (NO)3-N) and nitrous Nitrogen (NO)2-N) according to the formula DON (μ g/L, in N) ═ TDN- (NH)3-N+NO2-N+NO3-N) calculating the concentration of DONi(ii) a Then 2mL of the inoculation mother liquor MLSS with the initial concentration of 150mg/L and 200mL of the sample 1 are taken in a 250mL brown reagent bottle, mixed fully and shaken uniformly, and cultured for 14 days in a dark place at the constant temperature of 25 ℃. Under the same conditions, the blank test was supplemented with sterile water culture as a control group. Determining TDN, NH of the water sample after the culture3-N,NO3-N and NO2The value of N and the DON concentration calculated and recorded as DONfFinally, the BDON value is calculated, and the result is shown in figure 1.
Example 2:
taking reservoir water from a certain reservoir, marking as a sample 2, immediately filtering with a 0.22 μm filter membrane, and measuring total soluble organic nitrogen (TDN) and ammonia Nitrogen (NH) in the filtered sample3-N), nitrate Nitrogen (NO)3-N) and nitrous Nitrogen (NO)2-N) according to the formula DON (μ g/L, in N) ═ TDN- (NH)3-N+NO2-N+NO3-N) calculating the concentration of DONi(ii) a Then 2mL of the inoculation mother liquor MLSS with the initial concentration of 150mg/L and 200mL of the sample 1 are taken in a 250mL brown reagent bottle, mixed fully and shaken uniformly, and cultured for 14 days in a dark place at the constant temperature of 25 ℃. Under the same conditions, the blank test was supplemented with sterile water culture as a control group. Determining TDN, NH of the water sample after the culture3-N,NO3-N and NO2The value of N and the DON concentration calculated and recorded as DONfFinally, the BDON value is calculated, and the result is shown in figure 1.
Example 3;
a glycine solution with an initial mass concentration of 1mg/L (in terms of N) was prepared and recorded as sample 3, 2mL of an inoculum stock MLSS with an initial concentration of 150mg/L was added to 200mL of the glycine solution, and the mixture was incubated at a constant temperature of 25 ℃ for 14 days in the absence of light. Under the same conditions, the blank test was supplemented with sterile water culture as a control group. Determining total soluble organic nitrogen (TDN) and ammonia Nitrogen (NH) in the water sample after the culture3-N), nitrate Nitrogen (NO)3-N) and nitrous Nitrogen (NO)2-N) according to the formula DON (μ g/L, in N) ═ TDN- (NH)3-N+NO2-N+NO3-N) calculating the DONfAnd BDON, the results are shown in FIG. 1.
Example 4:
preparing a tyrosine solution with the initial mass concentration of 1mg/L (counted by N), recording as a sample 4, adding 2mL of inoculation mother liquor MLSS with the initial concentration of 150mg/L into 200mL of the tyrosine solution, and carrying out light-shielding culture for 14 days at the constant temperature of 25 ℃. Under the same conditions, the blank test was supplemented with sterile water culture as a control group. Determining total soluble organic nitrogen (TDN) and ammonia Nitrogen (NH) in the water sample after the culture3-N), nitrate Nitrogen (NO)3-N) and nitrous Nitrogen (NO)2-N) according to the formula DON (μ g/L, in N) ═ TDN- (NH)3-N+NO2-N+NO3-N) calculating the DONfAnd BDON, the results are shown in FIG. 1.
Example 5:
preparing 1mg/L (calculated by N) glutamic acid solution2mL of the inoculation mother liquor MLSS with the initial concentration of 150mg/L was added to 200mL of glutamic acid solution, and the mixture was incubated at a constant temperature of 25 ℃ for 14 days in the dark. Under the same conditions, the blank test was supplemented with sterile water culture as a control group. Determining total soluble organic nitrogen (TDN) and ammonia Nitrogen (NH) in the water sample after the culture3-N), nitrate Nitrogen (NO)3-N) and nitrous Nitrogen (NO)2-N) according to the formula DON (μ g/L, in N) ═ TDN- (NH)3-N+NO2-N+NO3-N) calculating the DONfAnd BDON, the results are shown in FIG. 1.
As can be seen from fig. 1, in the actual water sample, the BDON values of the sample 1 and the sample 2 are lower, and the BDON value of the water sample prepared from the amino acid solution is higher, so that actually, the amino acid standard is more easily biodegraded. Therefore, the determination method provided by the invention can also be used for determining the BDON value in a drinking water source.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (8)

1.一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,包括以下步骤:1. a kind of assay method of drinking water biodegradable dissolved organic nitrogen, is characterized in that, comprises the following steps: S110、待测样品预处理,用滤膜过滤待测水样,并测定过滤后水样的DON浓度,记为DONiS110, pretreatment of the sample to be tested, filters the water sample to be tested with a membrane filter, and measures the DON concentration of the filtered water sample, and is denoted as DON i ; S120、配置接种母液,配制接种活性污泥浓度为100~200mg/L的培养接种母液MLSS;S120, prepare an inoculation mother solution, and prepare a culture inoculation mother solution MLSS with an inoculation activated sludge concentration of 100-200 mg/L; S130、混合培养,取经步骤S110处理好的待测水样与经步骤S120制备的培养接种母液,取料比例为50-150:1,充分震荡混合均匀于试剂瓶中,并放置在恒温箱中避光培养7-20天,待培养结束后测定其中的DON浓度,记为DONfS130, mixed culture, take the water sample to be tested processed in step S110 and the culture inoculation mother solution prepared in step S120, the ratio of taking materials is 50-150:1, fully shake and mix them evenly in the reagent bottle, and place it in an incubator The 7-20 days of dark cultivation, the DON concentration wherein is measured after cultivating finishes, is denoted as DON f ; S140、根据公式BDON=DONi-DONf,计算待测水样的BDON值。S140, according to the formula BDON=DON i -DON f , calculate the BDON value of the water sample to be tested. 2.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S110中,滤膜为醋酸纤维膜,且该滤膜的孔径为0.22μm。2 . The method for measuring the biodegradable dissolved organic nitrogen of drinking water according to claim 1 , wherein in the step S110 , the filter membrane is a cellulose acetate membrane, and the pore size of the filter membrane is 0.22 μm. 3 . 3.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S120中,包括以下操作:3. A kind of assay method of drinking water biodegradable dissolved organic nitrogen according to claim 1, is characterized in that, in described step S120, comprises the following operations: S121、取水厂中好氧段活性污泥;S121. Activated sludge in the aerobic section of the water intake plant; S122、使用定量滤纸过滤测定活性污泥的MLSS浓度,记为MLSS0S122, use quantitative filter paper to filter and measure the MLSS concentration of activated sludge, and denote it as MLSS 0 ; S123、稀释活性污泥至100~200mg/L得到培养接种母液。S123, diluting the activated sludge to 100-200 mg/L to obtain a culture and inoculation mother liquor. 4.根据权利要求3所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述操作S123中,培养接种母液的污泥浓度为150g/L。4 . The method for measuring the biodegradable dissolved organic nitrogen of drinking water according to claim 3 , wherein, in the operation S123 , the sludge concentration of the culture and inoculation mother liquor is 150 g/L. 5 . 5.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S130中,待测水样与培养接种母液的取料比例为100:1。5 . The method for measuring the biodegradable dissolved organic nitrogen of drinking water according to claim 1 , wherein in the step S130 , the ratio of the water sample to be tested to the culture and inoculation mother liquor is 100:1. 6 . 6.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S130中,所述试剂瓶为棕色玻璃试剂瓶。6 . The method for measuring the biodegradable dissolved organic nitrogen in drinking water according to claim 1 , wherein, in the step S130 , the reagent bottle is a brown glass reagent bottle. 7 . 7.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S130中,所述恒温箱中温度为25±0.5℃。7 . The method for measuring the biodegradable dissolved organic nitrogen of drinking water according to claim 1 , wherein, in the step S130 , the temperature in the incubator is 25±0.5° C. 8 . 8.根据权利要求1所述一种饮用水可生物降解溶解性有机氮的测定方法,其特征在于,所述步骤S130中,培养时间为14天。8 . The method for measuring the biodegradable dissolved organic nitrogen in drinking water according to claim 1 , wherein, in the step S130 , the incubation time is 14 days. 9 .
CN202110282755.5A 2021-03-16 2021-03-16 Method for measuring biodegradable soluble organic nitrogen of drinking water Pending CN113138170A (en)

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Publication number Priority date Publication date Assignee Title
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CN107655842A (en) * 2017-09-19 2018-02-02 南京大学 A kind of degradable soluble organic nitrogen assay method of saprobia based on static culture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101782566A (en) * 2010-01-12 2010-07-21 同济大学 Method for measuring concentration of low-concentration soluble organic nitrogen in water
CN105158429A (en) * 2015-09-17 2015-12-16 哈尔滨工业大学 Method for measuring content of biodegradable organic carbon (BDOC) in water
CN107515287A (en) * 2017-09-19 2017-12-26 南京大学 A method for the determination of biodegradable dissolved organic nitrogen in sewage based on dynamic culture
CN107655842A (en) * 2017-09-19 2018-02-02 南京大学 A kind of degradable soluble organic nitrogen assay method of saprobia based on static culture

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