CN112964654A - Method for determining content of ammonia nitrogen in chlorine-containing wastewater and application thereof - Google Patents
Method for determining content of ammonia nitrogen in chlorine-containing wastewater and application thereof Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of ammonia nitrogen in chlorine-containing wastewater, which comprises the following steps: s1, mixing and reacting the wastewater after dechlorination with first silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and a Navier reagent to obtain a mixed solution; s2, performing spectrophotometry on the mixed solution; the ratio of the first silver nitrate to the first mercury sulfate to the first sodium thiosulfate to the first potassium sodium tartrate to the first sodium natrientate is (0.008-0.009) g: (0.009-0.011) g: (0.0017-0.0018) g: (0.4-0.6) g: (1.4-1.6) mL; the ammonia nitrogen content in the wastewater before dechlorination is more than or equal to 0.1 mg/L; the content of chloride ions in the wastewater before dechlorination is less than or equal to 15000 mg/L. According to the invention, the wastewater after dechlorination is mixed and reacted with the mercury sulfate, the first silver nitrate, the sodium thiosulfate, the potassium sodium tartrate and the Nashin reagent, so that the experimental accuracy is high, and the application value is high.
Description
Technical Field
The invention relates to a method for measuring the content of ammonia nitrogen in chlorine-containing wastewater and application thereof.
Background
Ammonia nitrogen means free ammonia (NH) in water3) And ammonium ion (NH)4 +) The main sources of ammonia and ammonia nitrogen in the form of ammoniaThe products of nitrogen-containing organic matters in industrial production drainage, farmland drainage and biological sewage under the action of microbial decomposition. Ammonia nitrogen is an important index for measuring the water environment pollution level and takes milligram per liter (mg/L) as a unit. Therefore, the accurate measurement of the ammonia nitrogen value of the water sample has important significance for truly reflecting the water pollution degree and monitoring and treating the industrial wastewater. However, chloride ions affect the accuracy of the measurement results to varying degrees.
Currently, a nano reagent spectrophotometry (HJ 535-2009), a salicylic acid spectrophotometry, a titration method, an electrode method and the like are generally adopted for measuring ammonia nitrogen. Although the methods are numerous, the interference of the chloride coexisting in the wastewater on the measured value of ammonia nitrogen is always a problem which is difficult to solve. By adopting the methods, the determination result of ammonia nitrogen is higher for wastewater with higher chlorine content. Wherein, the content of chloride ions is roughly judged in a nano reagent spectrophotometry (HJ 828-2017), and then the sodium thiosulfate mercury solution is added according to the content of the chloride ions in proportion, so that the method is easy to cause larger experimental deviation; the preparation of the reagent of salicylic acid spectrophotometry is relatively complex; the electrode method is easily interfered by chloride ions and is not suitable for being applied to high-chlorine wastewater.
Considering that most of the waste water contains chloride ions at present, especially some industrial waste water containing chloride with higher concentration. Therefore, it is an urgent need to solve the problem of accurately measuring the ammonia nitrogen content to accurately reflect the water quality under the condition of containing chloride ions, and it is important to develop a method for rapidly detecting the ammonia nitrogen content in high-chlorine wastewater.
CN104568936A discloses an ammonia nitrogen test paper and an application method thereof, comprising the following steps: (1) preparing a reagent solution: dissolving analytically pure sodium salicylate, sodium potassium tartrate and sodium nitrosoferricyanide in ammonia-free water to prepare a solution with the concentration of 280-380 mg of sodium salicylate, 50-68 mg of sodium potassium tartrate and 0.40-0.54 mg of sodium nitrosoferricyanide per liter; (2) dipping: completely soaking quantitative medium-speed filter paper into the solution in the step (1), and oscillating on a constant-temperature oscillator for 60-120 minutes; (3) molding: taking out the filter paper, placing the filter paper in parallel at room temperature, suspending and airing the filter paper, and cutting the filter paper and then carrying out plastic package for later use. The method needs to prepare the reagent by a salicylic acid method, is easy to generate human errors, and can not avoid the generation of flocculate in the high-chlorine wastewater during ammonia nitrogen detection, and practice operations also show that the error of the result measured by the method is larger.
Disclosure of Invention
The invention aims to solve the technical problems of large error and complex operation of the measurement result of the content of ammonia nitrogen in the waste water containing chloride ions in the prior art, and provides a method for measuring the content of ammonia nitrogen in the waste water containing chloride ions and application thereof. The method can be used for measuring the content of ammonia nitrogen in wastewater with higher chlorine content, can measure water samples in batches, and has wide application range, high accuracy and practical application value.
The invention solves the technical problems through the following technical scheme:
a method for measuring the content of ammonia nitrogen in chlorine-containing wastewater comprises the following steps:
s1, mixing and reacting the wastewater after dechlorination with first silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and a Navier reagent to obtain a mixed solution;
s2, performing spectrophotometry on the mixed solution;
the ratio of the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the sodium potassium tartrate and the Nassner reagent is (0.008-0.009) g: (0.009-0.011) g: (0.0017-0.0018) g: (0.4-0.6) g: (1.4-1.6) mL;
the ammonia nitrogen content in the wastewater before dechlorination is more than or equal to 0.1 mg/L;
the content of chloride ions in the wastewater before dechlorination is less than or equal to 15000 mg/L.
In step S1, the wastewater after chlorine removal is generally wastewater after removing chloride ions by a conventional chlorine removal method in the art. For example, the chlorine removal process may be a silver nitrate precipitation process. The dechlorinated wastewater generally does not discolor the starch-potassium iodide test paper.
In step S1, the wastewater after dechlorination is preferably prepared by the following steps: and mixing the wastewater before dechlorination and second silver nitrate for reaction, and performing solid-liquid separation to obtain filtrate, namely the wastewater after dechlorination.
In the preparation process of the wastewater after chlorine removal, preferably, the mass ratio of the chloride ions in the wastewater before chlorine removal to the second silver nitrate is (0-15): 170.
in the preparation process of the wastewater after chlorine removal, the second silver nitrate is generally added in the form of solution. When the second silver nitrate is added in the form of a solution, the concentration of the silver nitrate solution is preferably 0.075-0.125 mol/L, such as 0.1 mol/L.
The second silver nitrate is added into the wastewater before dechlorination, so that the wastewater after dechlorination is prevented from being directly contacted with the first silver nitrate, the mercury sulfate and the sodium thiosulfate to generate silver salt precipitates to the greatest extent, and further the subsequent test result is influenced.
In the preparation process of the wastewater after the dechlorination, in the process of the mixing reaction, the wastewater before the dechlorination and the second silver nitrate are generally uniformly dispersed so as to facilitate the complete reaction.
In the preparation process of the wastewater after the chlorine removal, the operation and conditions of the solid-liquid separation can be conventional in the field, and are generally centrifugal.
In step S1, the wastewater after chlorine removal is preferably diluted before the wastewater after chlorine removal is subjected to the mixing reaction.
Preferably, the concentration of nitrate radicals in the wastewater after the chlorine removal after the dilution is 0.12-0.2 mol/L. The effect of the introduction of nitrate on the results of subsequent analyses can be reduced by said dilution.
In step S1, the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the potassium sodium tartrate, and the na' S reagent are added in sequence without any special requirement, and may be added simultaneously or in steps. If the stepwise addition is adopted, the addition sequence of the substances is not in sequence.
In step S1, preferably, the wastewater after dechlorination is added to a mixed reagent of the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the potassium sodium tartrate, and the na' S reagent, and then the mixed reaction is performed.
In a preferred embodiment of the present invention, a mixed reagent of the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the potassium sodium tartrate and the na's reagent may be prepared in advance.
In the mixed reagent, the concentration range of the first silver nitrate is preferably 0.007 to 0.009mol/L, for example 0.008 mol/L.
In the mixed reagent, the concentration range of the mercury sulfate is preferably 0.005-0.006 mol/L, for example, 0.0056 mol/L.
In the mixed reagent, the concentration range of the sodium thiosulfate is preferably 0.0015 to 0.002mol/L, for example, 0.0018 mol/L.
In the mixed reagent, the concentration range of the potassium sodium tartrate is preferably 0.38 to 0.42mol/L, for example, 0.4 mol/L.
The first silver nitrate, the mercury sulfate, and the sodium thiosulfate are commercially available as is conventional in the art. The first silver nitrate, the mercury sulfate and the sodium thiosulfate are used for removing residual chlorine in the wastewater.
The na's reagent may be conventional and commercially available in the art. The NanS reagent can form a complex with the ammonia nitrogen in the wastewater, and the content of the ammonia nitrogen in the wastewater is reflected through the absorbance of the complex.
The potassium sodium tartrate may be commercially available as is conventional in the art. The potassium sodium tartrate is used for removing calcium and magnesium ions in wastewater.
In step S1, the method for determining the content of ammonia nitrogen in the wastewater before dechlorination may be conventional in the art. Generally, the judgment can be carried out through the color of the wastewater, when the wastewater is diluted to be orange, the content of ammonia nitrogen in the wastewater is more than or equal to 0.1mg/L, and the ammonia nitrogen determination can be carried out by adopting the method provided by the invention.
In step S1, the method for determining the chloride ion content in the wastewater before dechlorination may be conventional in the art, and may be generally determined according to the rough determination method of chloride ion content in annex a of HJ 828-. When the content of chloride ions in the wastewater before chlorine removal is more than or equal to 15000mg/L, excessive second silver nitrate is required to be introduced to remove the chloride ions, and the subsequent ammonia nitrogen test result is influenced by the excessive nitrate concentration. Diluting the wastewater after dechlorination can cause the content of the ammonia nitrogen to be less than 0.1mg/L, and the ammonia nitrogen cannot be measured.
Preferably, the content of chloride ions in the wastewater before dechlorination is 1000-15000 mg/L.
In step S2, the mixed solution is preferably diluted and then subjected to spectrophotometry.
Wherein, in the diluting process, the solvent for diluting can be conventional in the field. Preferably, the solvent for dilution is deionized water.
In the dilution process, the volume ratio of the mixed solution to the solvent for dilution is preferably 1: (6.5 to 7), for example, 1: 6.7.
as is known in the art, the diluted mixture is generally allowed to stand for 10 to 20min before the mixture is subjected to spectrophotometry.
In step S2, the spectrophotometric method may be conventional in the art. Generally, a matched program and a standard curve built in a spectrophotometer can be called to measure the absorbance at the wavelength of 420nm, and the value of the ammonia nitrogen content can be directly obtained by an instrument, wherein the manufacturing method of the standard curve is shown in HJ 535-2009. At the moment, under a spectrophotometer, the content of ammonia nitrogen in the chlorine-containing wastewater is in direct proportion to the absorbance of a complex formed by the chlorine-containing wastewater.
The invention also provides application of the method for determining the content of ammonia nitrogen in the chlorine-containing wastewater in the pharmaceutical industry, the food industry or the chemical industry.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The positive progress effects of the invention are as follows:
(1) the method is suitable for various chlorine-containing wastewater with the chloride ion content of less than or equal to 15000mg/L and the ammonia nitrogen content of more than or equal to 0.1mg/L, and has wide application range.
(2) The reagent is simple in preparation, the operation process is easy to control, and batch measurement can be carried out.
(3) According to the invention, the wastewater after dechlorination is mixed and reacted with the mercury sulfate, the first silver nitrate, the sodium thiosulfate, the potassium sodium tartrate and the NasLett reagent, so that the interference of residual chloride ions and nitrate ions on ammonia nitrogen determination can be effectively removed, the experimental accuracy is high, and the application value is high.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions. The reagents and starting materials used in the present invention are commercially available.
The reagents used in the examples and comparative examples were all of analytical purity.
Preparing a mixed reagent of first silver nitrate, mercury sulfate, sodium thiosulfate, sodium potassium tartrate and a Nassner reagent: adding 1mL of 500g/L potassium sodium tartrate liquid catalyst, 1.5mL of Nashi reagent, 0.5mL of 0.1mol/L first silver nitrate solution with synergistic effect, 0.5mL of 20g/L mercury sulfate solution, 0.5mL of 3.5g/L sodium thiosulfate solution masking agent and 2.0mL of deionized water into a colorimetric tube with ammonia nitrogen of 50mL, and standing for 15 min.
The operation and conditions of the nano-reagent spectrophotometry adopted in the embodiments of the invention are described in HJ 535-2009; the operation and conditions of the electrode method are described in HZ-HJ-SZ-0136.
Example 1
The embodiment 1 of the invention is used for detecting the ammonia nitrogen standard sample.
Preparing samples with chlorine contents of 1000mg/L, 5000mg/L, 10000mg/L and 15000mg/L by using sodium chloride, and adding an ammonia nitrogen standard solution prepared by ammonium nitrate to ensure that the ammonia nitrogen contents of the standard samples are 0.5mg/L and 1mg/L respectively.
The samples are measured by respectively adopting a traditional nano-grade reagent spectrophotometry method, an electrode method and the method of the invention.
When the method is adopted, the operation steps are as follows:
1) whether the chloride ion content is 1000 mg/L-15000 mg/L is determined according to the rough judgment method of the chloride ion content in the appendix A of HJ 828-. Because the sample in the embodiment is in a standard sample configuration, the content of chloride ions is in the range;
2) adding 10mL of 1mol/L second silver nitrate solution into 10mL of ammonia nitrogen standard sample to obtain dechlorinated wastewater, shaking up, precipitating, adding deionized water to dilute to a constant volume of 50mL volumetric flask, and performing centrifugal separation;
3) adding 0.5mL of the wastewater with constant volume into 6mL of a mixed reagent of first silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and a Nassner reagent to react to obtain a mixed solution A;
4) shaking the mixed solution A uniformly, fixing the volume to 50mL in a cuvette, standing for 10min, calling a matching program and a standard curve built in a spectrophotometer, and measuring the ammonia nitrogen content at the wavelength of 420 nm. For the preparation of the standard curve, refer to HJ 535-2009, and the calculation formula is as follows:
where ρ isNThe mass concentration of ammonia nitrogen in a water sample is mg/L in terms of nitrogen; a. thesThe absorbance of the water sample; a. thebAbsorbance for blank test; a is the intercept of the standard curve; b is the slope of the calibration curve; v is the sample volume, mL.
The specific measurement results are as follows:
TABLE 1 detection results of the Nas reagent method, the electrode method and the method of the present invention for the ammonia nitrogen value in the standard sample
As can be seen from the results in Table 1, the method of the present invention has a significantly improved accuracy and more accurate detection results than the Navier reagent method and the electrode method.
Example 2
The embodiment 2 of the invention is used for example detection and is respectively used for detecting the ammonia nitrogen content in papermaking wastewater, pharmaceutical wastewater and chemical wastewater.
Chlorine-containing wastewater samples are respectively from the wastewater in the middle process of three enterprises, and the wastewater of the three enterprises is characterized by higher content of chloride ions. The samples are measured by adopting a traditional method of a nano-reagent spectrophotometry and the method of the invention respectively.
When the method is adopted, the operation steps are as follows:
1) determining whether the chloride ion content is 1000 mg/L-15000 mg/L according to a rough judgment method of the chloride ion content in the appendix A of HJ 828-.
2) Adding 10mL of 1mol/L second silver nitrate solution into 10mL of wastewater sample to obtain dechlorinated wastewater, shaking up, precipitating, adding deionized water to dilute to a constant volume in a 50mL volumetric flask, and performing centrifugal separation;
3) adding 0.5mL of the wastewater with constant volume into 6mL of a mixed reagent of first silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and a Nassner reagent to react to obtain a mixed solution A;
4) shaking the mixed solution A uniformly, fixing the volume to 50mL in a cuvette, standing for 10min, calling a matching program and a standard curve built in a spectrophotometer, and measuring the ammonia nitrogen content at the wavelength of 420 nm.
The specific measurement results are as follows:
TABLE 2 detection results of the NanR reagent method and the method of the present invention for ammonia nitrogen values in wastewater samples
As can be seen from the results in Table 2, for wastewater samples with high chlorine content from different sources, the method of the present invention can effectively mask the interference of chloride ions therein, and has the advantages of wide application range and high accuracy.
Comparative example 1
0.5ml of 0.1mol/L first silver nitrate solution was not added to the first mixed reagent of silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and Navier reagent, and the test results were shown in Table 3 under the same conditions as in example 2.
Comparative example 2
0.5ml of 20g/L mercuric sulfate solution was not added to the first mixed reagent of silver nitrate, mercuric sulfate, sodium thiosulfate, potassium sodium tartrate and Nashi reagent, and the test results were shown in Table 3, except that the conditions were the same as in example 2.
Comparative example 3
0.5ml of 3.5g/L sodium thiosulfate solution was not added to the first mixed reagent of silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and Navier reagent, and the test results were shown in Table 3, except that the conditions were the same as in example 2.
Comparative example 4
0.5ml of a 0.1mol/L first silver nitrate solution, 0.5ml of a 20g/L mercuric sulfate solution, and 0.5ml of a 3.5g/L sodium thiosulfate solution were not added to the first mixed reagent of silver nitrate, mercuric sulfate, sodium thiosulfate, potassium sodium tartrate, and Nashi reagent, and the other conditions were the same as in example 2, and the results of the detection are shown in Table 3.
TABLE 3 detection results of Ammonia Nitrogen values of different comparative examples
The results in table 3 show that the interference of the mercury sulfate, the first silver nitrate and the sodium thiosulfate on the chloride ions produces a synergistic effect, and the ammonia nitrogen detection precision is remarkably improved. Similarly, in a standard sample with known ammonia nitrogen content and chloride ion content, the ammonia nitrogen measurement result of the sample added with the mercuric sulfate, the first silver nitrate and the sodium thiosulfate is closer to the standard value, and the measurement result is more accurate.
In conclusion, the mercury sulfate, the first silver nitrate and the sodium thiosulfate can effectively remove the interference of residual chloride ions on ammonia nitrogen determination; furthermore, the method is suitable for various water qualities containing chlorine, the concentration of the chlorine ions is less than or equal to 15000mg/L, the content of ammonia nitrogen is more than or equal to 0.1mg/L, and the measuring range is wide; the method has the advantages of simple reagent configuration, easy control of the operation process, batch measurement, high accuracy and experimental value and application value.
The present invention is not limited to the above-described embodiments, and any other changes, substitutions and simplifications which are made without departing from the spirit and principle of the present invention should be regarded as equivalent substitutions and shall be included in the protection scope of the present invention.
Claims (10)
1. A method for measuring the content of ammonia nitrogen in chlorine-containing wastewater comprises the following steps:
s1, mixing and reacting the wastewater after dechlorination with first silver nitrate, mercury sulfate, sodium thiosulfate, potassium sodium tartrate and a Navier reagent to obtain a mixed solution;
s2, performing spectrophotometry on the mixed solution;
the ratio of the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the sodium potassium tartrate and the Nassner reagent is (0.008-0.009) g: (0.009-0.011) g: (0.0017-0.0018) g: (0.4-0.6) g: (1.4-1.6) mL;
the ammonia nitrogen content in the wastewater before dechlorination is more than or equal to 0.1 mg/L;
the content of chloride ions in the wastewater before dechlorination is less than or equal to 15000 mg/L.
2. The method for measuring the content of ammonia nitrogen in chlorine-containing wastewater according to claim 1, wherein the wastewater after chlorine removal is prepared by the following steps: and mixing the wastewater before dechlorination and second silver nitrate for reaction, and performing solid-liquid separation to obtain filtrate, namely the wastewater after dechlorination.
3. The method for determining the content of ammonia nitrogen in chlorine-containing wastewater according to claim 2, wherein in the preparation process of the wastewater after chlorine removal, the mass ratio of the chloride ions in the wastewater before chlorine removal to the second silver nitrate is (0-15): 170.
4. the method for measuring the content of ammonia nitrogen in chlorine-containing wastewater according to claim 2, wherein in the preparation process of the wastewater after chlorine removal, when the second silver nitrate is added in the form of a solution, the concentration of the silver nitrate solution is 0.075-0.125 mol/L, for example 0.1 mol/L.
5. The method for determining the content of ammonia nitrogen in chlorine-containing wastewater according to claim 1, wherein the wastewater after chlorine removal is diluted before the wastewater after chlorine removal is subjected to the mixing reaction.
6. The method for measuring the content of ammonia nitrogen in chlorine-containing wastewater according to claim 5, wherein the concentration of nitrate nitrogen in the wastewater after the chlorine removal after the dilution is 0.12-0.2 mol/L.
7. The method for determining the content of ammonia nitrogen in chlorine-containing wastewater as claimed in claim 1, wherein the wastewater after dechlorination is added to a mixed reagent of the first silver nitrate, the mercury sulfate, the sodium thiosulfate, the potassium sodium tartrate and the na's reagent, and then the mixing reaction is carried out.
8. The method for measuring the content of ammonia nitrogen in the chlorine-containing wastewater according to claim 7, wherein the concentration of the first silver nitrate in the mixed reagent is in a range of 0.007 to 0.009mol/L, such as 0.008 mol/L;
and/or the concentration range of the mercury sulfate in the mixed reagent is 0.005-0.006 mol/L, such as 0.0056 mol/L;
and/or the concentration range of the sodium thiosulfate in the mixed reagent is 0.0015-0.002 mol/L, such as 0.0018 mol/L;
and/or the concentration range of the potassium sodium tartrate in the mixed reagent is 0.38-0.42 mol/L, for example 0.4 mol/L.
9. The method for measuring the content of ammonia nitrogen in chlorine-containing wastewater according to claim 1, wherein the content of chloride ions in the wastewater before chlorine removal is 1000-15000 mg/L.
10. The application of the method for determining the content of ammonia nitrogen in chlorine-containing wastewater according to claims 1-9 in the chlorine-containing wastewater in the pharmaceutical, food or chemical industry.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113607666A (en) * | 2021-07-27 | 2021-11-05 | 陕西师范大学 | Method for measuring ammonia nitrogen content in water by utilizing silver nanoparticles generated by improved silver mirror reaction |
| CN113607666B (en) * | 2021-07-27 | 2024-05-17 | 陕西师范大学 | Method for measuring ammonia nitrogen content in water by utilizing silver nanoparticles generated by improved silver mirror reaction |
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