CN106568816A - Reagent and method for rapidly measuring ammonia nitrogen content of oil refining sewage through electrode method - Google Patents
Reagent and method for rapidly measuring ammonia nitrogen content of oil refining sewage through electrode method Download PDFInfo
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- CN106568816A CN106568816A CN201610941654.3A CN201610941654A CN106568816A CN 106568816 A CN106568816 A CN 106568816A CN 201610941654 A CN201610941654 A CN 201610941654A CN 106568816 A CN106568816 A CN 106568816A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention aims to provide a reagent and method for rapidly measuring the ammonia nitrogen content of oil refining sewage through an electrode method. The method is rapid and efficient, and the operation is quick and efficient. The reagent is composed of a standard solution and a buffer solution. The standard solution is an ammonium chloride solution. The buffer solution is a mixed solution of sodium hydroxide, sodium potassium tartrate tetrahydrate, and EDTA (Ethylene Diamine Tetraacetic Acid), wherein the mass percentage of sodium hydroxide: sodium potassium tartrate tetrahydrate: EDTA is 40-200: 28.2-141: 7.44-74.4. During the measuring process, sodium hydroxide in the buffer solution is used to adjust the pH value of a water sample until the pH value of the water sample reaches more than 11; sodium potassium tartrate tetrahydrate and EDTA can eliminate the interference of multiple metal ions such as aluminum, zinc, cadmium, copper, iron, and the like; and thus the reagent is very suitable for measuring the ammonia nitrogen content of oil refining sewage.
Description
Technical field
The invention belongs to environmental monitoring, is related to the reagent that a kind of electrode method quickly determines ammonia-nitrogen content in oil refining sewerage
And method.
Background technology
Petrochemical industry is the pillar industry of Chinese national economy development, is the important industry for being related to national economy.In refining
During oil, the sewage containing ammonia nitrogen can be produced, when sewage is processed, its ammonia-nitrogen content is measured.At present oil refining is dirty
The measure of water ammonia nitrogen generally using the National Standard Method of Determination such as colorimetry or distillation titrimetry, needs numerous and diverse processing procedure, required
Reagent is more and minute is long, and is easily affected by water quality components.Especially petrochemical effluent composition is complicated, is disturbed
Complicated components are changeable.Ammonia nitrogen in determination of electrode water sample, with being not required to that pretreatment, interference factor be few and inspection range width etc. is excellent
Point, is a kind of environmental protection, fast and accurately simplicity, the high Two N-ammoniacal Measurements of degree and degree of accuracy, in other sewage treatment areas prisons
Survey has application, but the ammonia nitrogen that traditional electrode method is determined in oil refining sewerage is rarely reported, and reason is that oil refining sewerage water quality is more complicated, is contained
There is more metal ion, this can be interfered to measure.Therefore, research and develop it is simple, rapidly and efficiently, the electricity of low cost
Pole method quickly determines the reagent and method of ammonia-nitrogen content in oil refining sewerage, with stronger realistic meaning.
The content of the invention
It is an object of the invention to provide a kind of electrode method simple to operate, rapidly and efficiently quickly determines ammonia in oil refining sewerage
The reagent and method of nitrogen content.
The electrode method of the present invention quickly determines the reagent of ammonia-nitrogen content in oil refining sewerage by standard solution and buffer solution structure
Into the standard solution is ammonium chloride solution；The buffer solution is sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, ethylenediamine
The mixed solution of tetraacethyl disodium, the sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, disodiumedetate are molten in buffering
Mass percent in liquid is 40～200：28.2～141：7.44～74.4；The quality percentage of ammonium chloride in the standard solution
Concentration is with the ratio of the mass percentage concentration of sodium hydroxide in buffer solution：10.956：40～200.
Further, it is preferable to scheme be the sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, disodiumedetate
Mass percent in buffer solution is 100：70.5：18.6；In the standard solution mass percentage concentration of ammonium chloride with
The ratio of the mass percentage concentration of sodium hydroxide is in buffer solution：10.956：100.
Above-mentioned electrode method quickly determines the method for the reagent of ammonia-nitrogen content in oil refining sewerage and comprises the steps：
A：Buffer solution is put in water sample to be measured, and is stirred, with acidometer the current potential of water sample to be measured is measured, treat current potential
The reading of acidometer under numerical stability postscript；
B：Standard solution is added in water sample to be measured, with acidometer the current potential of water sample to be measured is measured, treat the stable postscript of potential value
The reading of lower acidometer；
C：According to the potential difference of the step of A, B two, the ammonia nitrogen concentration in water sample to be measured is calculated by the computing formula of standard addition method.
Further, when the water sample to be measured for high-concentration ammonia-nitrogen is measured, it is likely to result in measurement result inaccurate
Situation, present invention particularly provides following solutions：In the step C, when the ammonia nitrogen concentration of calculated water sample to be measured
During more than 40 mg/L, then water sample to be measured is extracted again, and water sample to be measured is diluted into prearranged multiple, then re-execute A, B, C step
Suddenly, until the ammonia nitrogen concentration of water sample to be measured for obtaining is in the range of 0～40mg/L, then by the ammonia nitrogen of resulting water sample to be measured
Concentration is multiplied by the multiple that water sample to be measured is diluted, and obtains the ammonia nitrogen concentration of final water sample to be measured.
Further, during said determination, the buffer solution, standard solution, the volume ratio of water sample to be measured are 1：
0. 25：25.
The principle of above-mentioned determination of electrode ammonia nitrogen is：Using ammonia gas-sensing electrode, it is a kind of combination electrode, with pH vitreors electricities
Extremely indicating electrode, silver-silver chloride electrode is reference electrode.Electrode is placed in plastic bushing, 0.1mol/L chlorinations are inside filled
Ammonium internal-filling liquid, and equipped with air-sensitive film.PH regulator liquid is added first toward water sample to be measured（That is buffer solution）, by pH bring up to 11 with
On, make ammonium salt be converted into ammonia, because diffusion is by air-sensitive film, ammonia is entered after internal-filling liquid the ammonia of generation, there is following balance：
NH3+H2O=NH4 ++OH-, the generation of ammonia makes reaction move right so that the pH value of internal-filling liquid is raised with the entrance of ammonia, in perseverance
Fixed ionic strength, electrode parameter and at a temperature of the electromotive force that measures, meet Nernst equation with ammonia nitrogen concentration in water sample.Thus
Can from the water sample potential value for measuring, so that it is determined that in water sample ammonia nitrogen content.
Sodium hydroxide in buffer solution is used to adjust water sample pH value to be measured so as to reach more than 11, and in buffer solution
Sodium potassium tartrate tetrahydrate tetrahydrate and disodiumedetate can eliminate the interference of many kinds of metal ions, for example aluminum, zinc,
Cadmium, copper, ferrum etc. so that reagent is very suitable for the measure of ammonia-nitrogen content in oil refining sewerage.
The computing formula of above-mentioned standard addition method is Cx=C△(10n△E/S-1)-1；Wherein C△=28.67mg/L, S=59.16, n=
1.For example：Certain solution to be measured is surveyed, after adding buffer solution, then reading potential E1 after current potential is stable adds standard solution,
Reading potential E2 after current potential is stable, by E1-E2 △ E are drawn, substituting into above-mentioned formula can calculate the ammonia nitrogen of the solution to be measured
Concentration C x.
The reagent type for adopting of the invention is less, configuration is simple, low cost；Using method it is simple to operate, rapidly and efficiently,
As a result it is accurate, it is adaptable to the measure of ammonia nitrogen in oil refining sewerage, the work efficiency of refinery environment monitoring department can be greatly improved.
Specific embodiment
Below by the description to embodiment, the shape of each component for example involved to the specific embodiment of the present invention
Mutual alignment and annexation, the effect of each several part and operation principle between shape, construction, each several part etc. are made further detailed
Explanation.
Embodiment 1：
The electrode method of the present embodiment quickly determines the reagent of ammonia-nitrogen content in oil refining sewerage and is made up of standard solution and buffer solution,
The standard solution is ammonium chloride solution, and the mass percentage concentration of the ammonium chloride in standard solution is 10.956 g/L；Buffering is molten
Liquid is sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, the mixed solution of disodiumedetate, each composition in buffer solution
Mass percentage concentration it is as follows：Sodium hydroxide：40 g/L；Sodium potassium tartrate tetrahydrate tetrahydrate：28.2 g/L；Ethylenediaminetetraacetic acid two
Sodium：7.44 g/L.
Using mentioned reagent and electrode method to carry out oil refining sewerage in ammonia nitrogen concentration determine process it is as follows：
A：Buffer solution 2ml is put in the water sample to be measured of 50ml, and is stirred, with acidometer the electricity of water sample to be measured is measured
Position, treats the reading E1 of acidometer under the stable postscript of potential value；
B：Add the standard solution of 0.5ml in above-mentioned water sample to be measured again, with acidometer the current potential of water sample to be measured is measured, treat current potential
The reading E2 of acidometer under numerical stability postscript；
C：Potential difference according to measured by the step of A, B two, the ammonia nitrogen in water sample to be measured is calculated by the computing formula of standard addition method
Concentration.
The computing formula of standard addition method is Cx=C△(10n△E/S-1)-1；Wherein C△=28.67mg/L, S=59.16, n=1, by
E1-E2 draws △ E, and substituting into above-mentioned formula can calculate the ammonia nitrogen concentration Cx of the solution to be measured.
In the step C, when the ammonia nitrogen concentration Cx of calculated water sample to be measured is more than 40 mg/L, then extract again
Water sample to be measured, and water sample to be measured is diluted into prearranged multiple, then re-executes A, B, step C, until the ammonia of water sample to be measured for obtaining
Nitrogen concentration Cx is in the range of 0～40mg/L, then that the ammonia nitrogen concentration Cx of resulting water sample to be measured is multiplied by into water sample institute to be measured is dilute
The multiple released, obtains the ammonia nitrogen concentration Cx of final water sample to be measured.
Embodiment 2：
The mass percentage concentration of the ammonium chloride in standard solution in the present embodiment is still 10.956 g/L, different from embodiment 1
, in the present embodiment, the mass percentage concentration of each composition in buffer solution is as follows：Sodium hydroxide：100 g/L；Winestone
Sour potassium sodium tetrahydrate：70.5 g/L；Disodiumedetate：18.6g/L.
The assay method of the present embodiment is same as Example 1, and here is omitted.
Embodiment 3：
The mass percentage concentration of the ammonium chloride in standard solution in the present embodiment is still 10.956 g/L, with embodiment 1 and 2 not
With in the present embodiment, the mass percentage concentration of each composition in buffer solution is as follows：Sodium hydroxide：200 g/L；Wine
Stone acid potassium sodium tetrahydrate：141g/L；Disodiumedetate：74.4g/L.
The assay method of the present embodiment is same as Example 1, and here is omitted.
The water sample to be measured of above three embodiment is certain water inlet of oil plant oil interceptor, Aerobic Pond O1Water outlet, secondary clarifier effluent are same
One batch water sample, the reagent for implementing row by above-mentioned 3 kinds and method and standard method《Measure distillation-the acid-base titration of Water quality ammonia nitrogen
Method》Measurement result compares, and the results are shown in Table 1.As a result show, the measurement result of three embodiments is all tied with the measure of standard method
Fruit is more or less the same, and wherein the measurement result error rate of embodiment 2 is minimum, so the buffer solution chosen described in embodiment 2 is matched somebody with somebody
Than for optimal proportion.
Table 1：The measurement result of each embodiment compares（Unit：mg/L）
Claims (5)
1. a kind of electrode method quickly determines the reagent of ammonia-nitrogen content in oil refining sewerage, it is characterised in that molten by standard solution and buffering
Liquid is constituted, and the standard solution is ammonium chloride solution；The buffer solution is sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, second
The mixed solution of edetate disodium, the sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, disodiumedetate are slow
The mass percent rushed in solution is 40～200：28.2～141：7.44～74.4；The quality of ammonium chloride in the standard solution
Percentage concentration is with the ratio of the mass percentage concentration of sodium hydroxide in buffer solution：10.956：40～200.
2. electrode method according to claim 1 quickly determines the reagent of ammonia-nitrogen content in oil refining sewerage, it is characterised in that institute
Sodium hydroxide, sodium potassium tartrate tetrahydrate tetrahydrate, mass percent of the disodiumedetate in buffer solution are stated for 100：
70.5：18.6；The mass percentage concentration of ammonium chloride is dense with the quality percentage of sodium hydroxide in buffer solution in the standard solution
The ratio of degree is：10.956：100.
3. reagent according to claim 1 carries out the method that electrode method quickly determines ammonia-nitrogen content in oil refining sewerage, and it is special
Levy is to comprise the steps：
A：Buffer solution is put in water sample to be measured, and is stirred, with acidometer the current potential of water sample to be measured is measured, treat current potential
The reading of acidometer under numerical stability postscript；
B：Standard solution is added in water sample to be measured, with acidometer the current potential of water sample to be measured is measured, treat the stable postscript of potential value
The reading of lower acidometer；
C：According to the potential difference of the step of A, B two, the ammonia nitrogen concentration in water sample to be measured is calculated by the computing formula of standard addition method.
4. the method that electrode method according to claim 3 quickly determines ammonia-nitrogen content in oil refining sewerage, it is characterised in that institute
In stating step C, when the ammonia nitrogen concentration of calculated water sample to be measured is more than 40 mg/L, then water sample to be measured is extracted again, and will
Water sample to be measured dilutes prearranged multiple, then re-executes A, B, step C, until the ammonia nitrogen concentration of water sample to be measured that obtains in 0～
In the range of 40mg/L, then the ammonia nitrogen concentration of resulting water sample to be measured is multiplied by into the multiple that water sample to be measured is diluted, obtains final
Water sample to be measured ammonia nitrogen concentration.
5. the method that the electrode method according to claim 3 or 4 quickly determines ammonia-nitrogen content in oil refining sewerage, it is characterised in that
The buffer solution, standard solution, the volume ratio of water sample to be measured are 1：0. 25：25.
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Cited By (5)
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| CN110849874A (en) * | 2019-12-05 | 2020-02-28 | 深圳市海聚源水产科技有限公司 | Ammonia nitrogen detection reagent formula suitable for high organic matter content culture water body and application |
| CN111879597A (en) * | 2020-07-20 | 2020-11-03 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
| CN112067416A (en) * | 2020-09-22 | 2020-12-11 | 广东石油化工学院 | Buffer solution and method for measuring ammonia nitrogen content in sewage by electrode method |
| EP3967738A1 (en) | 2020-09-15 | 2022-03-16 | Socar Turkey Enerji A.S. | Estimation method of nitrogen content in the hydrocracker reactor feedstock for temperature optimization |
| CN114252486A (en) * | 2021-12-28 | 2022-03-29 | 南通化学环境监测站有限公司 | Method for detecting ammonia nitrogen content in sewage |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110849874A (en) * | 2019-12-05 | 2020-02-28 | 深圳市海聚源水产科技有限公司 | Ammonia nitrogen detection reagent formula suitable for high organic matter content culture water body and application |
| CN111879597A (en) * | 2020-07-20 | 2020-11-03 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
| CN111879597B (en) * | 2020-07-20 | 2023-12-05 | 广东石油化工学院 | Buffer solution for detecting nitrate nitrogen in domestic sewage and detection method |
| EP3967738A1 (en) | 2020-09-15 | 2022-03-16 | Socar Turkey Enerji A.S. | Estimation method of nitrogen content in the hydrocracker reactor feedstock for temperature optimization |
| CN112067416A (en) * | 2020-09-22 | 2020-12-11 | 广东石油化工学院 | Buffer solution and method for measuring ammonia nitrogen content in sewage by electrode method |
| CN114252486A (en) * | 2021-12-28 | 2022-03-29 | 南通化学环境监测站有限公司 | Method for detecting ammonia nitrogen content in sewage |
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Application publication date: 20170419 |