CN101551328B - Resonance scattering spectrometry for rapidly measuring ammonia nitrogen in water - Google Patents
Resonance scattering spectrometry for rapidly measuring ammonia nitrogen in water Download PDFInfo
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- CN101551328B CN101551328B CN2009101140959A CN200910114095A CN101551328B CN 101551328 B CN101551328 B CN 101551328B CN 2009101140959 A CN2009101140959 A CN 2009101140959A CN 200910114095 A CN200910114095 A CN 200910114095A CN 101551328 B CN101551328 B CN 101551328B
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Abstract
The present invention discloses a resonance scattering spectrometry for measuring ammonia nitrogen in water rapidly, the measurement steps is that 1. a standard system of ammonium muriate is prepared,and a scattering intensity I is mensurated at a point of 447m; 2. a blank system without ammonium muriate is prepared, and a scattering intensity I0 is mensurated; 3. calculation of Delta I447m = I-I0; 4. a working curve is made according to the concentration relation of the Delta I447m to the ammonium muriate; 5. a detection system is prepared by adding a measuring object containing ammonium muriate with ignorance concentration, and Delta I447M of the measuring system is obtained; 6. according to the working curve, the ammonium muriate concentration of the measuring object is calculated. Comparing with the existing method, the instrument of the method of the invention is simple, operation is easy, reagent is obtained easily, sensitivity is high, measurement range is wide, and cost is low.
Description
Technical field
The present invention relates to the analytical chemistry field, specifically is the resonance scattering spectrometry of ammonia nitrogen in the fast measuring water.
Background technology
Ammonia nitrogen extensively is present in river, river, lake, sea and surface water and the underground water, is one of important indicator of water body quality assessment.What of nitrogen compound in the water can be used as the index that water body is subjected to the itrogenous organic substance pollution level.The method of measuring ammonia nitrogen at present mainly contains Na Shi colourimetry, phenol-hypochlorite (or salicylic acid-hypochlorite) colourimetry, electrode method and distillation-titrimetry.The Na Shi colourimetry is the classical assay method of ammonia, is classified as standard method of analysis by many countries.The method insufficient sensitivity height that in these assay methods, has, metallic ion, sulfide, aldehyde and ketone, water samples such as calcium, magnesium and iron have color in the water sample, and muddy, contain all influence mensuration such as other interfering materials, need do corresponding pre-service, the time of mensuration is long, complex operation.
Summary of the invention
The objective of the invention is for overcoming the deficiencies in the prior art, and the resonance scattering spectrometry of ammonia nitrogen in a kind of simple fast measuring water is provided.
Realize that purpose technical scheme of the present invention is: utilize the alkaline solution of mercuric iodixde and potassium iodide and ammonia react to generate fallow colloidization compound, ammonia nitrogen is along with the increase of its concentration, its resonance scattering intensity is linear to be strengthened, adopt fluorospectrophotometer that the fallow colloidization compound that generates is carried out synchronous scanning and obtain resonance scattering spectroscopy, according to the linear relationship of resonance scattering intensity and ammonium chloride concentration, the ammonia nitrogen in the fast measuring water.
Use ammonia nitrogen in the resonance scattering spectrometry fast measuring water, comprise the steps:
(1) the standard testing system of preparation ammonium chloride: in the 5mL color comparison tube, add 0.3mL 1.77mol/L potassium sodium tartrate solution successively, the 0.1mL nessler reagent, mixing, the ammonium chloride standard solution of adding 1-150 μ L, 10 μ g/mL, mixing, add no ammoniacal liquor again to 5.0mL, room temperature is placed 20min;
(2) do not add the ammonium chloride titer with the preparation of the method for step (1) and prepare the blank system;
(3) get above-mentioned system respectively in different quartz cells, on fluorospectrophotometer, equal in excitation wavelength under the condition of emission wavelength, synchronous scanning, obtain the synchro-resonance scattering spectrum of system, the resonance scattering intensity I at bioassay standard system 447nm place, the resonance scattering intensity of blank testing control systems is I
0, calculate Δ I
447nm=I-I
0
(4) with Δ I
447nmConcentration relationship workmanship to ammonium chloride makes curve;
(5) method according to step (1) prepares detection architecture, and wherein the ammonium chloride of Jia Ruing is to contain ammonium chloride but the measured object of unknown concentration, obtains the Δ I of measured object
447nm
(6), calculate the concentration of the ammonium chloride of measured object according to the working curve of (4).
Nessler reagent described in the step (1) is dissolved in the 25mL water for taking by weighing the 20g potassium iodide, gradation while stirring adds about 10g mercuric chloride on a small quantity, when vermilion precipitation occurring and be difficult for dissolving, change into and drip saturated liquor hydrargyri perchloridi, and fully stir, when the micro-vermilion precipitation of appearance is no longer dissolved, stop to drip saturated liquor hydrargyri perchloridi; This solution is injected the potassium hydroxide solution of 250mL 4.2857mol/L slowly, be diluted with water to 400mL, mixing is nessler reagent.
No ammoniacal liquor described in the step (1) is to obtain by adding the distillation of the 0.1mL concentrated sulphuric acid in every liter of distilled water.
Advantage of the present invention is: compare with existent method, the instrument of this assay method is simple, and is easy and simple to handle, and reagent is easy to get, and is highly sensitive, and measurement range is wide, and is with low cost.
Description of drawings:
Fig. 1 is the resonance light scattering spectrogram of specific embodiment of the invention ammonium chloride solution.
Among the figure: a. ammonium chloride testing standard system b. blank system
Embodiment
(1) standards system of preparation ammonium chloride: in 5 5mL color comparison tubes, add 0.3mL 1.77mol/L potassium sodium tartrate solution respectively successively, 0.1mL nessler reagent, mixing, pipetting concentration with liquid-transfering gun then is that the ammonium chloride standard solution 1-150 μ L of 10 μ g/mL injects 5 colour tubes respectively, mixing adds no ammoniacal liquor again to 5.0mL, and room temperature is placed 20min;
(2) method with step (1) prepares the blank system, does not add the ammonium chloride titer;
(3) get above-mentioned system respectively in different quartz cells, on fluorospectrophotometer, synchronous scanning excitation wavelength lambda ex and emission wavelength lambda em (λ ex=λ em), obtain the synchro-resonance scattering spectrum of system, the resonance scattering intensity of measuring the 447nm place is I, and reagent blank is the resonance scattering intensity I
0, calculate Δ I
447nm=I-I
0
(4) with Δ I
447nmConcentration relationship workmanship to ammonium chloride makes curve;
(5) according to the method for step (1), prepare test system, wherein add the measured object that contains ammonium chloride of unknown concentration, obtain the Δ I of tested systems
447nm
(6) can obtain ammonium chloride concentration in the unknown sample according to the working curve equation.
Claims (1)
1. the resonance scattering spectrometry of ammonia nitrogen in the fast measuring water, it is characterized in that: assay method comprises that step is as follows:
(1) standards system of preparation ammonium chloride: in the 5mL color comparison tube, add 0.3mL 1.77mol/L potassium sodium tartrate solution successively, 0.1mL nessler reagent, mixing, the ammonium chloride standard solution that adds 1-150 μ L 10 μ g/mL, mixing, add no ammoniacal liquor again to 5.0mL, room temperature is placed 20min, and described nessler reagent is dissolved in the 25mL water for taking by weighing the 20g potassium iodide, gradation while stirring adds about 10g mercuric chloride on a small quantity, when vermilion precipitation occurring and be difficult for dissolving, change into and drip saturated liquor hydrargyri perchloridi, and fully stir, when the micro-vermilion precipitation of appearance is no longer dissolved, stop to drip saturated liquor hydrargyri perchloridi; This solution is injected the potassium hydroxide solution of 250mL 4.2857mol/L slowly, be diluted with water to 400mL, mixing makes;
(2) do not add the ammonium chloride titer with the method for step (1) and prepare the blank system;
(3) get above-mentioned system respectively in different quartz cells, on fluorospectrophotometer, equal in excitation wavelength under the condition of emission wavelength, synchronous scanning, obtain the synchro-resonance scattering spectrum of standards system, the resonance scattering intensity of measuring the 447nm place is I, and the resonance scattering intensity of reagent blank control systems is I
0, calculate Δ I
447nm=I-I
0
(4) with Δ I
447nmConcentration relationship workmanship to ammonium chloride makes curve;
(5) method according to step (1) prepares detection architecture, wherein add for to contain ammonium chloride but the measured object of unknown concentration, obtain the Δ I of tested systems
447nm
(6), calculate the concentration of the ammonium chloride of measured object according to the working curve of (4).
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| CN101551328B true CN101551328B (en) | 2011-02-16 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102645422B (en) * | 2012-04-13 | 2014-04-16 | 广西师范大学 | Method for measuring pipemidic acid by using resonance scattering spectrum |
| CN103353448A (en) * | 2013-07-19 | 2013-10-16 | 广西师范大学 | Resonant rayleigh scattering spectrometry scattering method for measuring dissolved oxygen |
| CN103389291A (en) * | 2013-07-19 | 2013-11-13 | 广西师范大学 | Resonance Rayleigh scattering spectrum method for formaldehyde determination |
| CN103604792A (en) * | 2013-11-29 | 2014-02-26 | 广西师范大学 | Resonance Rayleigh scattering (RRS) method for measuring bromide ion |
| CN104034721A (en) * | 2014-04-14 | 2014-09-10 | 西北农林科技大学 | Detection method of ammoniacal nitrogen in fermenting liquid |
| CN104535506A (en) * | 2015-01-30 | 2015-04-22 | 四川清和科技有限公司 | Drainage basin ammonia-nitrogen concentration detection method |
| CN107870152A (en) * | 2017-08-16 | 2018-04-03 | 广西师范大学 | It is a kind of to regulate and control nano silicon active absorption spectroscopic assay Hg with aptamers2+Method |
| CN112964654A (en) * | 2021-01-28 | 2021-06-15 | 上海中西三维药业有限公司 | Method for determining content of ammonia nitrogen in chlorine-containing wastewater and application thereof |
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| CN101319999A (en) * | 2008-04-30 | 2008-12-10 | 河南农大迅捷测试技术有限公司 | Novel nessler's reagent and method for rapidly measuring soil ammonium nitrogen |
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| CN1387039A (en) * | 2001-05-17 | 2002-12-25 | 中国石化集团齐鲁石油化工公司 | Titration method for monitoring and analyzing potential of ammonical nitrogen in water |
| CN101158682A (en) * | 2007-11-19 | 2008-04-09 | 广西师范大学 | Enzyme catalysis tetrabutyl ammonium bromide syntony scattering spectrometry detecting trace amount H2O2 |
| CN101319999A (en) * | 2008-04-30 | 2008-12-10 | 河南农大迅捷测试技术有限公司 | Novel nessler's reagent and method for rapidly measuring soil ammonium nitrogen |
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