CN108168988A - The assay method of ammonia nitrogen in a kind of high calcium waste water - Google Patents
The assay method of ammonia nitrogen in a kind of high calcium waste water Download PDFInfo
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- CN108168988A CN108168988A CN201711129359.9A CN201711129359A CN108168988A CN 108168988 A CN108168988 A CN 108168988A CN 201711129359 A CN201711129359 A CN 201711129359A CN 108168988 A CN108168988 A CN 108168988A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention discloses a kind of assay methods of ammonia nitrogen in high calcium waste water, belong to water quality index and measure field.Since Berthelot spectrophotometry surveys the calcium ion in the tartaric acid meeting complexing moiety high calcium waste water added in during ammonia nitrogen, calcium tartrate solubility is relatively low, when calcium ion concentration is higher, Calcium Tartrate is easily precipitated and then interferes colorimetric.The present invention carries out pretreatment using sodium carbonate and eliminates calcium ion interference, first adjusts pH value of waste water to 8 ~ 9, adds 20g/L sodium carbonate, form precipitation of calcium carbonate, utilize 0.45 μm of membrane filtration；Then it takes in a certain amount of filtrate to colorimetric cylinder, its ammonia nitrogen concentration is measured using Berthelot spectrophotometry.The present invention can completely eliminate the interference of calcium ion, easy to operate, and relative error is no more than 3%, can meet the requirement of water-quality determination.
Description
Technical field
The invention belongs to water-quality determination fields, and in particular to the assay method of ammonia nitrogen in a kind of high calcium waste water.
Background technology
The contaminated object that ammonia nitrogen is an important indicator of body eutrophication and every profession and trade mainly controls at present, and
Pollutant emission standard is electroplated（GB21900-2008）Middle three standard of table is 8 mg/L to the emission request of ammonia nitrogen.Milk of lime neutralizes
Method is widely used in the processing of electroplating wastewater, introduces a large amount of calcium ion, concentration is up to 1000 more than mg/L, while waste water passes through
After crossing reverse osmosis membrane concentration, calcium ion higher in the waste water of discharge.Therefore, the low ammonia nitrogen of high-calcium ionic is presented in plating waste discharge
Feature.
The method for measuring ammonia nitrogen at present has spectrophotometry, electrode method and gas molecule in space absorption process, due to by cost
Control, spectrophotometry are and the wherein nessler reagent spectrophotometrics in a kind of most widely used method of most of sewage treatment plant
Method is the most universal.According to HJ535-2009《The measure Berthelot spectrophotometry of Water quality ammonia nitrogen》In introduce calcium and magnesium ion meeting
Interference is generated to ammonia nitrogen determination, suitable potassium sodium tartrate solution can eliminate interference, but not generate the dense of interference to calcium and magnesium ion
Degree illustrates.The paper delivered according to carbuncle et al. is killed《The influence and disappear that calcium and magnesium ion measures Liquor-making industry ammonia nitrogen in waste water
It removes》Described, when calcium ion concentration is more than 15 mg/L, after being developed the color using Na's reagent, solution is gradually muddy, there is graininess
Suspended matter generates, and measurement deviation is big, and the interference problem of calcium ion can be solved by extension rate method.Therefore, using nessler reagent
Method measures the ammonia nitrogen in high-calcium ionic waste water, it is necessary to take corresponding preprocess method.Although mark-on dilution method can eliminate calcium
The influence of ion, but the waste water that calcium ion is high and ammonia nitrogen is low is directed to, excessive extension rate will influence low-concentration ammonia-nitrogen in waste water
Measurement result.In addition, calcium ion effect is completely eliminated using the way of distillation, but operation is cumbersome, and distill consumption electricity
Energy.
Therefore, it there is an urgent need for proposing a kind of method that low-concentration ammonia-nitrogen high calcium waste water is measured suitable for Na's reagent, eliminates
The interference of calcium ion to meet the accuracy measured and accuracy, and simplifies ammonia nitrogen pretreatment process, be water quality monitoring and
The adjustment of technique provides accurate data.
Invention content
The present invention is intended to provide one kind effectively eliminates high concentration calcium ion interference, the side of Accurate Determining water sample low-concentration ammonia-nitrogen
Method.
It is small to be less than 7500 mg/L, ammonia nitrogen concentration suitable for calcium ion concentration for the assay method of ammonia nitrogen in a kind of high calcium waste water
In the water sample of 8 mg/L, this method is measured ammonia nitrogen using Berthelot spectrophotometry, it is characterised in that utilizes carbonic acid
Sodium carries out high calcium waste water pretreatment and eliminates calcium ion interference, and process specific steps include：
（1）100 mL of high concentration calcic waste water is taken, if pH value is less than 8, the NaOH for adding in 10% adjusts pH most 8 ~ 9, if pH value
More than 8, then pH need not be adjusted, then add in 2 g sodium carbonate and react 2 min, after 10 ~ 20 min precipitations, supernatant be taken to note
Emitter and 0.45 μm of membrane filtration；
（2）The filtrate of certain volume is taken to be settled to 25 mL in 25 mL color-comparison tubes with distilled water, it is dense first to add in 0.5 mL
Spend the sodium potassium tartrate tetrahydrate for 500 g/L, mixing is rear to add in 0.75 mL nessler reagents, mixing, after 10 min that develop the color, in 420 nm
Measure absorbance.
With the pretreatment of existing ammonia nitrogen compared with assay method, the invention has the advantages that：
（1）Influence of the removal calcium ion to measurement result is precipitated, and to ammonia nitrogen without co-precipitation, operation letter using sodium carbonate
Single, error is small；
（2）Using 25 mL color-comparison tubes, compared with 50 mL than national regulations, the usage amount of harmful substance is reduced, is subtracted
Few environmental hazard；
（3）Compared with the way of distillation pre-processes, the present invention is easy to operate, and equipment requirement is low, without consuming electric energy.
Specific embodiment
Embodiment 1
The ammonia nitrogen simulated wastewater of distilled water configuration is measured using this method, wherein ammonia nitrogen concentration is respectively 0.5 mg/L, 1 mg/L
With 2 mg/L, each ammonia nitrogen concentration sets calcium ion concentration as 100 mg/L, 1000 mg/L and 5000 mg/L respectively, as a result such as
Shown in table 1.The result shows that sodium carbonate can effectively eliminate high concentration calcium ion interference, process is generated without precipitation, and sodium carbonate is to aobvious
Color is no more than 3% without influence, relative error.
Table 1 measures ammonia nitrogen simulated wastewater using method provided by the invention
Embodiment 2
Actual waste water derives from the 4 electroplating sewerage treatment plant floss holes and 1 reverse osmosis concentrated water using milk of lime processing, wherein
Calcium ion concentration is 1000 ~ 5000 mg/L, respectively after the pretreatment of direct measuring method, the way of distillation and method of the present invention,
Again ammonia nitrogen is measured with Na's reagent.The result shows that if not preprocessed, calcium ion seriously affects the measure of ammonia nitrogen, and error is very
Greatly, it distills method for pretreating and the method for the present invention surveys that ammonia nitrogen concentration is close, and relative standard deviation is no more than 2.5%.
Influence of the 2 different pretreatments method of table to low-concentration ammonia-nitrogen concentration mensuration result in high calcium waste water
Claims (1)
1. the assay method of ammonia nitrogen in a kind of high calcium waste water is less than 7500 mg/L suitable for calcium ion concentration, ammonia nitrogen concentration is less than
The water sample of 8 mg/L, this method are measured ammonia nitrogen using Berthelot spectrophotometry, it is characterised in that utilize sodium carbonate
Pretreatment is carried out to high calcium waste water and eliminates calcium ion interference, process specific steps include：
（1）100 mL of high calcium waste water is taken, if pH value is less than 8, the NaOH for adding in 10% adjusts pH to 8 ~ 9, if pH value is more than 10,
PH need not be then adjusted, 2 g sodium carbonate is then added in and reacts 2 min, after precipitating 10 ~ 20 min, supernatant is taken, with 0.45 μm of filter
Membrane filtration；
（2）The filtrate of certain volume is taken to be settled to 25 mL in 25 mL color-comparison tubes with distilled water, first add in 0.5 mL's
500 g/L sodium potassium tartrate tetrahydrates, mixing, add in 0.75 mL nessler reagent, mixing, develop the color 10 min after, in 420 nm measure inhale
Luminosity.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113916815A (en) * | 2021-10-13 | 2022-01-11 | 海南大学 | Method for measuring content of ammonia nitrogen in seawater by using Nashin's reagent spectrophotometry |
Citations (7)
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|---|---|---|---|---|
| CN1958471A (en) * | 2005-10-31 | 2007-05-09 | 中国石油化工股份有限公司 | Method for treating ammonia nitrogen wastewater |
| CN102001774A (en) * | 2010-12-28 | 2011-04-06 | 湘潭大学 | Alkaline high-calcium wastewater decalcification treatment method |
| CN102735627A (en) * | 2012-06-20 | 2012-10-17 | 苏州国环环境检测有限公司 | Spectrophotometric method for determining ammonia nitrogen content in water |
| CN104034681A (en) * | 2014-06-26 | 2014-09-10 | 南通永康检测技术有限公司 | Method for detecting content of ammonia nitrogen in sewage |
| CN105334208A (en) * | 2015-04-09 | 2016-02-17 | 中国科学院城市环境研究所 | Method for determining ammonia nitrogen in trace amount of solution under interference of iron and copper metal ions |
| CN106007272A (en) * | 2016-08-11 | 2016-10-12 | 桂琪 | Biochemical treatment method and apparatus for high calcium and high magnesium waste water |
| CN107162264A (en) * | 2017-06-07 | 2017-09-15 | 江苏龙净科杰催化剂再生有限公司 | The minimizing technology of calcium ion in useless denitrating catalyst regeneration treatment waste water |
-
2017
- 2017-11-15 CN CN201711129359.9A patent/CN108168988A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1958471A (en) * | 2005-10-31 | 2007-05-09 | 中国石油化工股份有限公司 | Method for treating ammonia nitrogen wastewater |
| CN102001774A (en) * | 2010-12-28 | 2011-04-06 | 湘潭大学 | Alkaline high-calcium wastewater decalcification treatment method |
| CN102735627A (en) * | 2012-06-20 | 2012-10-17 | 苏州国环环境检测有限公司 | Spectrophotometric method for determining ammonia nitrogen content in water |
| CN104034681A (en) * | 2014-06-26 | 2014-09-10 | 南通永康检测技术有限公司 | Method for detecting content of ammonia nitrogen in sewage |
| CN105334208A (en) * | 2015-04-09 | 2016-02-17 | 中国科学院城市环境研究所 | Method for determining ammonia nitrogen in trace amount of solution under interference of iron and copper metal ions |
| CN106007272A (en) * | 2016-08-11 | 2016-10-12 | 桂琪 | Biochemical treatment method and apparatus for high calcium and high magnesium waste water |
| CN107162264A (en) * | 2017-06-07 | 2017-09-15 | 江苏龙净科杰催化剂再生有限公司 | The minimizing technology of calcium ion in useless denitrating catalyst regeneration treatment waste water |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113916815A (en) * | 2021-10-13 | 2022-01-11 | 海南大学 | Method for measuring content of ammonia nitrogen in seawater by using Nashin's reagent spectrophotometry |
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Application publication date: 20180615 |