CN109187388A - A kind of colorimetry-turbidity compensation measuring method of Liquor-making industry ammonia nitrogen in waste water - Google Patents
A kind of colorimetry-turbidity compensation measuring method of Liquor-making industry ammonia nitrogen in waste water Download PDFInfo
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- CN109187388A CN109187388A CN201811031388.6A CN201811031388A CN109187388A CN 109187388 A CN109187388 A CN 109187388A CN 201811031388 A CN201811031388 A CN 201811031388A CN 109187388 A CN109187388 A CN 109187388A
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- 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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- 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
- G01N2021/3185—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry typically monochromatic or band-limited
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Abstract
The invention discloses a kind of colorimetry-turbidities of Liquor-making industry ammonia nitrogen in waste water to compensate measuring method, using Berthelot spectrophotometry, it does not need to pre-process, direct chromogenic assay absorbance, a blank sample need to be prepared, 2mL coloration-determining amount liquid is then added into sample, the coloration or turbidity in sample are eliminated, but sodium potassium tartrate tetrahydrate and nessler reagent solution is not added.Then the absorbance of blank sample is deducted from the absorbance of sample.This method is simple and efficient, accurate and reliable, meets the needs of Liquor-making industry ammonia nitrogen in waste water treatment process is adjusted in time.
Description
Technical field
The present invention relates to a kind of colorimetry-turbidities of Liquor-making industry ammonia nitrogen in waste water to compensate measuring method, belongs to ammonia nitrogen in waste water and surveys
Determine method field.
Background technique
Ammonia nitrogen is one of national water quality discharge index, it is desirable that outlet water concentration must reach national emission standard, so must
The content of palpus each stage Water quality ammonia nitrogen of strict control guarantees outer draining qualified discharge.The measuring method of ammonia nitrogen has nessler reagent point
Light photometry, distillation-neutralization titration etc..It can be in advance when sample is muddy or has color if being provided in Berthelot spectrophotometry
The way of distillation or flocculent precipitation processing, then nessler reagent chromogenic reaction is carried out, measure absorbance.Distillation-neutralization titration is sample
Product pass through pre-distillation, then titrate the ammonia nitrogen in distillate with hydrochloric acid standard solution, that is, measure the method for ammonia nitrogen concentration.It is above two
Pretreatment all have passed through for the sample containing colorimetry-turbidity in method, therefore sample measurement takes a long time, working efficiency is low.
Summary of the invention
The present invention is in order to avoid above-mentioned existing deficiencies in the technology, it is desirable to provide a kind of Liquor-making industry waste water ammonia
The colorimetry-turbidity of nitrogen compensates measuring method.
The colorimetry-turbidity of Liquor-making industry ammonia nitrogen in waste water of the present invention compensates measuring method, does not need to pre-process, and directly colour developing is surveyed
Determine absorbance, the absorbance of blank sample is then deducted from the absorbance of sample.This method is simple and efficient, accurately may be used
It leans on, is mainly used in the measurement of Liquor-making industry ammonia nitrogen in waste water content, instructs process operation in time.
Liquor-making industry waste water of the present invention is the waste liquid generated after the distillation of five grains is fermented, more after each link stepwise disposal
The general name of kind of waste water, wherein the waste water of most original is known as residual water, is in yellow, thick semisolid, thus such waste water have compared with
High coloration and turbidity.In the measurement of ammonia nitrogen, it need to consider to exclude the influence of coloration and turbidity to result.
The colorimetry-turbidity of Liquor-making industry ammonia nitrogen in waste water of the present invention compensates measuring method, using Berthelot spectrophotometry,
But it does not need to pre-process, direct chromogenic assay absorbance.Specifically comprise the following steps:
Step 1: the acquisition of sample
The acquisition of Liquor-making industry waste water is placed in polyethylene bottle or vial, and sample presentation is analyzed immediately;If Liquor-making industry
It needs to save after waste water acquisition, sulfuric acid should be added to make to be acidified to pH < 2 into Liquor-making industry waste water, can be reserved for 7 days at 2-5 DEG C;
Step 2: the drafting of calibration curve
The ammonia nitrogen of 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL are taken respectively
Standard working solution simultaneously be added 8 50mL colorimetric cylinders in, corresponding to ammonia-nitrogen content be respectively 0.0 μ g, 5.0 μ g, 10.0 μ g,
20.0 μ g, 40.0 μ g, 60.0 μ g, 80.0 μ g and 100 μ g, add water to graticule;Then to being separately added into 1.0mL winestone in colorimetric cylinder
Sour potassium sodium solution simultaneously shakes up, then is separately added into nessler reagent 1.0mL and shakes up, after standing 10min at wavelength 420nm, with water
Make reference measurement absorbance (20mm cuvette), using the absorbance after blank correction as ordinate, with its corresponding ammonia-nitrogen content
(μ g) is abscissa, draws calibration curve.
Density p=500g/L of the potassium sodium tartrate solution, process for preparation are as follows: weighing 50.0g sodium potassium tartrate tetrahydrate
(KNaC4H6O6·4H2O it) is dissolved in 100mL water, heating is boiled to drive away ammonia, is diluted to 100mL after being fully cooled.
The ρ N=10 μ g/mL of the ammonia nitrogen standard working solution, process for preparation are as follows:
It is soluble in water to weigh 3.8190g ammonium chloride, moves into l000mL volumetric flask, is diluted to graticule, can be saved at 2-5 DEG C
1 month, obtain ammonia nitrogen standard stock solution, ρ N=1000 μ g/mL;5.00mL ammonia nitrogen standard stock solution is drawn to hold in 500mL
In measuring bottle, being diluted to scale can be obtained ammonia nitrogen standard working solution.Prepared before use.
The blank correction is directed to add water to graticule in 50mL colorimetric cylinder, and 1.0mL potassium sodium tartrate solution is then added
With 1.0mL nessler reagent and shake up, stand after 10min at wavelength 420nm, reference measurement absorbance made with water, deducts the suction
Luminosity data.
Step 3: the measurement of sample
3a, the Liquor-making industry wastewater sample for taking step 1 to acquire are added in 50mL tool plug graded tube, add water to graticule constant volume,
It should be shaken up when sampling, all have representative sample to obtain dissolution part and floating parts;It fills in graded tube and adds then to tool
Enter 1.0mL potassium sodium tartrate solution and shake up, add nessler reagent 1.0mL and shake up, in wavelength 420nm after standing 10min
Under, reference measurement absorbance (20mm cuvette) is made with water;
3b, blank sample is prepared according to the step of 3a, i.e., with the tartaric acid in 2mL coloration-determining amount liquid alternative steps 3a
Potassium sodium solution and nessler reagent, stand 10min after at wavelength 420nm, reference measurement absorbance (20mm colorimetric is made with water
Ware);
3c, it the absorbance data obtained in 3a subtracted into the absorbance data obtained in 3b can be obtained Liquor-making industry waste water
The absorbance data of sample, then pass through the calibration curve that step 2 is drawn and can be obtained the ammonia-nitrogen content of Liquor-making industry wastewater sample,
Then the ammonia nitrogen concentration for obtaining Liquor-making industry wastewater sample is calculated by following formula.
Ammonia nitrogen concentration C=m/v
In formula:
C --- the concentration of ammonia nitrogen, mg/L in water sample;
M --- the content of ammonia nitrogen in water sample, μ g;
V --- volume of water sample, mL.
In step 3a, the Liquor-making industry wastewater sample for taking step 1 to acquire is added in 50mL tool plug graded tube, adds water to graticule
It is 0.1-2mg/L that ammonia nitrogen concentration should be controlled after constant volume.If ammonia nitrogen concentration is higher (>=2mg/L) in sample, volume can be with when sampling
It reduces.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
Influence the present invention overcomes sample colorimetry-turbidity to testing result can not influence to test accuracy
Under the premise of, improve working efficiency.
Detailed description of the invention
Fig. 1 is calibration curve linear relationship chart.
Specific embodiment
1 reagent and material
1.1 potassium sodium tartrate solutions, ρ=500g/L.
Weigh 50.0g sodium potassium tartrate tetrahydrate (KNaC4H6O6·4H2O it) is dissolved in 100mL water, heating is boiled to drive away ammonia, is filled
100mL is diluted to after dividing cooling.
1.2 nessler reagent solution
16.0g sodium hydroxide (NaOH) is weighed, is dissolved in 50mL water, is cooled to room temperature.Weigh 7.0g potassium iodide (KI) and
10.0g mercuric iodixde (HgI2), it is soluble in water, then under stiring by this solution, it is molten to be slowly added into above-mentioned 50mL sodium hydroxide
In liquid, it is diluted with water to 100mL.It stores in polyethylene bottle, is covered tightly with rubber stopper or polyethylene lid, stored in dark place, effectively
Phase 1 year.
1.3 colorations-determining amount liquid
Mix a volume sodium hydroxide solution (160g/L) and a volume potassium sodium tartrate solution (1.1).
1.4 Ammonia nitrogen standard liquid
1.4.1 ammonia nitrogen standard stock solution, ρ N=1000 μ g/mL.
Weigh 3.8190g ammonium chloride (NH4Cl, excellent pure grade, in 100-105 DEG C of dry 2h), it is soluble in water, move into l000mL
In volumetric flask, it is diluted to graticule, can be saved 1 month at 2-5 DEG C.
1.4.2 ammonia nitrogen standard working solution, ρ N=10 μ g/mL.
5.00mL ammonia nitrogen standard stock solution is drawn in 500mL volumetric flask, is diluted to scale.Prepared before use.
2 key instruments and equipment
2.1 50mL tool plug (ground) graded tube.
2.2 spectrophotometer.
3 samples
3.1 sample collection and keeping
Water sampling will be analyzed as early as possible in polyethylene bottle or vial.If you need to save, sulfuric acid should be added to be acidified to water sample
It can be reserved for 7 days at pH < 2,2-5 DEG C.
The preparation of 3.2 samples
Take 50mL sample in tool plug graded tube.It should carefully shake up when taking, have to obtain dissolution part and floating parts
Representational sample.If ammonia nitrogen concentration is higher in sample, volume of sample can be reduced.
4 determination steps
4.1 calibration curve
In 8 50mL colorimetric cylinders, be separately added into 0.00m L, 0.50mL, 1.00mL, 2.00 0mL, 4.00mL,
6.00mL, 8.00mL and 10.00mL ammonia nitrogen standard working solution, corresponding to ammonia-nitrogen content be respectively 0.0 μ g, 5.0 μ g,
10.0 μ g, 20.0 μ g, 40.0 μ g, 60.0 μ g, 80.0 μ g and 100 μ g, add water to graticule.It is molten that 1.0mL sodium potassium tartrate tetrahydrate is added
Liquid shakes up, and adds nessler reagent 1.0mL, shakes up.After placing 10min, at wavelength 420nm, with 20mm cuvette, with water
Make reference, measures absorbance.Using the absorbance after blank correction as ordinate, with its corresponding ammonia-nitrogen content (μ g) for horizontal seat
Mark draws calibration curve.
The measurement of 4.2 samples
4.2.1 50mL (if ammonia nitrogen concentration is more than 2mg/L in water sample, can suitably lack water sampling volume) is directly taken, is pressed and school
The identical step of directrix curve measures absorbance.
4.2.2 it prepares a blank sample and 2mL coloration-determining amount liquid is then added into sample, but tartaric acid is not added
Potassium sodium and nessler reagent solution.Then the absorbance of blank sample is deducted from the absorbance of sample.
4.3 blank test
Water sample is replaced with water, is measured by the step identical as sample.
4.4 calculating
Ammonia nitrogen concentration C=m/v
In formula:
C --- the concentration of ammonia nitrogen, mg/L in water sample;
M --- the content of ammonia nitrogen in water sample, μ g;
V --- volume of water sample, mL.
The regression equation of curve matching: y=a+bx
In formula:
The absorbance of y --- solution;
The ammonia nitrogen quality that x --- curve checks in, with above-mentioned m;
A --- regression equation intercept;
B --- regression equation slope;
5 applications
5.1 draw calibration curve
1 calibration curve drawing data table of table
The data for drawing calibration curve are shown in Table 2, Fig. 1, acquire unary linear regression equation: y=a+bx, calibration curve parameter
A=0.0030, b=0.0067, R2=0.9992, show linear preferable.
The verifying of 5.2 method veracity and precisions
5.2.1 the preparation of sample
The ammonia nitrogen standard that 5.00mL10mg/L is separately added into 4 50mL color-comparison tubes uses solution, 5.00mL500
The magnesium ion standard solution of the color standard stock solution of degree, 2mL1000mg/L, is settled to 50mL graticule, the i.e. concentration of ammonia nitrogen
It is 50 degree for 1mg/L, coloration, magnesium ion concentration 40mg/L.
5.2.2 sample treatment and result calculate
2 standard sample of table tests process and result
By 2 experimental result of table it is found that have the sample of coloration and turbidity by colorimetry-turbidity penalty method can eliminate coloration and
Influence of the turbidity to measurement result, accuracy, precision are higher.
5.3 specific embodiment
5.3.1 sample ID: Liquor-making industry waste water residual water, secondary settling tank water sample
5.3.2 determination step
It takes the sample of appropriate volume in 50mL color-comparison tube, being settled to scale, it is molten that 1.0mL sodium potassium tartrate tetrahydrate is added
Liquid shakes up, and adds nessler reagent 1.0mL, shakes up.After placing 10min, at wavelength 420nm, with 20mm cuvette, with water
Make reference, measures absorbance.
5.3.2 experimentation and result
3 residual water of table and secondary settling tank water sample test process and result
By 3 experimental result of table it is found that choosing representational sample residual water and secondary settling tank water sample, residual water is white wine
Industrial original waste water, ammonia nitrogen concentration is higher, but coloration, turbidity are clearly, is the thick semisolid liquid of yellow, needs
It is diluted step by step, the sample coloration after dilution, turbidity have certain reduction, by table 3 it is found that the suction of colorimetry-turbidity compensation
Luminosity mean value is only 0.006, influences less on result, but still has certain influence;Secondary settling tank water sample is the useless of aerobic phase process
Water, which substantially reduces, but equally has higher coloration and turbidity, can by table 3 after twice of dilution
Know, the absorbance mean value of colorimetry-turbidity compensation is 0.038, opposite true value higher about 10%, turbid it is therefore necessary to remove coloration-
Spend the influence to sample result.As shown in Table 3, as a result relative deviation is smaller, and precision is preferable, with a high credibility.
4 flocculent precipitation of table is compared with colorimetry-turbidity penalty method result
By table 4 it is found that industry standard methods take flocculent precipitation pre-treatment and the inventive method colorimetry-turbidity to compensate
Methods and results compare it is found that relative deviation is in claimed range, meet the requirements, and illustrate accurate higher.
5.3.3 the comparison sheet of used time is tested
The comparison of 5 total phosphorus determination working times
By table 5 it is found that the inventive method used time is shorter, under the premise of guaranteeing accuracy and precision, imitate work
Rate improves 6 times.
Claims (5)
1. a kind of colorimetry-turbidity of Liquor-making industry ammonia nitrogen in waste water compensates measuring method, it is characterised in that include the following steps:
Step 1: the acquisition of sample
The acquisition of Liquor-making industry waste water is placed in polyethylene bottle or vial, and sample presentation is analyzed immediately;If Liquor-making industry waste water
It needs to save after acquisition, sulfuric acid should be added to make to be acidified to pH < 2 into Liquor-making industry waste water, can be reserved for 7 days at 2-5 DEG C;
Step 2: the drafting of calibration curve
The ammonia nitrogen standard of 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL are taken respectively
Working solution simultaneously be added 8 50mL colorimetric cylinders in, corresponding to ammonia-nitrogen content be respectively 0.0 μ g, 5.0 μ g, 10.0 μ g, 20.0
μ g, 40.0 μ g, 60.0 μ g, 80.0 μ g and 100 μ g, add water to graticule;Then to being separately added into 1.0mL potassium tartrate in colorimetric cylinder
Sodium solution simultaneously shakes up, then is separately added into nessler reagent 1.0mL and shakes up, and after standing 10min at wavelength 420nm, is joined with water work
Than measuring absorbance, using the absorbance after blank correction as ordinate, using its corresponding ammonia-nitrogen content as abscissa, calibration is drawn
Curve;
Step 3: the measurement of sample
3a, the Liquor-making industry wastewater sample for taking step 1 to acquire are added in 50mL tool plug graded tube, add water to graticule constant volume, sample
When should shake up, with obtain dissolution part and floating parts all have representative sample;It fills in graded tube and is added then to tool
1.0mL potassium sodium tartrate solution simultaneously shakes up, and adds nessler reagent 1.0mL and shakes up, after standing 10min at wavelength 420nm,
Make reference measurement absorbance with water;
3b, blank sample is prepared according to the step of 3a, i.e., with the sodium potassium tartrate tetrahydrate in 2mL coloration-determining amount liquid alternative steps 3a
Solution and nessler reagent, stand 10min after at wavelength 420nm, reference measurement absorbance is made with water;
3c, it the absorbance data obtained in 3a subtracted into the absorbance data obtained in 3b can be obtained Liquor-making industry wastewater sample
Absorbance data, then the calibration curve drawn by step 2 can be obtained the ammonia-nitrogen content of Liquor-making industry wastewater sample, then
The ammonia nitrogen concentration for obtaining Liquor-making industry wastewater sample is calculated by following formula:
Ammonia nitrogen concentration C=m/v
In formula:
C --- the concentration of ammonia nitrogen, mg/L in water sample;
M --- the content of ammonia nitrogen in water sample, μ g;
V --- volume of water sample, mL.
2. measuring method according to claim 1, it is characterised in that:
In step 2, density p=500g/L of the potassium sodium tartrate solution, process for preparation is as follows: weighing 50.0g potassium tartrate
Sodium is dissolved in 100mL water, and heating is boiled to drive away ammonia, is diluted to 100mL after being fully cooled.
3. measuring method according to claim 1, it is characterised in that:
In step 2, the ρ N=10 μ g/mL of the ammonia nitrogen standard working solution, process for preparation is as follows:
It is soluble in water to weigh 3.8190g ammonium chloride, moves into l000mL volumetric flask, is diluted to graticule, 1 can be saved at 2-5 DEG C
Month, obtain ammonia nitrogen standard stock solution, ρ N=1000 μ g/mL;5.00mL ammonia nitrogen standard stock solution is drawn in 500mL volumetric flask
In, being diluted to scale can be obtained ammonia nitrogen standard working solution.
4. measuring method according to claim 1, it is characterised in that:
In step 2, the blank correction is directed to add water to graticule in 50mL colorimetric cylinder, and 1.0mL sodium potassium tartrate tetrahydrate is then added
Solution and 1.0mL nessler reagent simultaneously shake up, and after standing 10min at wavelength 420nm, make reference measurement absorbance with water, deduct
The absorbance data.
5. measuring method according to claim 1, it is characterised in that:
In step 3a, the Liquor-making industry wastewater sample for taking step 1 to acquire is added in 50mL tool plug graded tube, adds water to graticule constant volume
After should control ammonia nitrogen concentration be 0.1-2mg/L.
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CN112098348A (en) * | 2020-08-20 | 2020-12-18 | 厦门斯坦道科学仪器股份有限公司 | Total phosphorus turbidity compensation method applied to high-turbidity water body online monitoring |
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CN113607725A (en) * | 2021-07-30 | 2021-11-05 | 云南铜业股份有限公司西南铜业分公司 | Method for determining ammonia nitrogen content in wastewater |
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CN115436354A (en) * | 2022-08-31 | 2022-12-06 | 上海博取仪器有限公司 | Anti-interference water quality analyzer testing method |
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CN112098348A (en) * | 2020-08-20 | 2020-12-18 | 厦门斯坦道科学仪器股份有限公司 | Total phosphorus turbidity compensation method applied to high-turbidity water body online monitoring |
CN112098348B (en) * | 2020-08-20 | 2023-12-26 | 厦门斯坦道科学仪器股份有限公司 | Total phosphorus turbidity compensation method applied to high turbidity water on-line monitoring |
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 |
CN113607725A (en) * | 2021-07-30 | 2021-11-05 | 云南铜业股份有限公司西南铜业分公司 | Method for determining ammonia nitrogen content in wastewater |
CN113884450A (en) * | 2021-09-15 | 2022-01-04 | 五邑大学 | Turbidity chromaticity correction method for automatic water quality monitor |
CN115436354A (en) * | 2022-08-31 | 2022-12-06 | 上海博取仪器有限公司 | Anti-interference water quality analyzer testing method |
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