CN108344703A - The method of amino benzenes compounds in spectrophotometry water quality - Google Patents
The method of amino benzenes compounds in spectrophotometry water quality Download PDFInfo
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- CN108344703A CN108344703A CN201810102511.2A CN201810102511A CN108344703A CN 108344703 A CN108344703 A CN 108344703A CN 201810102511 A CN201810102511 A CN 201810102511A CN 108344703 A CN108344703 A CN 108344703A
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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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract
The invention belongs to analyze detection field, and in particular to a kind of method of amino benzenes compounds in spectrophotometry water quality.The method of the present invention, including following steps：(1) preparation of aniline standard curve；(2) amino benzenes compounds concentration in sample to be tested is measured；Advantageous effect of the present invention is, the method being previously mentioned in respect to the background art i.e. N (1 naphthalene) ethylenediamine azo spectrophotometry, the color developing agent that the method for the present invention uses greatly reduces the harm caused by operating personnel and environment in experimentation, pass through condition optimizing simultaneously, make this method that there is good reliability, high sensitivity and detection limit are low.
Description
Technical field
The invention belongs to analyze detection field, and in particular to amino benzenes compounds in a kind of spectrophotometry water quality
Method.
Background technology
Amino benzenes compounds in addition to being widely used in the industrial productions such as chemical industry, printing and dyeing and pharmacy or synthetic drug, dye
One of the important source material of material, insecticide, high molecular material, explosive etc..Aniline and its derivatives can by sucking, eating or thoroughly
It crosses skin to absorb and cause to be poisoned, blood circulation system damage, liver cell toxic lesion, nervous system damage can be caused, separately
Outer amino benzenes compounds also have carcinogenic and mutagenic effect.China's integrated wastewater discharge standard requires, benzene in industrial wastewater
Aminated compounds highest allows a concentration of 5mg/L of discharge quality.
Currently, the standard method for measuring amino benzenes compounds both at home and abroad is still N- (1- naphthalenes) ethylenediamine azo point of early stage
Light photometry (GB 11889-1989), principle be, amino benzenes compounds (pH1.5-2.0) and nitrous acid in acid condition
Salt diazotising, then be coupled with N- (1- naphthalenes) ethylenediamine-hydrochloride, aubergine dyestuff is generated, spectrophotometry measurement is carried out, is surveyed
Amount wavelength is 545nm, and the method is easy to operate, high sensitivity, but hydrochloride naphthodiamide is a kind of strong carcinogen, and toxicity is big,
It can cause damages to operating personnel and environment.
It is, thus, sought for a kind of new method measuring amino benzenes compounds spectrophotometric, can mitigate due to using salt
The harm to human body caused by sour naphthodiamide, and sensitivity, accuracy in detection process can not be reduced.
Invention content
Technical problem to be solved by the present invention lies in establishing to measure amino benzenes compounds spectrophotometric new system, select
A kind of new color developing agent H acid substitutes highly toxic hydrochloride naphthodiamide in old system, reduces experimental implementation to personnel and ring
Harm caused by border, while optimization method condition make it have good reliability, highly sensitive, low detection limits.
The present invention, which uses its design of the concentration of amino benzenes compounds in water by Spectrophotometry matter, to be added into sample
Hydrochloric acid conditioning solution pH 1-2, are then added sodium nitrite, shake up, and stand 3 minutes；It is excessive to add Amcide Ammate elimination
Sodium nitrite is added sodium carbonate liquor and adjusts pH value of solution 7-9, is eventually adding the colour developing of H acid after ten minutes, is existed with 10mm cuvettes
520nm colorimetrics.
The detection method of the present invention, is as follows：
(1) drafting of aniline standard curve：
A. 7 50mL color-comparison tubes are taken, 0.00,1.00,2.00,3.00,4.00,5.00,6.00mL benzene are separately added into
Amine standard solution is settled to 25mL, is added 1:9 hydrochloric acid 1.0mL adjust 7 above-mentioned samples to pH1-2, are separately added into the Asias 5g/L
Sodium nitrate solution 3.0mL, mixing stand 3 minutes；
B. it is separately added into 5g/L Amcide Ammate 1.5mL in each solution obtained in a, is placed 3 minutes after fully shaking,
Wait for that bubble eliminates, it is spare；
C. 5g/L sodium carbonate about 3mL are added, adjusts pH value of solution spare in b to 7-9, is settled to 50mL, add 1%H sour
1.0mL, mixing are placed 10 minutes；
D. the solution obtained in c is taken to be placed in 10mm cuvettes, at 520nm wavelength, using water as reference measurement absorbance；
E. the absorbance A of water reference is subtracted with the absorbance A of measurement0For ordinate y, in the series standard solution of preparation
The content of aniline is abscissa x, draws curve, and the calibration curve equation of gained is：Y=0.0051x-0.0014, r=
0.9998；
(2) in sample to be tested amino benzenes compounds concentration measurement
F. water sample is adjusted to neutrality, as sample to be tested；
G. the aniline standard solution described in sample to be tested alternative steps a is taken, and is waited for according to step b, c, d, e operation
Solution absorbance is surveyed, the standard curve of absorbance and above-mentioned drafting is compared, amino benzenes compounds in water sample to be measured are calculated
Concentration, the calculation formula of amino benzenes compounds is in sample：ρ (mg/L)=(A-A0+ 0.0014)/0.0051/50, according to upper
The formula stated obtains the concentration of amino benzenes compounds.
Concentration mensuration ranging from concentration limit is 0.04mg/L, a concentration of 2.50mg/L of determination of the upper limit
1:9 hydrochloric acid are volume ratio.
If water sample to be measured is muddy, Medium speed filter paper filtering flushed Ke Jingshui is measured again after discarding primary filtrate 20mL.
In step f, pH value is adjusted using hydrochloric acid or sodium carbonate liquor.
Advantageous effect of the present invention is, with respect to the background art in the method i.e. GB 11889-1989 water quality benzene that is previously mentioned
Measurement N- (1- naphthalenes) ethylenediamine azo spectrophotometry of aminated compounds, the color developing agent that method of the invention uses drop significantly
The harm caused by operating personnel and environment in low experimentation, while passing through condition optimizing, so that this method is had good
Reliability, high sensitivity and detection limit are low.
Description of the drawings
Fig. 1 is the Specification Curve of Increasing figure of the present invention；
Fig. 2 is influence of the medium wavelength of the present invention to chromogenic reaction absorbance；
Fig. 3 is influence of the hydrochloric acid addition to chromogenic reaction absorbance in the present invention；
Fig. 4 is influence of the Sodium Nitrite addition of the present invention to chromogenic reaction absorbance；
Fig. 5 is influence of the Amcide Ammate addition to chromogenic reaction absorbance in the present invention；
Fig. 6 is influence of the sodium carbonate addition to chromogenic reaction absorbance in the present invention；
Fig. 7 is influence of the H acid addition to chromogenic reaction absorbance in the present invention.
Specific implementation mode
The present invention is further described with reference to the accompanying drawings and detailed description, so as to the technology of this field
Personnel know more about the present invention, but do not limit the present invention with this.
Embodiment 1
The test of sample
Experiment agents useful for same is top pure grade, and test water is two level water.
Sodium nitrite, 5g/L：0.5g sodium nitrites are weighed, is dissolved in a small amount of water, is diluted to 100mL, be stored in brown bottle
In.
Amcide Ammate, 5g/L：0.5g Amcide Ammates are weighed, is dissolved in a small amount of water, is diluted to 100mL, be stored in palm fibre
In color bottle.
Sodium carbonate, 0.5mol/L：4.15g sodium carbonate is weighed, is dissolved in a small amount of water, is diluted to 100mL, be stored in reagent bottle
In.
H acid, 1%：1g H acid is weighed, is dissolved in a small amount of water, is diluted to 100mL, be stored in brown bottle, it is now with the current.
Sulfuric acid standard solution：0.05mol/L.
Aniline standard reserving solution：0.05mol/L sulfuric acid solution 10mL are added in 25ml volumetric flasks, (standard is extremely for weighing
0.0001g), 5 drop aniline reagents are added, then weigh, is diluted to graticule with 0.05mol/L sulfuric acid solutions, shakes up, calculate every milli
Rise the amount of aniline contained in solution.
Aniline standard solution：Standard reserving solution is diluted to a concentration of 1.00mL solution 20.0 μ g's containing aniline with pure water
Standard solution.
The preparation of standard curve：
7 50mL color-comparison tubes are taken, 0.00,1.00,2.00,3.00,4.00,5.00,6.00mL aniline are separately added into
Standard is settled to 25mL using solution with two level water, adds (1:9) hydrochloric acid 1.0mL；Add 5g/L sodium nitrite solution 3.0mL, mixing,
Stand 3 minutes；5g/L Amcide Ammate 1.5mL are added, is placed 3 minutes after fully shaking, waits for that bubble eliminates；0.5mol/L is added
Sodium carbonate, 3.0mL are settled to 50mL, add 1%H acid 1.0mL mixings, place 10 minutes, with 10mm colorimetrics at 520nm wavelength
Ware, using water as reference measurement absorbance；The absorbance A of water reference is subtracted with the absorbance A of measurement0For ordinate, with preparation
The content of aniline is abscissa in series standard solution, draws curve；Obtained calibration curve equation：Y=0.0051x-
0.0014 (r=0.9998), as shown in Fig. 1.
Measure the concentration of amino benzenes compounds in water sample to be measured：
If water sample is muddy to be filtered through the flushed Medium speed filter paper of water, after discarding primary filtrate 20mL, with hydrochloric acid or sodium carbonate
Solution is adjusted to neutrality, as sample to be tested；It takes in suitable sample to be tested to 50mL colorimetric cylinders, sample is measured according to above-mentioned steps
Product absorbance A, the calculation formula of aniline is in sample：ρ (mg/L)=(A-A0+0.0014)/0.0051/50；
Veracity and precision determination experiment
7 surveys are carried out using the method in embodiment 1 respectively to the aniline solution of a concentration of 0.500mg/L and 1.50mg/L
Fixed, it is respectively 0.503mg/L and 1.50mg/L that 7 times, which measure average value, and relative error is respectively 0.6% and 0.0%, opposite mark
Quasi- deviation (RSD) is respectively 1.1% and 1.3%, and this method accuracy, precision are good.
| Measurement result | 1 | 2 | 3 | 4 | 5 | 6 | 7 | Average value | Relative standard deviation % (RSD) |
| 0.500mg/L | 0.500 | 0.502 | 0.508 | 0.492 | 0.506 | 0.507 | 0.504 | 0.503 | 1.1 |
| 1.50mg/L | 1.51 | 1.48 | 1.52 | 1.48 | 1.47 | 1.51 | 1.51 | 1.50 | 1.3 |
Embodiment 2
Influence of the wavelength to chromogenic reaction absorbance
According to the method for embodiment 1, influence of the test different wave length to light absorption value is as shown in Fig. 2 in wavelength
There is maximum absorbance under 520nm.
Embodiment 3
Difference (1:9) influence of the hydrochloric acid addition to reaction absorbance
According to the method for embodiment 1, difference (1 is tested:9) hydrochloric acid addition must influence reaction light absorption value, such as attached drawing 3
It is shown, (1:9) hydrochloric acid addition is 0.1-4.0mL, i.e. when pH is 1-2, absorbance is maximum, method choice (1:9) hydrochloric acid adds
It is 1.0mL to enter amount.
Embodiment 4
Influence of the different sodium nitrite additions to reaction light absorption value
According to the method for example 1, influence of the different sodium nitrite additions to reaction light absorption value is tested, such as 4 institute of attached drawing
Show, when sodium nitrite addition is 3mL, light absorption value reaches maximum.
Embodiment 5
Influence of the different Amcide Ammate additions to reaction light absorption value
According to the method for example 1, influence of the different Amcide Ammate additions to reaction light absorption value is tested, such as attached drawing 5
It is shown,
Be added 1.0mL Amcide Ammates, can both eliminate excessive sodium nitrite well, it is contemplated that if aniline amount compared with
It is low, excessively more sodium nitrites, method choice 1.5mL Amcide Ammates may be added.
Embodiment 6
Influence of the different sodium carbonate additions to reaction light absorption value
According to the method for example 1, influence of the different sodium carbonate additions to light absorption value is tested, as shown in Fig. 6,
When sodium carbonate addition is 2.0-3.0mL, i.e., when pH value is between 7-9, light absorption value reaches maximum, method choice
3mL sodium carbonate is added.
Embodiment 7
Different H acid additions must influence reaction light absorption value
According to the method for example 1, influence of the different H acid additions to light absorption value is tested, as shown in Fig. 7,
When H acid additions are 1.0mL, absorbance is larger, is had slightly although continuing growing H acid addition light absorption values
It increases, but also improves blank absorbency simultaneously, therefore the H acid additions of method choice 1.0mL.
Embodiment 8
The measurement of the apparent mole coefficient of some amino benzenes compounds and the comparison with national standard method measurement result.
Respectively according to the assay method and national standard method of amino benzenes compounds provided by the invention, respectively to some phenyl amines
The apparent mole coefficient of compound is determined, and is as a result listed in table 1.By table 1 as it can be seen that this method measures amino benzenes compounds
Apparent mole coefficient it is higher compared with National Standard Method.
The apparent mole coefficient that 1 amino benzenes compounds of table measure
Embodiment 9
Environment water sample analysis
Analysis is sampled to surface water river, measures amino benzenes compounds concentration in water body, and carries out mark-on reclaims reality
It tests, while check experiment is carried out with National Standard Method, be as a result listed in table 2.By measurement result as it can be seen that this method measures phenyl amines in water quality
Compound results are closer to National Standard Method, and the relative deviation of measurement result is low, recovery of standard addition is high, illustrate this method essence
Density and accuracy are all preferable.
2 environmental water sample measurement result of table
It is opposite to mark by above experiment sum number it was demonstrated that the high sensitivity of its detection of the method for the present invention, precision is good
Quasi- deviation is small, and recovery of standard addition is high, with respect to the background art disclosed in the light splitting of method, that is, N- (1- naphthalenes) ethylenediamine azo
Photometry, method security of the invention is high, will not cause damages to operating personnel and environment.
Claims (6)
1. the method for spectrophotometry amino benzenes compounds, including following steps：
(1) drafting of aniline standard curve：
A. 7 50mL color-comparison tubes are taken, 0.00,1.00,2.00,3.00,4.00,5.00,6.00mL aniline marks are separately added into
Quasi- solution is settled to 25mL, and hydrochloric acid 1mL is added, adjusts 7 above-mentioned samples to pH1-2, it is molten to be separately added into 5g/L sodium nitrites
Liquid 3.0mL, mixing stand 3 minutes；
B. it is separately added into 5g/L Amcide Ammate 1.5mL in each solution obtained in a, is placed 3 minutes after fully shaking, waits for gas
Bubble eliminates, spare；
C. pH value of solution spare in b is adjusted to 7-9, is settled to 50mL, and 1%H acid 1.0mL, mixing is added to place 10 minutes；
D. the solution obtained in c is taken to be placed in 10mm cuvettes, at 520nm wavelength, using water as reference measurement absorbance；
E. the absorbance of water reference is subtracted as ordinate using the absorbance of measurement, is contained with aniline in the series standard solution of preparation
Amount is abscissa, draws curve, and the calibration curve equation of gained is：Y=0.0051x-0.0014, r=0.9998；
(2) in sample to be tested amino benzenes compounds concentration measurement
F. water sample is adjusted to neutrality, as sample to be tested；
G. the aniline standard solution described in sample to be tested alternative steps a is taken, and to be measured molten according to step b, c, d, e operation acquisition
The standard curve of absorbance and above-mentioned drafting is compared liquid absorbance, calculates the dense of amino benzenes compounds in water sample to be measured
It spends, the calculation formula of amino benzenes compounds is in sample：ρ (mg/L)=(A-A0+ 0.0014)/0.0051/50, according to above-mentioned
Formula obtains the concentration of amino benzenes compounds.
2. the method for spectrophotometry amino benzenes compounds as described in claim 1, which is characterized in that in sample to be tested
Amino benzenes compounds concentration limit is 0.04mg/L, a concentration of 2.50mg/L of determination of the upper limit.
3. the method for spectrophotometry amino benzenes compounds as described in claim 1, which is characterized in that in a, aniline mark
Quasi- solution concentration is 20.0mg/L.
4. the method for spectrophotometry amino benzenes compounds as described in claim 1, which is characterized in that in a, hydrochloric acid is molten
The volumetric concentration of liquid is 10%.
5. the method for spectrophotometry amino benzenes compounds as described in claim 1, which is characterized in that adjust pH in c
Using 5g/L sodium carbonate liquors.
6. the method for spectrophotometry amino benzenes compounds as described in claim 1, which is characterized in that in f, using salt
Acid solution or sodium carbonate liquor adjust pH value.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111912802A (en) * | 2020-08-25 | 2020-11-10 | 潍坊市生态环境局寿光分局 | Method for detecting nitrite nitrogen by spectrophotometry |
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2018
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| CN101655461A (en) * | 2009-10-20 | 2010-02-24 | 北京城市排水集团有限责任公司 | Method for determining ion content of cationic polyacrylamide by utilizing spectrophotometry |
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| CN111912802A (en) * | 2020-08-25 | 2020-11-10 | 潍坊市生态环境局寿光分局 | Method for detecting nitrite nitrogen by spectrophotometry |
| CN111912802B (en) * | 2020-08-25 | 2023-05-26 | 潍坊市生态环境局寿光分局 | Method for detecting nitrite nitrogen by spectrophotometry |
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