CN102928369A - Method for measuring nitrite - Google Patents
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- CN102928369A CN102928369A CN2012104226224A CN201210422622A CN102928369A CN 102928369 A CN102928369 A CN 102928369A CN 2012104226224 A CN2012104226224 A CN 2012104226224A CN 201210422622 A CN201210422622 A CN 201210422622A CN 102928369 A CN102928369 A CN 102928369A
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Abstract
The invention discloses a method for measuring nitrite. The method comprises the following steps of: taking supernatant liquor with the volume being V1 of a water sample after standing for 30 minutes, shifting the supernatant liquor to a colorimetric tube, then sequentially adding a potassium bromide water solution, a 2-amino-5-naphthol-7sulfoacid water solution and a hydrochloric acid water solution to the colorimetric tube, standing the mixture for 1-5minutes after uniformly shaking to record as a second solution; taking a volumetric flask to record as a first volumetric flask, and adding a certain amount of water solution of sodium carbonate to the first volumetric flask; then shifting the second solution to the first volumetric flask, washing the colorimetric tube by a small amount of deionized water, shifting the cleansing solution to the first volumetric flask, uniformly shaking, metering the volume by the deionized water to obtain a third solution, and standing the third solution for 5-30minutes to obtain a fourth solution; measuring the absorbancy of the fourth solution by taking reagent blank as a reference solution; and calculating to obtain the content of the nitrite in the water sample according to a regression equation of a standard work curve and the absorbancy.
Description
Technical field
The present invention relates to food security and field of environment protection, be specifically related to a kind of assay method of nitrite.
Background technology
Nitrite enters the people and knows from experience generation high price haemoglobin in blood, causes histanoxia, causes acute poisoning.Also can in the intestines and stomach sour environment, be converted into Carcinogenic Nitrosamines.WHO classifies the nitrous acid in food, the environment water as strict control object.At present, the assay method of the most frequently used nitrite is spectrophotometric method (State Standard of the People's Republic of China: the mensuration of the GB/T 5750.5-2006 drinking water standard method of inspection-nitrite-diazo coupling spectrophotometric method; Mensuration-the spectrophotometric method of GB/T 5009.33 food security national standard-nitrite) the used diazo reagent of these methods is sulfanilamide (SN) and sulfanilic acid, coupling reagent is hydrochloride naphthodiamide, it has strong carcinogenicity, can work the mischief and easily forms secondary pollution environment, operating personnel.
2-amino-5-naphthols-7-sulfonic acid is commonly called as J acid, is a kind of important dyestuff intermediate, can be used for making azo dyes, also can be used as diazo reagent.Because 2-amino-5-naphthols-7-sulfonic acid is low toxicity reagent, therefore, it is widely used in manufacturing industry as a kind of important intermediate.
Summary of the invention
In view of this, the purpose of this invention is to provide a kind of method of measuring nitrite, select hypotoxic 2-amino-5-naphthols-7-sulfonic acid to replace the strong carcinogenicity diazo reagent and the coupling reagent that use in the classic method as diazonium from coupling reagent among the present invention, carcinogenic by force to solve in the existing assay method reagent, to environment, operating personnel work the mischief and easily form the problem of secondary pollution, and do not need to add respectively diazo reagent and coupling reagent in the course of reaction and only need add 2-amino-5-naphthols-this diazonium of 7-sulfonic acid from coupling reagent, then can realize the purpose of diazo reaction and coupling reaction.
Therefore, the present invention has adopted following technical scheme:
A kind of method of measuring nitrite may further comprise the steps:
Step 1, water sampling left standstill 30 minutes, then got the supernatant liquor that volume is this water sample of V1;
Step 3 is got a volumetric flask, is designated as the first volumetric flask, to the aqueous solution that wherein adds a certain amount of sodium carbonate as the PH correctives;
Step 4, the second solution is transferred to from the first color comparison tube in the first volumetric flask of the aqueous solution that fills sodium carbonate, and with a small amount of deionized water rinsing of the first color comparison tube, washing lotion changes in the first volumetric flask of the aqueous solution that fills sodium carbonate equally, then shakes up, use the deionized water constant volume, obtain the 3rd solution, its pH value is between 8.2～10.2 scopes, again with the 3rd solution left standstill number minute, time of repose is designated as B, obtains the 4th solution;
Step 5 as reference solution, is measured the absorbance of the 4th solution with reagent blank at wavelength 500nm place;
Wherein, when the concentration of potassium bromide in described the first solution is 0.8mg/mL the diazo reaction time the fastest,
A is 1～5min, and B is 5～30min,
In the above-mentioned steps 2, in the 2-of adding amino-5-naphthols-7-sulfonic acid aqueous solution-amino-5-naphthols-concentration of 7-sulfonic acid in the first solution is 5.00 * 10
-5～4.00 * 10
-4Mol/L scope internal absorbance is stable,
Above-mentioned each step reaction is all at room temperature carried out,
Diazo salt and excessive 2-amino-5-naphthols-7-sulfonic acid coupling generates red azo compounds in aqueous sodium carbonate, and the absorption peak of this compound is at the 500nm place, and therefore, the absorbance of described solution is measured at wavelength 500nm place.
Further, the method for mensuration nitrite provided by the invention, its feature can also for: concentration of hydrochloric acid when 0.30～0.60mol/L, absorbance is stable and maximum.
Further, the method for mensuration nitrite provided by the invention, its feature can also for: the mentioned reagent blank configures by the following method:
Step 7, getting volume is color comparison tube of the other injection of deionized water of V1, is designated as the second color comparison tube;
Step 8, in the second color comparison tube, add successively the kbr aqueous solution in the step 2,2-amino-5-naphthols-7-sulfonic acid aqueous solution adds the aqueous hydrochloric acid solution in the step 2 at last, obtains the 5th solution, then described the 5th solution is shaken up, leave standstill after shaking up, time of repose is the A in the step 2 again, obtains the 6th solution;
Step 9, other gets a volumetric flask, is designated as the second volumetric flask, to the aqueous solution that wherein adds the sodium carbonate in the step 3;
Step 10, the 6th solution is transferred to from the second color comparison tube in the second volumetric flask of the aqueous solution that fills sodium carbonate, and with a small amount of deionized water rinsing of described the second color comparison tube, washing lotion changes in described the second volumetric flask equally, then uses the deionized water constant volume, shake up again, obtain the 7th solution, then with the 7th solution left standstill, time of repose is the B in the step 4, obtain the 8th solution, be reagent blank.
Further, the method for mensuration nitrite provided by the invention, its feature can also for: the concentration range of contained nitrite must be at 0.02mg/L～0.60mg/L in the water sample of mensuration.
Further, the method for mensuration nitrite provided by the invention, its feature can also for: the assay method of above-mentioned standard working curve is as follows, may further comprise the steps:
Step 11, the sodium nitrite titer of different volumes is moved into respectively in the other N color comparison tube, be designated as the 3rd color comparison tube series, then add respectively deionized water in the 3rd color comparison tube series and be diluted to equal volume, thereby obtain having the 9th solution series of equal volume;
Step 12, add successively the kbr aqueous solution in the step 2 in the 9th solution series, 2-amino-5-naphthols-7-sulfonic acid aqueous solution, add at last the aqueous hydrochloric acid solution in the step 2, then shake up, obtain the tenth solution series, its pH value is between 1.0～2.0, the tenth solution series is left standstill, time of repose is the A in the step 2 again, obtains the 11 solution series;
Step 13, the 11 solution series is changed over to respectively from described the 3rd color comparison tube series in the volumetric flask of aqueous solution that other N fills the sodium carbonate in the step 3, be designated as the 3rd volumetric flask series, and with a small amount of deionized water rinsing of the 3rd color comparison tube series, washing lotion changes in the 3rd volumetric flask series equally, then shake up, and use the deionized water constant volume, its pH value is between 8.2～10.2, obtain the 12 solution series, then shake up, leave standstill again afterwards, time of repose is the B in the step 4, obtains the 13 solution series;
Step 14 as reference solution, is measured the absorbance of the 13 solution series with the reagent blank in the step 5 one by one at wavelength 500nm place;
Step 15 according to the absorbance drawing standard curve of the 13 solution series, is carried out linear fit to typical curve again and is obtained regression equation;
Wherein, N is not less than 5 natural number.
In the method for said determination nitrite, the coexisting ion in the solution can not exert an influence substantially to measurement result.For example, in the sodium nitrite solution of 0.688mg/L, add (unit: mg/L) K
+(200), Na
+(200), Ca
2+(550), Mg
2+(550), Al
3+(0.2), Fe
3+(0.3), Pb
2+(0.1), Cu
+(1.0), Cd
2+(0.01), Ag
+(0.05), Cr
3+(0.1), Hg
2+(0.001), Ni
2+(0.02), Zn
2+(2.0), NO
3 -(10), SO
4 2-(250), H
2PO
4 -(0.4), F
-(1.5), Cl
-(250), CN
-(0.2).Result of study shows: tested test solution absorbance relative error is all less than 5%.
Invention effect and effect
The present invention discloses a kind of method of measuring nitrite, utilize 2-amino-5-naphthols-7-sulfonic acid as diazonium from coupling reagent, by spectrophotometry, measure the content of nitrite.It is little that the method has a reagent toxicity, simple operation, sensitivity is higher, the result is accurate, etc. advantage, be fit to very much promote.
Description of drawings
Fig. 1 adopts method that the present invention measures nitrite in embodiment one water sample to be analyzed and the water sample analysis that obtains figure as a result;
Fig. 2 adopts method that the present invention measures nitrite in embodiment two water sample to be analyzed and the water sample analysis that obtains figure as a result;
Fig. 3 adopts method that the present invention measures nitrite in embodiment three water sample to be analyzed and the water sample analysis that obtains figure as a result.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.It should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.
Embodiment one
Sample pretreatment: water sample is taken from respectively Huangpu River tributary and pond, campus, and water sample leaves standstill 30min, gets supernatant liquor 25mL.
Sample tests: pipette water sample 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 1.5mL, shakes up and make diazo liquid, and its pH value is 1.0, with solution left standstill 1min, generates diazonium salt solution.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 3mL.Diazonium salt solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, the solution pH value is 8.2, leaves standstill 5min, and diazo salt can generate red azo compounds with excessive 2-amino-5-naphthols-7-sulfonic acid coupling under alkaline environment.Then, use the 1cm cuvette, reagent blank is made reference, measures the absorbance of solution at wavelength 500nm place.Calculate the content of nitrite according to standard working curve.Do recovery experiment (n=8) and compare with National Standard Method (GB/T 75750.5-2006) with standard addition method.Fig. 1 is.
The configuration of reagent blank: pipette deionized water 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 1.5mL, shakes up, with solution left standstill 1min.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 3mL.Solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, and leaving standstill 5min, the solution that obtains is reagent blank.
The drafting of standard working curve: pipette 2.5 * 10
-4Mol/L sodium nitrite titer 0mL, 0.2mL, 0.5mL, 1.0mL, 1.2mL and 1.5mL also add respectively 10mL, 9.8mL, 9.5mL, 9mL, 8.8mL and the dilution of 8.5mL deionized water in 6 25mL color comparison tubes.Add successively 1% potassium bromide solution 1.0mL, 1.0 * 10
-2Mol/L J acid solution 1.0mL, 1.5mol/L hydrochloric acid solution 1.5mL shakes up, and makes diazonium salt solution, and its pH value is 1.0, with solution left standstill 1min.Other gets 6 25mL volumetric flasks, adds 1.0mol/L sodium carbonate liquor 3mL.Diazonium salt solution is changed in the sodium carbonate liquor, a small amount of deionized water rinsing of diazonium salt solution color comparison tube, washing lotion changes in the sodium carbonate liquor equally, shakes up to dilute constant volume with deionized water afterwards, leaves standstill 5min.Use the 1cm cuvette, reagent blank is made reference, and in wavelength 500nm place its absorbance of sequentially determining, take absorbance as ordinate, nitrite concentration is horizontal ordinate, the drawing standard curve.
According to Specification Curve of Increasing regression equation: A=0.852c (mg/L)+3.0 * 10
-3(r=0.998,0.02mg/L～0.60mg/L).Apparent molar absorption coefficient ε=3.93 * 10
4Lmol
-1Cm
-1Wherein: A is absorbance; C is nitrite concentration.
Fig. 1 adopts method that the present invention measures nitrite in embodiment one water sample to be analyzed and the water sample analysis that obtains figure as a result.By among Fig. 1 as can be known, 2-amino-5-naphthols-7-sulfonic acid is from coupling spectrophotometry environment water nitrite: relative standard deviation 1.80%, the recovery 98.7%～101.2%.
Embodiment one effect and effect
The present invention discloses a kind of method of measuring nitrite, select hypotoxic 2-amino-5-naphthols-7-sulfonic acid to replace the strong carcinogenicity diazo reagent and the coupling reagent that use in the classic method as diazonium from coupling reagent in the embodiments of the invention one, under the room temperature, diazo-reaction occurs in nitrite and J acid in dilute hydrochloric acid solution, diazo salt and excessive J acid coupling generates red azo compounds compound absorption peak at the 500nm place in aqueous sodium carbonate, calculates the concentration of nitrite by the absorbance of measuring solution.Above experimental result shows, not only simple operation but also sensitivity is higher, the result is accurate of the present invention, and also agents useful for same toxicity is little, can greatly reduce the pollution to operating personnel and environment.
Embodiment two
Sample pretreatment: water sample is taken from respectively Huangpu River tributary and pond, campus, and water sample leaves standstill 30min, gets supernatant liquor 25mL.
Sample tests: pipette water sample 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 1.0mL, shakes up and make diazo liquid, and its pH value is 1.5, with solution left standstill 3min, generates diazonium salt solution.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 5mL.Diazonium salt solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, the solution pH value is 9.0, leaves standstill 18min, and diazo salt can generate red azo compounds with excessive 2-amino-5-naphthols-7-sulfonic acid coupling under alkaline environment.Then, use the 1cm cuvette, reagent blank is made reference, measures the absorbance of solution at wavelength 500nm place.Calculate the content of nitrite according to standard working curve.Do recovery experiment (n=8) and compare with National Standard Method (GB/T 75750.5-2006) with standard addition method.
The configuration of reagent blank: pipette deionized water 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 1.0mL, shakes up, with solution left standstill 3min.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 5mL.Solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, and leaving standstill 18min, the solution that obtains is reagent blank.
The drafting of standard working curve: pipette 2.5 * 10
-4Mol/L sodium nitrite titer 0mL, 0.2mL, 0.5mL, 1.0mL, 1.2mL and 1.5mL also add respectively 10mL, 9.8mL, 9.5mL, 9mL, 8.8mL and the dilution of 8.5mL deionized water in 6 25mL color comparison tubes.Add successively 1% potassium bromide solution 1.0mL, 1.0 * 10
-2Mol/L J acid solution 1.0mL, 1.5mol/L hydrochloric acid solution 1.0mL shakes up, and makes diazonium salt solution, and its pH value is 1.5, with solution left standstill 3min.Other gets 6 25mL volumetric flasks, adds 1.0mol/L sodium carbonate liquor 5mL.Diazonium salt solution is changed in the sodium carbonate liquor, a small amount of deionized water rinsing of diazonium salt solution color comparison tube, washing lotion changes in the sodium carbonate liquor equally, shakes up to dilute constant volume with deionized water afterwards, leaves standstill 18min.Use the 1cm cuvette, reagent blank is made reference, and in wavelength 500nm place its absorbance of sequentially determining, take absorbance as ordinate, nitrite concentration is horizontal ordinate, the drawing standard curve.
According to Specification Curve of Increasing regression equation: A=0.852c (mg/L)+3.0 * 10
-3(r=0.998,0.02mg/L～0.60mg/L).Apparent molar absorption coefficient ε=3.93 * 10
4Lmol
-1Cm
-1Wherein: A is absorbance; C is nitrite concentration.
Fig. 2 adopts method that the present invention measures nitrite in embodiment two water sample to be analyzed and the water sample analysis that obtains figure as a result.By among Fig. 2 as can be known, 2-amino-5-naphthols-7-sulfonic acid is from coupling spectrophotometry environment water nitrite: relative standard deviation 1.80%, the recovery 98.7%～101.2%.
Embodiment two effect and effects
The present invention discloses a kind of method of measuring nitrite, select hypotoxic 2-amino-5-naphthols-7-sulfonic acid to replace the strong carcinogenicity diazo reagent and the coupling reagent that use in the classic method as diazonium from coupling reagent in the embodiments of the invention two, under the room temperature, diazo-reaction occurs in nitrite and J acid in dilute hydrochloric acid solution, diazo salt and excessive J acid coupling generates red azo compounds compound absorption peak at the 500nm place in aqueous sodium carbonate, calculates the concentration of nitrite by the absorbance of measuring solution.Above experimental result shows, not only simple operation but also sensitivity is higher, the result is accurate of the present invention, and also agents useful for same toxicity is little, can greatly reduce the pollution to operating personnel and environment.
Embodiment three
Sample pretreatment: water sample is taken from respectively Huangpu River tributary and pond, campus, and water sample leaves standstill 30min, gets supernatant liquor 25mL.
Sample tests: pipette water sample 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 0.2mL, shakes up and make diazo liquid, and its pH value is 2.0, with solution left standstill 5min, generates diazonium salt solution.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 6mL.Diazonium salt solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, the solution pH value is 10.0, leaves standstill 30min, and diazo salt can generate red azo compounds with excessive 2-amino-5-naphthols-7-sulfonic acid coupling under alkaline environment.Then, use the 1cm cuvette, reagent blank is made reference, measures the absorbance of solution at wavelength 500nm place.Calculate the content of nitrite according to standard working curve.Do recovery experiment (n=8) and compare with National Standard Method (GB/T 75750.5-2006) with standard addition method.
The configuration of reagent blank: pipette deionized water 10.0mL in the 25mL color comparison tube with transfer pipet, add successively 1% kbr aqueous solution 1.0mL, 1.0 * 10
-2Then the 2-amino of mol/L-5-naphthols-7-sulfonic acid aqueous solution 1.0mL add 1.5mol/L aqueous hydrochloric acid solution 0.2mL, shakes up, with solution left standstill 5min.Other gets the 25mL volumetric flask, adds 1.0mol/L aqueous sodium carbonate 6mL.Solution in the color comparison tube is changed in the volumetric flask that fills aqueous sodium carbonate, then color comparison tube is used a small amount of deionized water rinsing, washing lotion changes in the volumetric flask in the lump, again the solution in the volumetric flask is shaken up, and dilute constant volume with deionized water, and leaving standstill 30min, the solution that obtains is reagent blank.
The drafting of standard working curve: pipette 2.5 * 10
-4Mol/L sodium nitrite titer 0mL, 0.2mL, 0.5mL, 1.0mL, 1.2mL and 1.5mL also add respectively 10mL, 9.8mL, 9.5mL, 9mL, 8.8mL and the dilution of 8.5mL deionized water in 6 25mL color comparison tubes.Add successively 1% potassium bromide solution 1.0mL, 1.0 * 10
-2Mol/L J acid solution 1.0mL, 1.5mol/L hydrochloric acid solution 0.2mL shakes up, and makes diazonium salt solution, with solution left standstill 5min.Other gets 6 25mL volumetric flasks, adds 1.0mol/L sodium carbonate liquor 6mL.Diazonium salt solution is changed in the sodium carbonate liquor, a small amount of deionized water rinsing of diazonium salt solution color comparison tube, washing lotion changes in the sodium carbonate liquor equally, shakes up to dilute constant volume with deionized water afterwards, leaves standstill 30min.Use the 1cm cuvette, reagent blank is made reference, and in wavelength 500nm place its absorbance of sequentially determining, take absorbance as ordinate, nitrite concentration is horizontal ordinate, the drawing standard curve.
According to Specification Curve of Increasing regression equation: A=0.852c (mg/L)+3.0 * 10
-3(r=0.998,0.02mg/L～0.60mg/L).Apparent molar absorption coefficient ε=3.93 * 10
4Lmol
-1Cm
-1Wherein: A is absorbance; C is nitrite concentration.
Fig. 3 adopts method that the present invention measures nitrite in embodiment three water sample to be analyzed and the water sample analysis that obtains figure as a result.As shown in Figure 3,2-amino-5-naphthols-7-sulfonic acid is from coupling spectrophotometry environment water nitrite: relative standard deviation 1.80%, the recovery 98.7%～101.2%.
Embodiment three effect and effects
The present invention discloses a kind of method of measuring nitrite, select hypotoxic 2-amino-5-naphthols-7-sulfonic acid to replace the strong carcinogenicity diazo reagent and the coupling reagent that use in the classic method as diazonium from coupling reagent in the embodiments of the invention three, under the room temperature, diazo-reaction occurs in nitrite and J acid in dilute hydrochloric acid solution, diazo salt and excessive J acid coupling generates red azo compounds compound absorption peak at the 500nm place in aqueous sodium carbonate, calculates the concentration of nitrite by the absorbance of measuring solution.Above experimental result shows, not only simple operation but also sensitivity is higher, the result is accurate of the present invention, and also agents useful for same toxicity is little, can greatly reduce the pollution to operating personnel and environment.
Claims (5)
1. a method of measuring nitrite is characterized in that, may further comprise the steps:
Step 1, water sampling left standstill 30 minutes, then got the supernatant liquor that volume is the described water sample of V1;
Step 2 moves into described supernatant liquor in the color comparison tube, and this color comparison tube is designated as the first color comparison tube, then add successively the certain density kbr aqueous solution of certain volume, 2-amino-5-naphthols-7-sulfonic acid aqueous solution adds aqueous hydrochloric acid solution at last, then shakes up, obtain diazo liquid, be designated as the first solution, its pH value is between 1.0～2.0 scopes, with described first solution left standstill a period of time, the length of described time of repose is designated as A, then obtains the second solution;
Step 3 is got a volumetric flask, is designated as the first volumetric flask, to the aqueous solution that wherein adds a certain amount of sodium carbonate as the PH correctives;
Step 4, described the second solution is transferred to from described the first color comparison tube in the first volumetric flask of the described aqueous solution that fills sodium carbonate, and with a small amount of deionized water rinsing of described the first color comparison tube, washing lotion changes in described the first volumetric flask equally, then shakes up, use the deionized water constant volume, obtain the 3rd solution, its pH value is between 8.2～10.2 scopes, again with described the 3rd solution left standstill number minute, described time of repose is designated as B, obtains the 4th solution;
Step 5 as reference solution, is measured the absorbance of described the 4th solution with reagent blank at wavelength 500nm place;
Step 6 in the regression equation with described absorbance substitution standard working curve, calculates the content of described water sample nitrite;
Wherein, described A is 1～5min;
Described B is 5～30min;
In the step 2, in the described 2-amino of adding-5-naphthols-7-sulfonic acid aqueous solution-amino-concentration of 5-naphthols-7-sulfonic acid in described the first solution is 5.00 * 10
-5～4.00 * 10
-4Mol/L scope internal absorbance is stable.
2. the method for mensuration nitrite according to claim 1 is characterized in that: wherein, the concentration of described hydrochloric acid in described the first solution is during at 0.30～0.60mol/L, and absorbance is stable and maximum.
3. the method for mensuration nitrite according to claim 1, it is characterized in that: wherein, the collocation method of described reagent blank may further comprise the steps:
Step 7, getting volume is color comparison tube of the other injection of deionized water of V1, is designated as the second color comparison tube;
Step 8, in described the second color comparison tube, add successively described kbr aqueous solution, 2-amino-5-naphthols-7-sulfonic acid aqueous solution adds described aqueous hydrochloric acid solution at last, obtains the 5th solution, then described the 5th solution is shaken up, leave standstill after shaking up, described time of repose length is described A, then obtains the 6th solution again;
Step 9, other gets a volumetric flask, is designated as the second volumetric flask, to the aqueous solution that wherein adds described a certain amount of sodium carbonate as the PH correctives;
Step 10, described the 6th solution is transferred to from described the second color comparison tube in the second volumetric flask of the described aqueous solution that fills sodium carbonate, and with a small amount of deionized water rinsing of described the second color comparison tube, washing lotion changes in described the second volumetric flask equally, then uses described deionized water constant volume, shake up again, obtain the 7th solution, then with described the 7th solution left standstill, described time of repose is described B, obtain the 8th solution, be reagent blank.
4. the method for mensuration nitrite according to claim 1 is characterized in that: wherein, the concentration range of contained nitrite must be at 0.02mg/L～0.60mg/L in the water sample that described method is measured.
5. the method for mensuration nitrite according to claim 1, it is characterized in that: wherein, the assay method step of described standard working curve is as follows:
Step 11, the sodium nitrite titer of different volumes is moved into respectively in the other N color comparison tube, be designated as the 3rd color comparison tube series, then add respectively deionized water in described the 3rd color comparison tube series and be diluted to equal volume, thereby obtain having the 9th solution series of equal volume;
Step 12, in described the 9th solution series, add successively described kbr aqueous solution, 2-amino-5-naphthols-7-sulfonic acid aqueous solution, add at last aqueous hydrochloric acid solution, then shake up, obtain the tenth solution series, its pH value is between 1.0～2.0, the tenth solution series is left standstill, time of repose is described A again, then obtains the 11 solution series;
Step 13, described the 11 solution series is changed over to respectively from described the 3rd color comparison tube series in the volumetric flask of aqueous solution that other described N fills described sodium carbonate, be designated as the 3rd volumetric flask series, and with a small amount of deionized water rinsing of described the 3rd color comparison tube series, washing lotion changes in described the 3rd volumetric flask series equally, then shake up, and with described deionized water constant volume, its pH value is between 8.2～10.2, obtain the 12 solution series, then shake up, leave standstill again afterwards, described time of repose is described B, obtains at last the 13 solution series;
Step 14 as reference solution, is measured the absorbance of the 13 solution series with described reagent blank one by one at wavelength 500nm place;
Step 15 according to the absorbance drawing standard curve of described the 13 solution series, is carried out linear fit to described typical curve again and is obtained regression equation;
Wherein, described N is not less than 5 natural number.
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| CN2012104226224A CN102928369A (en) | 2012-10-30 | 2012-10-30 | Method for measuring nitrite |
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Cited By (7)
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| CN104458619A (en) * | 2014-12-12 | 2015-03-25 | 上海理工大学 | Method for determining content of oxynitride in air |
| CN104777111A (en) * | 2015-03-27 | 2015-07-15 | 上海理工大学 | Sodium nitrite determination method |
| CN105277542A (en) * | 2015-02-05 | 2016-01-27 | 温州医科大学 | On-site rapid detection method for nitrite in water and capable of eliminating reagent blank effects |
| CN107356539A (en) * | 2017-07-13 | 2017-11-17 | 山东科技大学 | A kind of method of nitrogen nutrition salinity in quick detection seawater |
| CN108732299A (en) * | 2018-06-01 | 2018-11-02 | 遵义医学院 | The colorimetric detection method of water quality nitrite |
| CN109030396A (en) * | 2018-08-04 | 2018-12-18 | 海南威尔检测技术有限公司 | The rapid assay methods of nitrate in cultivation water |
| CN110261377A (en) * | 2019-07-24 | 2019-09-20 | 四川农业大学 | A kind of nitrite quick detection reagent and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458619A (en) * | 2014-12-12 | 2015-03-25 | 上海理工大学 | Method for determining content of oxynitride in air |
| CN105277542A (en) * | 2015-02-05 | 2016-01-27 | 温州医科大学 | On-site rapid detection method for nitrite in water and capable of eliminating reagent blank effects |
| CN105277542B (en) * | 2015-02-05 | 2018-02-06 | 温州医科大学 | A kind of water nitrite field fast detection method for eliminating reagent blank influence |
| CN104777111A (en) * | 2015-03-27 | 2015-07-15 | 上海理工大学 | Sodium nitrite determination method |
| CN107356539A (en) * | 2017-07-13 | 2017-11-17 | 山东科技大学 | A kind of method of nitrogen nutrition salinity in quick detection seawater |
| CN108732299A (en) * | 2018-06-01 | 2018-11-02 | 遵义医学院 | The colorimetric detection method of water quality nitrite |
| CN108732299B (en) * | 2018-06-01 | 2020-10-16 | 遵义医科大学 | Colorimetric detection method for nitrite in water |
| CN109030396A (en) * | 2018-08-04 | 2018-12-18 | 海南威尔检测技术有限公司 | The rapid assay methods of nitrate in cultivation water |
| CN110261377A (en) * | 2019-07-24 | 2019-09-20 | 四川农业大学 | A kind of nitrite quick detection reagent and preparation method thereof |
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