CN109856123A - A kind of nitrate quick detection reagent and detection method - Google Patents
A kind of nitrate quick detection reagent and detection method Download PDFInfo
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Abstract
The invention discloses a kind of nitrate quick detection reagent and detection methods, the nitrate quick detection reagent includes reagent I and reagent II, in which: the reagent I consists of the following mass percentage components: organic acid: 58%~88.5%, cadmium powder: 1%~10%, sulfanilamide (SN): 0.5%~2%, polyvinylpyrrolidone: 10%~30%；The reagent II consists of the following mass percentage components: hydrochloride naphthodiamide: 2%~6%, organic acid: 94%~98%.Nitrate field fast detection method of the invention adds nitrate quick detection reagent of the invention, develops the color the following steps are included: 1) by water sample to be measured addition colorimetric bottle；2) reference standard colorimetric card or the standard curve of drafting, obtain the nitrate content of water sample to be measured.The adaptable of nitrate quick detection reagent of the invention, stability are good, and the fast-field evaluation of nitrate in water quality and food sample can be carried out with planning standard colorimetric card or portable colorimeter.
Description
Technical field
The present invention relates to a kind of nitrate quick detection reagent and detection methods.
Background technique
NO3-N and NO2-N is the most common nitrogenous compound in nature.The appearance and flavour of nitrite all with
Salt is similar, can be used as food additives use, but the nitrite added in food is excessive and will lead to eater's poisoning.
The intracorporal nitrate of people can be converted to nitrite under the action of microorganism, so to determine whether water quality and food pacify
Entirely, it not only needs to measure the content of nitrite, but also needs to measure the content of nitrate.Such as: white sugar is commonly to eat
Product additive, different material preparation white sugar in the content of nitrite and nitrate have larger difference, nitre in general beet sugar
The content of hydrochlorate is apparently higher than sucrose, so content of the enterprise of production beet sugar in addition to needing to control nitrite in finished product,
Also need to control the content of nitrate in finished product.
The measuring method of nitrate mainly has Ultraviolet Photometric Method, chromotropic acid photometry, Cadmium column reduction-diazonium even in laboratory
Close colour developing photometry etc..Ultraviolet Photometric Method need to use large-scale spectrophotometer, and big by matrix interference.Chromotropic acid photometry needs
The concentrated sulfuric acid is used, and reagent itself easily changes colour, it is not easy to maintain.Cadmium column reduction-diazo coupling colour developing photometry not only operates numerous
Trivial time-consuming, and as access times increase, it is unstable to will cause test data for the cadmium aging of column.Currently, the quick inspection of nitrate
Survey method mainly has nitrate-test strip method and cadmium powder method of testing.The sensitivity of nitrate-test strip method and test accuracy are relatively low,
It is unsuitable for carrying out high precision measurement.There is poor repeatability in existing cadmium powder method of testing, carry out for same sample multiple
Test, test result is it is possible that difference at double.
Therefore, it is necessary to develop a kind of high sensitivity, the nitrate quick detection reagent that easy to operate, measuring accuracy is high and
Detection method.
Summary of the invention
The purpose of the present invention is to provide a kind of nitrate quick detection reagent and detection methods.
The technical solution used in the present invention is:
A kind of nitrate quick detection reagent, including reagent I and reagent II, in which:
The reagent I consists of the following mass percentage components: organic acid: 58%~88.5%, cadmium powder: 1%~
10%, sulfanilamide (SN): 0.5%~2%, polyvinylpyrrolidone: 10%~30%；
The reagent II consists of the following mass percentage components: hydrochloride naphthodiamide: 2%~6%, organic acid:
94%~98%.
Preferably, the organic acid is one of tartaric acid, citric acid.
Preferably, the partial size of the cadmium powder is less than 38 μm.
Preferably, a kind of nitrate quick detection reagent, including reagent I and reagent II, in which:
The reagent I consists of the following mass percentage components: tartaric acid: 75.7%, cadmium powder: 3.3%, sulfanilamide (SN):
1%, polyvinylpyrrolidone: 20%；
The reagent II consists of the following mass percentage components: hydrochloride naphthodiamide: 2%, tartaric acid: 98%.
Preferably, the reagent I and reagent II are independently dispensed, and the quality of every part of reagent I is 0.2~0.3g, and reagent II is every
The quality of part is 0.1~0.2g.
A method of nitrate field quick detection, including following step are carried out using above-mentioned nitrate quick detection reagent
It is rapid:
1) water sample to be measured is added in clean colorimetric bottle, addition reagent I, 2~4min of shaking, 2~4min of standing, then plus
Enter reagent II, shake up, stands 10~15min；
2) reference standard colorimetric card carries out color contrast, obtains the nitrate content of water sample to be measured, alternatively, the standard of drafting is bent
It is detected after line using portable colorimeter or spectrophotometer, obtains the nitrate content of water sample to be measured.
Preferably, the mode of the step 1) shaking is shaking manually or the shaking of vortex instrument, and shaking frequency is greater than 250
Secondary/min.
Preferably, the step 2) standard color comparison card the production method is as follows:
1) be 0.05mg/L, 0.1mg/L with pure water compound concentration, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L,
The nitrate nitrogen standard solution of 0.7mg/L, 1.0mg/L；
2) the nitrate nitrogen standard solution that concentration is 0.05mg/L is added in clean colorimetric bottle, reagent I, shaking is added
2~4min stands 2~4min, adds reagent II, shake up, and stands 10~15min, observes the color of solution, and in Pan Tongse
Corresponding reference colour is found out on card, repeats the operation, is respectively 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/ to concentration
L, the nitrate nitrogen standard solution of 0.5mg/L, 0.7mg/L, 1.0mg/L are tested；
3) control pantone obtains the color value of each reference colour, by computer color-mixed and printing, obtains standard color comparison card.
It, can be with the beneficial effects of the present invention are: the adaptable of nitrate quick detection reagent of the invention, stability are good
Planning standard colorimetric card or portable colorimeter carry out the fast-field evaluation of nitrate in water quality and food sample.
1) it is added with polyvinylpyrrolidone (PVP) in nitrate quick detection reagent of the invention, there is following 4 side
The effect in face: PVP can promote merging for cadmium powder and other components, and then can be to avoid reagent during mixing and packaging
There is separation layering, ensure that the uniformity that cadmium powder is distributed in reagent；PVP can go to destatic, and then can exist to avoid reagent
Mix and packaging during cadmium powder and container friction generate electrostatic and adsorb on the wall, avoid because cadmium powder loss and
The problem of caused test result inaccuracy；The dispersion of cadmium powder in the solution when reaction can be enhanced using its surface-active in PVP
Property, so can be dissolved in an acidic solution to avoid cadmium powder aggregation it is blocking caused by reduction efficiency decline the problem of；PVP is readily soluble
Yu Shui, and this is as chemical inertness, will not influence reduction and color developing effect；
2) present invention also further by the size controlling of cadmium powder at 38 μm hereinafter, not only increasing the uniform of cadmium powder diameter
Property, guarantee that effective surface area is consistent when the reduction of cadmium powder, but also cadmium powder can be further avoided and separate layering with other components；
3) reaction time of shaking time, frequency, each step is optimized in the present invention, is first carried out using reagent I
Then adequately reduction and diazo-reaction carry out coupling colour development reaction using reagent II again, can shorten the chromogenic reaction time,
So that absorbance is rapidly achieved stabilization, significantly improves the controllability of reaction.
Specific embodiment
The present invention will be further explained combined with specific embodiments below and explanation.
Embodiment 1:
A kind of nitrate quick detection reagent, including reagent I and reagent II, in which:
The reagent I is composed of the following components: tartaric acid: 75.70g, cadmium powder (partial size is less than 38 μm): 3.30g, sulfanilamide (SN):
1.00g, PVP:20.00g；Each component in reagent I is sufficiently mixed uniformly, then is packed on powder automatic packaging machine, specification
For 0.30g/ packet；
The reagent II is composed of the following components: hydrochloride naphthodiamide: 2.00g, tartaric acid: 98.00g；It will be in reagent II
Each component be sufficiently mixed uniformly, then packed on powder automatic packaging machine, specification is 0.20g/ packet.
Embodiment 2:
A kind of nitrate quick detection reagent, including reagent I and reagent II, in which:
The reagent I is composed of the following components: tartaric acid: 74.00g, cadmium powder (partial size is less than 38 μm): 5.00g, sulfanilamide (SN):
1.00g, PVP:20.00g；Each component in reagent I is sufficiently mixed uniformly, then is packed on powder automatic packaging machine, specification
For 0.20g/ packet；
The reagent II is composed of the following components: hydrochloride naphthodiamide: 4.00g, tartaric acid: 96.00g；It will be in reagent II
Each component be sufficiently mixed uniformly, then packed on powder automatic packaging machine, specification is 0.10g/ packet.
Embodiment 3:
Standard color comparison card the production method is as follows:
1) be 0.05mg/L, 0.1mg/L with pure water compound concentration, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L,
The nitrate nitrogen of 0.7mg/L, 1.0mg/L are (with NO3- N meter) standard solution；
2) the nitrate nitrogen standard solution that concentration is 0.05mg/L is added in clean colorimetric bottle to 10mL graduation mark, is added
The reagent I for entering the preparation of 1 packet embodiment 1 shakes 3min on vortex instrument, stands 2min, adds the examination of 1 packet embodiment 1 preparation
Agent II, shakes 5min on vortex instrument, stands 10min, then colorimetric bottle is placed in white PVC board, from bottleneck downwards from
The color of solution, and corresponding reference colour is found out in pantone, the operation is repeated, be respectively 0.1mg/L to concentration,
The nitrate nitrogen standard solution of 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.7mg/L, 1.0mg/L are tested；
3) control pantone obtains the color value of each reference colour, by computer color-mixed and printing, obtains standard color comparison card.
Test case 1:
Referring to embodiment 1, it is 0,5.0%, 10.0%, 20.0%, 30.0% that the content of PVP in reagent I, which is adjusted separately,
The content of tartaric acid accordingly adjusts are as follows: and 95.7%, 90.7%, 85.7%, 75.7%, 65.7%, remaining constituent content is constant, point
It is not configured to nitrate quick detection reagent, uses the nitrate nitrogen that concentration is 1.0mg/L (with NO3- N meter) standard liquid, in vortex
3min is shaken on instrument at a high speed, after colour developing on spectrophotometer, at wavelength 525nm, using pure water as reference, using 1cm cuvette
The test of standard coloration liquid absorbance value is carried out, every kind of reagent is tested in the different time sections sampling of packaging (survey altogether respectively
Examination 5 times), test result is as follows shown in table:
Influence of the 1 PVP content of table to test effect
As shown in Table 1:
1) content of PVP has very big influence to test effect；
2) when being free of PVP in formula, not only developing sensitivity is not high, but also the also very bad (RSD=of test repeatability
7.9%), visual observations are attracted on chamber wall and aluminum foil sack to cadmium powder part and cause loss, cadmium powder after reaction
There is apparent caking phenomenon, and separation lamination occurs in mixing and packaging process in cadmium powder；
3) increasing with PVP additional amount, measurement sensitivity and precision are gradually increased, visual observations to cadmium powder agglomeration situation
It fades away, mixing and the absorption in packaging process and separation lamination no longer occur；
4) in order to guarantee measurement sensitivity and precision, in reagent I the content of PVP it is necessary >=10%, but PVP content simultaneously
It is not preferably greater than 30% (PVP too high levels, which are easy the moisture absorption, to be caused to can not be successfully blanking when packaging), optimum content 20%.
Test case 2:
Commercially available cadmium powder (purity: 5N) is separated with 80,150,200,325,400,500 mesh standard sieves respectively, refers again to reality
It applies example 1 and nitrate quick detection reagent is respectively prepared, use the nitrate nitrogen that concentration is 1.0mg/L (with NO3- N meter) standard liquid,
3min is shaken on vortex instrument at a high speed, after colour developing on spectrophotometer, at wavelength 525nm, using pure water as reference, using 1cm ratio
Color ware carries out the test of standard coloration liquid absorbance value, and every group reagent carries out 5 parallel tests respectively, test result is as follows table institute
Show:
Influence of the 2 cadmium powder diameter of table to test collimation
As shown in Table 2: the partial size of cadmium powder has very big influence to test repeatability and developing sensitivity.When cadmium powder
When diameter is larger, cadmium powder is difficult to be evenly distributed in reagent and (estimate it can be seen that apparent separation lamination, each section cadmium powder is all
It is gathered in bottom)；As cadmium powder diameter becomes smaller, cadmium powder is gradually evenly distributed in reagent, effectively restores surface area and also increases therewith
Add, the repeatability and developing sensitivity of test all gradually improve；In order to guarantee that test effect, the mesh number of cadmium powder have to be larger than 400
Mesh (i.e. partial size is less than 38 μm).
Test case 3:
Using the nitrate quick detection reagent prepared in embodiment 1, use nitrate nitrogen that concentration is 1.0mg/L (with
NO3- N meter) standard liquid, it is shaken at a high speed on vortex instrument, the change shaking time (adds in nitrate field fast detection method step 1
The shaking time after entering reagent I), after the different time that develops the color on spectrophotometer, at wavelength 525nm, using pure water as reference,
The test of standard coloration liquid absorbance value is carried out using 1cm cuvette, test result is as follows shown in table:
The influence of the shaking time of table 3
As shown in Table 3: there is larger impact in the shaking time to test result, when colour developing absorbance is with shaking when being lower than 3min
Between extension and improve, and the color stability time is gradually shortened to 5min, reduces instead greater than test result after 3min, it may be possible to
Nitrate nitrogen over reduction is to select vortex shaking 3min the most suitable caused by ammoniacal nitrogen.
Test case 4:
It is tested using actual water sample, white sugar sample and syrup sample.
1) sample pre-treatments:
White sugar sample (offer of research institute, China Oil and Food Import and Export Corporation): claim 5.00g white sugar, 100mL sample is configured to using deionized water or pure water
Solution.Test result is multiplied by extension rate: 20.
Syrup sample (offer of research institute, China Oil and Food Import and Export Corporation): claim 1.00g syrup, 1000mL sample is configured to using deionized water or pure water
Solution.Test result is multiplied by extension rate: 1000 (syrup sample as dark brown, more than 1000 times of dilution can just eliminate
Background color bring influences).
2) drafting of standard curve:
Preparing series of concentrations (in terms of N) is 0.1mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L
Nitrate standard solution.1 clean colorimetric bottle is taken, the reagent prepared in 1 packet embodiment 1 is added in mark-on liquid to 10mL graduation mark
I, 3min is shaken on vortex instrument at a high speed, 2min is stood, adds the reagent II prepared in 1 packet embodiment 1, shake up dissolution, standing
10min is reacted, on spectrophotometer, at wavelength 525nm, using pure water as reference, standard coloration liquid is carried out using 1cm cuvette
The test of absorbance value, is depicted as standard curve.
Calibration curve equation are as follows: C=0.4679A-0.0069, R2=0.9999 (equation linearity is very good, test model
It encloses for 0~1.0mg/L), wherein C is nitrate concentration, and A is colour developing absorbance.
3) test of sample:
A clean colorimetric bottle is taken, adds water sample to 10mL graduation mark, develops the color according to standard liquid test method, colorimetric cylinder is placed on
The intermediate blank area of standard color comparison card prepared by embodiment 3, from the downward visual colorimetric determination of bottleneck, color identical with solution tone in bottle
Rank instruction concentration is the content of nitrate in sample liquid, while the test of absorbance, generation are carried out on DR3900 spectrophotometer
Enter in above-mentioned standard curvilinear equation and calculates nitrate content.If water sample test result no to scale, is tested after can suitably diluting.
Recovery of standard addition test has been carried out according to photometry test result simultaneously.Test result is as follows for water sample shown in table:
4 water sample test result of table
Note: no to scale range when being tested with actual water sample retests after 5 times of dilution, and above-mentioned test result is to measure
Data are multiplied by obtained by extension rate.Standard substance is added in raw water sample when testing in mark-on.
A clean colorimetric bottle is taken, adds white sugar sample or syrup sample to 10mL graduation mark, develops the color, will compare according to standard liquid test method
Colour tube is placed on the intermediate blank area of the standard color comparison card of the preparation of embodiment 3, from the downward visual colorimetric determination of bottleneck, with solution color in bottle
It adjusts identical color range instruction concentration to be the content of nitrate in sample liquid, while carrying out absorbance on DR3900 spectrophotometer
Test, substitute into above-mentioned standard curvilinear equation in calculate nitrate content.Added simultaneously according to photometry test result
Mark recovery test.Test result is as follows shown in table for white sugar sample and syrup sample:
5 white sugar sample of table and syrup sample test result
Note: carrying out mark-on test for convenience, and standard substance is directly added in dilution, and result above is that dilution is straight
Test result is connect, not multiplied by extension rate.
From table 4 and table 5: colorimetric block-regulations and photometry test result are more consistent, are very suitable for field application.And
This method measurement sensitivity is relatively high, and particularly suitable for the dark sample such as syrup, these samples are diluted to almost colourless rear survey
Examination still can accurately test out result.This test recovery of standard addition illustrates creek between 96.00% to 102.00%
Water sample, white sugar sample and syrup sample can be measured directly after simply preparing or diluting, reliable test result.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of nitrate quick detection reagent, it is characterised in that: including reagent I and reagent II, in which:
The reagent I consists of the following mass percentage components: organic acid: 58%~88.5%, cadmium powder: 1%~10%, sulphur
Amine: 0.5%~2%, polyvinylpyrrolidone: 10%~30%；
The reagent II consists of the following mass percentage components: hydrochloride naphthodiamide: 2%~6%, organic acid: 94%~
98%.
2. nitrate quick detection reagent according to claim 1, it is characterised in that: the organic acid is tartaric acid, lemon
One of lemon acid.
3. nitrate quick detection reagent according to claim 1, it is characterised in that: the partial size of the cadmium powder is less than 38 μ
m。
4. nitrate quick detection reagent according to claim 1, it is characterised in that: including reagent I and reagent II,
In:
The reagent I consists of the following mass percentage components: tartaric acid: 75.7%, cadmium powder: 3.3%, sulfanilamide (SN): 1%, gathering
Vinyl pyrrolidone: 20%；
The reagent II consists of the following mass percentage components: hydrochloride naphthodiamide: 2%, tartaric acid: 98%.
5. nitrate quick detection reagent described according to claim 1~any one of 4, it is characterised in that: the reagent I
It is independently dispensed with reagent II, the quality of every part of reagent I is 0.2~0.3g, and the quality of every part of reagent II is 0.1~0.2g.
6. a kind of nitrate field fast detection method, it is characterised in that: using described in any one of Claims 1 to 5
Nitrate quick detection reagent is detected, specifically includes the following steps:
1) water sample to be measured is added in clean colorimetric bottle, reagent I is added, shake 2~4min, stood 2~4min, add examination
Agent II, shakes up, and stands 10~15min；
2) reference standard colorimetric card carries out color contrast, obtains the nitrate content of water sample to be measured, alternatively, after drawing standard curve
It is detected using portable colorimeter or spectrophotometer, obtains the nitrate content of water sample to be measured.
7. nitrate field fast detection method according to claim 6, it is characterised in that: the side of the step 1) shaking
Formula is shaking manually or the shaking of vortex instrument, and shaking frequency is greater than 250 times/min.
8. nitrate field fast detection method according to claim 6, it is characterised in that: the step 2) standard colorimetric
Card the production method is as follows:
It 1) is 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.7mg/ with pure water compound concentration
L, the nitrate nitrogen standard solution of 1.0mg/L；
2) the nitrate nitrogen standard solution that concentration is 0.05mg/L is added in clean colorimetric bottle, addition reagent I, shaking 2~
4min stands 2~4min, adds reagent II, shake up, and stands 10~15min, observes the color of solution, and in pantone
On find out corresponding reference colour, repeat the operation, respectively to concentration be 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L,
The nitrate nitrogen standard solution of 0.5mg/L, 0.7mg/L, 1.0mg/L are tested；
3) control pantone obtains the color value of each reference colour, by computer color-mixed and printing, obtains standard color comparison card.
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| CN113418913A (en) * | 2021-06-24 | 2021-09-21 | 神美科技有限公司 | Stable nitrite test paper and preparation method thereof |
| CN113670902A (en) * | 2021-07-02 | 2021-11-19 | 四川师范大学 | Detection agent for rapidly and quantitatively determining nitrite and detection method thereof |
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| CN115575390A (en) * | 2022-09-30 | 2023-01-06 | 广东省环境科学研究院 | Combined reagent for monitoring water quality and use method thereof |
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| CN113418913A (en) * | 2021-06-24 | 2021-09-21 | 神美科技有限公司 | Stable nitrite test paper and preparation method thereof |
| CN113670902A (en) * | 2021-07-02 | 2021-11-19 | 四川师范大学 | Detection agent for rapidly and quantitatively determining nitrite and detection method thereof |
| CN115436585A (en) * | 2022-07-25 | 2022-12-06 | 广州伊创科技股份有限公司 | Online intelligent labeling method for water quality monitoring |
| CN115575390A (en) * | 2022-09-30 | 2023-01-06 | 广东省环境科学研究院 | Combined reagent for monitoring water quality and use method thereof |
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