CN107091823A - A kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method - Google Patents
A kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method Download PDFInfo
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Abstract
The invention belongs to water quality inspection technique field, specifically related to a kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method, the low-concentration ammonia-nitrogen fluoroscopic examination solid reagent includes a sodium sulfite-buffer reagent bag and an O-phthalic aldehyde reagent bag, and the sodium sulfite-buffer reagent bag includes 30-40wt% sodium sulfite, 5-15wt% borax, 0-1wt% lithium hydroxide and 50-60wt% sodium chloride；The O-phthalic aldehyde reagent bag is made up of OPA.The low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method of the present invention, can accurately determine the ammonia nitrogen value in water body, and detection reagent sensitivity is high, and the holding time is long.
Description
Technical field
The invention belongs to water quality inspection technique field, and in particular to a kind of low-concentration ammonia-nitrogen fluoroscopic examination solid examination
Agent and its detection method.
Background technology
Ammonia nitrogen refers to the ammonia existed in water with free ammonia and ammonium salts.During the source of ammonia nitrogen is mainly sanitary sewage
Itrogenous organic substance is by the catabolite of microbial action, some industrial wastewaters, such as water flowers waste water and synthesis ammonification
Fertile factory etc., and agricultural drain.Ammonia nitrogen is the nutrient in water body, and water eutrophication phenomenon can be caused to produce,
It is the main oxygen consumption pollutant in water body, it is toxic to fish and some aquatiles.The analysis of current ammonia nitrogen
Detection method has this several class：(1) AAS, including Na's reagent, salicylic acid-hypochlorite ratio
Color method, indophenol blue photometry etc.；(2) electrochemical methods, including ammonia gas-sensing electrode, stripping-conductance method,
Ammonium ion selective electrode；(3) instrumental method, including Kjeldahl's method, chromatography；(4) other
Method also has, distillation-titration, Flow Injection Analysis, enzyme process etc..But, these existing ammonia nitrogen detection sides
Method still has defect.For example, Na's reagent, salicylic acid-hypochlorite colorimetric method easily by calcium in water,
The metal ion such as magnesium and iron, sulfide, aldehyde and ketone, color, and the interference such as muddiness, need to do corresponding
Pretreatment.Electrode method survey ammonia nitrogen interference be mainly volatile amine produce, mercury and Yin Yin and ammino make a concerted effort it is strong and
There are interference, the interference of high concentration dissolving ion.Instrumental method needs expensive instrument, is unfavorable for just
Take and field assay.Enzyme process and RNA isolation kit survey ammonia nitrogen, and accuracy is poor, is not suitable for quantitative analysis.Adjacent benzene
Fluorescent derivatization between dicarbaldehyde and ammonia nitrogen, which reacts, causes the micro ammonia nitrogen in Fluorometric assay water body turns into can
Energy.
The existing method for surveying ammonia nitrogen is all constrained to the conditions such as instrument, equipment and reagent；And the measurement of ammonia nitrogen
Sensitivity be mg/L.
The fluorescence measurement ammonia nitrogen of document report, is all to use OPA solution and sodium sulfite solution, but deposit
In problems with --- sodium sulfite solution normal temperature preserves unstable；OPA solution process for preparation dissolves
Time is long, needs to be kept in dark place after preparing, the defect such as storage life is short.
The content of the invention
, can be accurate invention broadly provides a kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method
The true ammonia nitrogen value determined in water body, detection reagent sensitivity is high, and the holding time is long.Its technical scheme is as follows：
A kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent, including a sodium sulfite-buffer reagent bag and an adjacent benzene
Diformazan aldehyde reagent bag, the sodium sulfite-buffer reagent bag includes 30-40wt% sodium sulfite, 5-15wt%
Borax, 0-1wt% lithium hydroxide and 50-60wt% sodium chloride；The O-phthalic aldehyde reagent bag is by neighbour
Phthalaldehyde is constituted.
It is preferred that, the weight of a sodium sulfite-buffer reagent bag is 0.08-0.12g.
It is preferred that, the weight of a sodium sulfite-buffer reagent bag is 0.1g.
It is preferred that, the weight of an O-phthalic aldehyde reagent bag is 0.03-0.05g.
It is preferred that, the weight of an O-phthalic aldehyde reagent bag is 0.04g.
A kind of detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent, comprises the following steps：
(1) 10ml water samples are taken, a sodium sulfite-buffer reagent bag is added in water sample, rocks and is allowed to molten
Solution；
(2) a cosolvent is added, is shaken up；
(3) add an O-phthalic aldehyde reagent bag and rock and be allowed to dissolve；
(4) fluorescence signal is detected on SP-900 Portable water-quality analysis instruments, calculates ammonia nitrogen in sample
Solubility.
It is preferred that, the volume of a cosolvent is 1ml in step (2), and the cosolvent is ethylene glycol and second
The mixed solution of alcohol.
It is preferred that, the cosolvent is that ethylene glycol and ethanol are 2 by volume:The solution of 8 ratio mixing.
It is preferred that, the excitation wavelength of detection fluorescence signal is 300-400nm in step (4), and launch wavelength is
350-450nm。
Using above-mentioned low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method, the present invention has following excellent
Point：
Low content ammonia nitrogen is detected using solid reagent bag in the detection method of the present invention, specific is to use sulfurous
Sour sodium and OPA solid reagent bag, solves the problem of both solution are unstable.Otherwise for adjacent benzene
The problem of dicarbaldehyde is water insoluble, the ethylene glycol that this method is added in cosolvent, cosolvent causes O-phthalic
Aldehyde is easier to be dissolved in water sample, more traditional detection method, and the reagent in the method is stored more easily, detection
Method is more convenient, and testing result is more accurate.
Brief description of the drawings
Fig. 1 is the standard fluorometric detection curve map of ammonia nitrogen.
Embodiment
A kind of detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent, comprises the following steps：
(1) 10ml water samples are taken, a sodium sulfite-buffer reagent bag is added in water sample, rocks and is allowed to molten
Solution；
(2) a cosolvent is added, is shaken up；
(3) add an O-phthalic aldehyde reagent bag and rock and be allowed to dissolve；
(4) fluorescence signal is detected on SP-900 Portable water-quality analysis instruments, calculates ammonia nitrogen in sample
Solubility.
Wherein, the weight of a sodium sulfite-buffer reagent bag is 0.08-0.12g, the Asia in step (1)
Sodium sulphate-buffer reagent bag includes 30-40wt% sodium sulfite, 5-15wt% borax, 0-1wt% hydrogen-oxygen
Change lithium and 50-60wt% sodium chloride.
The volume of a cosolvent is 1ml in step (2), and the cosolvent is that ethylene glycol and ethanol press volume
Than for 2:The solution of 8 ratio mixing.
The weight of an O-phthalic aldehyde reagent bag is 0.03-0.05g, the OPA in step (3)
Reagent bag is made up of OPA.
The excitation wavelength of detection fluorescence signal is 300-400nm in step (4), and launch wavelength is 350-450nm.
Specific embodiment
Embodiment 1
1. the preparation of sodium sulfite-buffer reagent bag
One sodium sulfite-buffer reagent includes：0.03g sodium sulfite, 0.01g borax, 0.001g
Lithium hydroxide and 0.059g sodium chloride.
2. the preparation of cosolvent
A cosolvent is mixed by 0.2ml ethylene glycol and 0.8ml ethanol, shady place sealing preserve.
3. the preparation of O-phthalic aldehyde reagent bag
One O-phthalic aldehyde reagent includes 0.04g OPA powder.
Embodiment 2
1. the preparation of sodium sulfite-buffer reagent bag
One sodium sulfite-buffer reagent includes：0.035g sodium sulfite, 0.015g borax and 0.05g
Sodium chloride.
2. the preparation of cosolvent
A cosolvent is mixed by 0.2ml ethylene glycol and 0.8ml ethanol, shady place sealing preserve.
3. the preparation of O-phthalic aldehyde reagent bag
One O-phthalic aldehyde reagent includes 0.05g OPA powder.
Embodiment 3
1. the preparation of sodium sulfite-buffer reagent bag
One sodium sulfite-buffer reagent includes：0.04g sodium sulfite, 0.005g borax, 0.001g
Lithium hydroxide and 0.054g sodium chloride.
2. the preparation of cosolvent
A cosolvent is mixed by 0.2ml ethylene glycol and 0.8ml ethanol, shady place sealing preserve.
3. the preparation of O-phthalic aldehyde reagent bag
One O-phthalic aldehyde reagent includes 0.03g OPA powder.
Embodiment 4
1. the preparation of Ammonia nitrogen standard liquid
The accurate 3.145g ammonium chlorides (purity more than 99.5%) that weigh are placed in dissolving in 250mL beakers, move into
In 1000mL volumetric flasks, scale is diluted to ultra-pure water, is shaken up, the ammonia nitrogen in this solution is (with NH3)
Concentration is 1000ppm.
The accurate ammonia nitrogen for measuring 1.0mL, 1000ppm is diluted to quarter with ultra-pure water into 100mL volumetric flasks
Degree, shakes up, the ammonia nitrogen in this solution is (with NH3) concentration be 10ppm.
The accurate ammonia nitrogen for measuring 1.0mL, 10ppm is diluted to scale into 100mL volumetric flasks with ultra-pure water,
Shake up, the ammonia nitrogen in this solution is (with NH3) concentration be 100ppb.
Accurately measure 0.5 respectively, 1.0,1.5,2.0,2.5,3.0,3.5mL 100ppb ammonia nitrogen to 50mL
In volumetric flask, scale is diluted to ultra-pure water, is shaken up, the ammonia nitrogen in this solution is (with NH3) concentration point
Wei not 10ppb, 20ppb, 30ppb, 40ppb, 50ppb, 60ppb, 70ppb.
2. the drafting of ammonia nitrogen standard fluorometric detection curve
Take 10 respectively, 20,30,40,50,60,70ppb Ammonia nitrogen standard liquid, pour into 7 colorimetrics
In bottle, to 10mL graduation marks；First add one embodiment 1 in sodium sulfite buffer reagent bag, shake up to
Solid dissolving；Then the cosolvent added in a embodiment 1, is mixed；Add in one embodiment 1
O-phthalic aldehyde reagent bag, shake up to solid and be completely dissolved；After reaction 30 minutes, finally in SP-900
On Portable Water Analyzer (Portable water-quality analysis instrument) by 365nm of excitation wavelength, transmitted wave
A length of 420nm condition detection fluorescence signal, draws standard curve.Standard curve is as shown in figure 1, linear
Scope is 10-70ppb.Calibration curve equation is Y=610.15X+13966, R2=0.9989 (X=ammonia nitrogen concentrations,
Y=fluorescence signals).
Embodiment 5
Detection limit is defined
Tested with seven groups of blank samples, the reagent that following reagent bag or cosolvent are selected in embodiment 1.Take
It is each to add 10mL ultra-pure waters in 7 colorimetric bottles, first add a sodium sulfite buffer reagent bag, shake up to
Solid dissolving；Then a cosolvent is added, is mixed, is eventually adding an O-phthalic aldehyde reagent bag, shakes
It is even to solid dissolving；After reaction 30 minutes, fluorescence is detected on SP-900Portable Water Analyzer
Signal.7 groups of fluorescence intensity is 10656,9430,10449,10675,10855,10580,9761 respectively,
Standard deviation is 533.86.According to formula below, detection limit is calculated：
DL in formula --- detection limit；σ --- the standard deviation of 7 groups of blank samples；B --- standard curve it is oblique
Rate.
So detection is limited to 2.6ppb.
Embodiment 6
So that the ammonia nitrogen concentration of water sample is 10ppb as an example, ammonia is carried out with the method in conventional method and the present invention respectively
The measure of nitrogen content.
Conventional method：Prepare 0.3M sodium sulfite solutions, borax-sodium hydroxide buffer solution (pH=9.4) and
40g/L OPA ethanol solutions.1mL sodium sulfite solutions, 1mL boron are added in 10mL water samples
Sand-sodium hydroxide buffer solution (pH=9.4) and 1mL OPA solution, react 30 minutes, in SP-900
Fluorescence signal is detected on Portable Water Analyzer.
Method in the present invention：The reagent that following reagent bag or cosolvent are selected in embodiment 2.In 10mL
A sodium sulfite-buffer reagent bag, a cosolvent and a O-phthalic aldehyde reagent are sequentially added in water sample
Bag, rocks and treats that solid reagent dissolves, react 30 minutes, on SP-900Portable Water Analyzer
By 365nm of excitation wavelength, launch wavelength detect fluorescence signal for 420nm condition, then substitute into
Y=610.15X+13966 is calculated, and draws corresponding ammonia nitrogen concentration.
Each horizontal survey of two methods 3 times, it is as a result as follows：
The measurement result of table 1
As a result with analysis：Both method measurement results are consistent.Car following-theory value is compared, the solid reagent in the present invention
Bao Fageng is accurately and reliably.
Embodiment 7
The stability of OPA solution and OPA solid compares
1. prepare OPA solution：Precise 2.000g OPAs are in 50mL ethylene glycol-ethanol
(volume ratio is 2：8) in solution, it is sufficiently mixed, lucifuge is rocked, lucifuge sealing preserve.Due to adjacent benzene two
Formaldehyde is less soluble, so need to shift to an earlier date preparation in 2 days.
OPA solid reagent bag：Vacuum sealing, is kept in dark place at room temperature.
Reacted 2. being made of OPA solution：After 7 days, reaction solution fluorescence signal declines 18.3%；After 14 days,
Reaction solution fluorescence signal declines 39.3%
Make and react of OPA solid reagent bag：After 30 days, reaction solution fluorescence signal is constant.
In summary, OPA solution process for preparation dissolution time is long, needs to be kept in dark place after preparing,
Storage life is less than 14 days.Solid reagent bag method is simple to operate liquid reagent solidification, can for a long time preserve and (protect
The phase is deposited more than 30 days), with very big advantage.
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make it
Its various corresponding changes and deformation, and all these change and deformation should all belong to power of the present invention
Within the protection domain that profit is required.
Claims (9)
1. a kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent, including a sodium sulfite-buffer reagent bag and one
Individual O-phthalic aldehyde reagent bag, sodium sulfite of the sodium sulfite-buffer reagent bag including 30-40wt%,
The sodium chloride of 5-15wt% borax, 0-1wt% lithium hydroxide and 50-60wt%；The OPA examination
Agent bag is made up of OPA.
2. low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 1, it is characterised in that：One
The weight of individual sodium sulfite-buffer reagent bag is 0.08-0.12g.
3. low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 2, it is characterised in that：One
The weight of individual sodium sulfite-buffer reagent bag is 0.1g.
4. low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 1, it is characterised in that：One
The weight of individual O-phthalic aldehyde reagent bag is 0.03-0.05g.
5. low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 4, it is characterised in that：One
The weight of individual O-phthalic aldehyde reagent bag is 0.04g.
6. a kind of detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent as claimed in claim 1, its
It is characterised by：Comprise the following steps：
(1) 10ml water samples are taken, a sodium sulfite-buffer reagent bag is added in water sample, rocks and is allowed to molten
Solution；
(2) a cosolvent is added, is shaken up；
(3) add an O-phthalic aldehyde reagent bag and rock and be allowed to dissolve；
(4) fluorescence signal is detected on SP-900 Portable water-quality analysis instruments, calculates ammonia nitrogen in sample
Solubility.
7. the detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 6, it is special
Levy and be：The volume of a cosolvent is 1ml in step (2), and the cosolvent is ethylene glycol and ethanol
Mixed solution.
8. the detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 7, it is special
Levy and be：The cosolvent is that ethylene glycol and ethanol are 2 by volume:The solution of 8 ratio mixing.
9. the detection method of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent according to claim 6, it is special
Levy and be：The excitation wavelength of detection fluorescence signal is 300-400nm in step (4), and launch wavelength is
350-450nm。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001196A (en) * | 2018-10-10 | 2018-12-14 | 闫宏涛 | A kind of solid powder detection agent measuring ammonium nitrogen content |
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Cited By (1)
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| CN109001196A (en) * | 2018-10-10 | 2018-12-14 | 闫宏涛 | A kind of solid powder detection agent measuring ammonium nitrogen content |
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Application publication date: 20170825 |