CN108956595A - A kind of reagent of the quick colorimetric detection ammonium root of high stable - Google Patents
A kind of reagent of the quick colorimetric detection ammonium root of high stable Download PDFInfo
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Abstract
The present invention provides a kind of reagents of the quick colorimetric detection ammonium root of high stable, the reagent is to be formulated by thymol blue, tetrabutylammonium hydroxide and solvent for ultrapure water, the phenomenon that it is mainly utilized under alkaline condition, and ammonium root can make blue thymol blue solution be quickly turned to yellow realizes detection.The reagent reaches Glassless discoloration in 1 s after contacting with ammonium root, the ammonium salt residue in ammonium ion and non-standard explosion raw material in detectable environment shows extremely low detection limit (open hole detection limits 10 μM and ultraviolet-visible detection is limited to 51 nM) and high selectivity to ammonium root.Have the characteristics that without complicated organic synthesis, time saving and energy saving, green non-poisonous, easy to operate, color speed is fast, high sensitivity, at low cost.
Description
Technical field
The invention belongs to environment and non-standard explosion raw material detection field, and preservation can not only be stablized by providing one kind,
And the reagent of green non-poisonous colorimetric detection ammonium root.The detection of this reagent limits low, strong interference immunity and the reaction time is short, completely may be used
To realize the purpose of low cost, real-time colorimetric detection ammonium root.
Background technique
With industry and agricultural rapid development, a large amount of nitrogenous compound (such as ammonium root class compound) be discharged into surface and
In underground water (Sensors and Actuators B:Chemical, 2018,256:167-175).In these nitrogenous compounds
In, the ammonium root of dissolution is the very important component of nitrogen cycle process in ecological environment.And excessive ammonium root will lead to algae in water
The fast breeding of plant, and the hyper-proliferative of algae can exhaust the dissolved oxygen in water, to destroy the balance of aquatic organism
(Sensors and Actuators B:Chemical,2004,98:12-17).More seriously, ammonium salt base explosive quilt
It is widely used in attack of terrorism activity.Such as: " Irish Republican Army " is mixed using ammonium nitrate and candy, in Northern Ireland and London system
The a large amount of attack of terrorism (Science and Justice, 2009,49:73-80) is made；Terroristic organization of Spain Etard
(ETA), Colombian Revolutionary Armed Forces (FARC) and Palestinian extremist are widely used ammonium nitrate-petroleum progress terror and attack
Hit movable (Applied Magnetic Resonance, 2012,43:557-566).In addition to this, ammonium perchlorate is since its is excellent
Different combustion characteristics, become the most widely used oxidant in composite fuel (Combustion and Flame, 2018,
192:10-24).Therefore, it is detected for ammonium root, not only for maintaining the ecological balance in environment most important, is even more closed
It is the safety of life and property of the people of the world.Currently, the method that scientific research personnel has been developed for various detection ammonium roots, such as ion
Chromatography (Journal of Chromatography A, 2003,997:191-197；Journal of Chromatography
A, 2003,1003:197-202), capillary electrophoresis technique (Journal of Chromatography A, 2006,1106:61-
66), air-sensitive method (Limnology and Oceanography:Methods, 2009,7:144-156), chemoluminescence method
(Analytica Chimica Acta, 1999,398:33-39) etc..However, there are experimental facilities to hold high for these detection methods
Expensive, to need profession technical operation personnel, the disadvantages of detection takes a long time, anti-interference is poor, seriously limit it in practice
Application.Compared with the above detection method, colorimetric detection method is because having easy to operate, at low cost, selectivity and high sensitivity, inspection
The advantages that range is wide, the response time is short is surveyed, and receives the extensive concern of people.
Currently, most important two kinds of detection methods of colorimetric detection ammonium root are Na's reagent (Journal of
Chemistry, 2013,2013:9) and ammonia-nitrogen (Sensors and Actuators B:Chemical, 2018,256:
167–175).Nessler reagent be 1856 by German chemist Nessler invention (Chemical Center, 1856,27,
Nene Folge 1,529), and the ammonium root detection reagent being widely used always, such as national standard HJ535-2009 " water quality ammonia
The measurement Berthelot spectrophotometry of nitrogen " it is exactly using the ammonium root in nessler reagent detection water.However, since it contains largely
Mercury ion easily causes environmental pollution, and is easy by other ion interferences, such as Cl2、Cl-、Mg2+、Fe2+Plasma all can be to ammonium root
Detection generates serious interference (Journal of the American Chemical Society, 1934,56:769-774),
Seriously limit its application in practice.Although passing through the improvement of scientific research personnel later, effectively shielded by the way that tartaric acid is added
The interference of other metal ions is covered, but its stability difference and the characteristic of severe toxicity still remain.Chemist in 1859
Berthelot have developed than nessler reagent have more highly sensitive reagent, the reagent by phenol and hypochlorite mixing and
At encountering becomes blue (Report, chimie appliquee, 1859,1:284) from colourless after measured ion ammonium root to be checked.This
It is exactly the ammonium root detection reagent being widely adopted at present, is commonly called as ammonia-nitrogen.However since phenol has extremely strong toxicity, reaction
Speed excessively slowly, the unstability of hypochlorite the disadvantages of limit its application.Scientific research personnel passes through effort in more than 100 years,
Phenol is replaced using nontoxic salicylic acid or sodium salicylate, sodium nitroprussiate or Mn is added2+The methods of reaction speed etc. is improved, is had very much
Effect improves its toxicity and reaction speed.However, for its stability problem, Newell (Journal of the Marine
Biological Association of the United Kingdom, 1967,47:271), Stegemann (Hoppe-
Seylers Z.Physiol.Chem., 1969,329:241), Haussler (Wiener Klinische
Wochenschrift, 1960,17:874) etc. scientific research personnel take hypochlorous acid substituted with more stable sodium dichloro cyanurate
Root, King Tong Lau (Sensors and ActuatorsB:Chemical, 2004,98:12-17), Yong Shin
Reagent is made into solid by the seminars such as Kimb (Sensors and Actuators B:Chemical, 2018,256:167-175)
The method of state is to improve its stability.However, regrettably its validity period at most also can only achieve 24 hours.In addition, international
On scientific research personnel's method for also developing a variety of colorimetric detection ammonium roots.Such as the Nagao Kobayashi class of northeastern Japan university
Topic has been combined into out a kind of novel B ODIPY class fluorescent molecule, fully achieves the purpose of naked eye colorimetric detection ammonium root
(Chemical Communications, 2011,47:12092-12094), but this fluorescent molecule synthesis process is complicated, at
This is higher, not can manufacture.
The present invention develops a kind of reagent of colorimetric detection ammonium root, mainly utilizes under alkaline condition, ammonium root can make
The phenomenon that blue thymol blue solution is quickly turned to yellow realizes detection.In addition, not only there is this reagent raw material can pass through quotient
Industry approach is commercially available, prepares easy, cheap advantage, and green non-poisonous, quick, sensitive, highly selective and operation
Simply, very there are the potentiality promoted and applied.
Summary of the invention
Present invention aims at provide a kind of reagent of quick colorimetric detection ammonium root of high stable, which is by thymol
Blue, tetrabutylammonium hydroxide and solvent are formulated for ultrapure water, mainly utilize under alkaline condition, ammonium root can make blue
The phenomenon that thymol blue solution is quickly turned to yellow realizes detection, is developed using the property of thymol blue pH indicator without multiple
The reagent of miscellaneous organic synthesis, time saving and energy saving, green non-poisonous, easy to operate, high sensitivity, colorimetric detection ammonium root at low cost.
Detection reagent of the invention shows extremely low detection limit to ammonium root (open hole detection limits 10 μM and ultraviolet-visible detection is limited to 51nM)
With high selectivity, this guarantees the ammonium root ingredients that can be directed in environment and non-standard explosion raw material to be detected.
In addition, this reagent reaches Glassless discoloration in 1s after contacting with ammonium root, without complicated analytical equipment, to realize ammonium
Inexpensive, the instant detection of root.Overcome existing colorimetric detection ammonium root method strong toxicity, stability difference and probe molecule synthesis
The deficiencies of complicated.
A kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention, which is by chemical reagent thymol
Blue, tetrabutylammonium hydroxide and solvent are formulated for ultrapure water, in which:
The concentration of tetrabutylammonium hydroxide in the solution is 61.6nM-308nM；
The concentration of thymol blue in the solution is 2.14 μM -107 μM；
Tetrabutylammonium hydroxide and thymol blue are dissolved in ultrapure water by molar concentration, stirred evenly, mixing time
The reagent of the quick colorimetric detection ammonium root of high stable is arrived for 10-30min.
The detection reagent of preparation is applied to ammonium by a kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention
The colorimetric detection of root, the specific steps are as follows:
Prepare detection reagent:
(1) 10 times are diluted to get arriving in tetrabutylammonium hydroxide (TBAH) the reagent ultrapure water of water by the 40% of purchase
154 μM tetrabutylammonium hydroxide (TBAH) aqueous solution；
(2) weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution to get thymol blue
Molar concentration is 214 μM；
(3) respectively measure tetrabutylammonium hydroxide (TBAH) amount be 4 μ L, 6 μ L, 8 μ L, 10 μ L, 12 μ L, 14 μ L, 16 μ L,
The amount of 18 μ L and 20 μ L and thymol blue aqueous solution be 100 μ L, 200 μ L, 400 μ L, 600 μ L, 800 μ L, 1mL, 1.2mL,
Then 1.4mL, 1.6mL, 1.8mL, 2mL, 2.5mL, 3mL, 3.5mL, 4mL, 4.5mL and 5mL are settled to ultrapure water mixing
10mL is stirred evenly, and mixing time is 10-30min to get being 61.6nM- to tetrabutylammonium hydroxide (TBAH) molar concentration
308nM, the detection reagent that thymol blue molar concentration is 2.14 μM -107 μM；
The detection reagent of preparation is applied to the colorimetric detection of ammonium root:
(4) NH is weighed4Cl is dissolved in ultrapure water, be configured to ammonium root concentration of standard solution be 1M, 900mM, 800mM,
700mM、600mM、500mM、400mM、300mM、200mM、100mM、90mM、80mM、70mM、60mM、50mM、40mM、30mM、
20mM、10mM、9mM、8mM、7mM、6mM、5mM、4mM、3mM、2mM、1mM、900μM、800μM、700μM、600μM、500μM、
The NH of concentration needed for 400 μM, 300 μM, 200 μM and 100 μM4Cl aqueous solution；
(5) extinction with ultraviolet-visible spectrophotometer test different ratio reagent before and after encountering same concentrations ammonium root
Degree variation, the absorbance after then test agent is reacted with various concentration ammonium root, using the changing value of absorbance as ordinate, ammonium root
Concentration is abscissa, and fitting obtains the linear equation with one unknown of working curve, so that it is determined that the detection of reagent limits, wherein with it is ultraviolet-
The detection reagent volume of visible absorption spectra scanning is 3mL, and addition standard ammonium root aqueous solution volume is 30 μ L；
(6) 1mL step is added in the centrifuge tube of 2mL capacity in the ammonium root aqueous solution for measuring 10 μ L various concentrations with liquid-transfering gun
Suddenly (5) prepared reagent, the open hole detection limit for determining reagent detection ammonium root of taking pictures, naked eye contrast agent encounter various concentration ammonium
The color change of root reaction front and back determines the open hole detection limit of reagent.
(7) it is wiped respectively with sampling paper and takes micro (NH4)3PO4、NH4HCO3、NH4F、NH4Cl、KNO3、KClO3、NaNO3With
NaNO2Afterwards, 1-2 drop detection reagent in drop is observed color change, is determined whether containing ammonium salt.
A kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention, not only can detecte the ammonium in liquid
Root can also detect micro solid ammonium salt residual.In addition, this reagent has excellent choosing for common inorganic salts chaff interferent
Selecting property.
A kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention explodes mainly for environment and non-standard
Ammonium root ingredient in object is detected, solve can not currently be carried out for ammonium root ingredient green non-poisonous, high stable, quickly, can
Depending on change, low cost detection problem.
Compared with prior art, the beneficial effects of the present invention are:
1. a kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention, raw material can pass through commercial market
It is commercially available and green non-poisonous environmental-friendly；
2. a kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention, inspection that can be sensitive, highly selective
Survey ammonium root；
3. a kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention, rapid reaction can be real in 1s
Now ammonium root is identified；
4. a kind of reagent of the quick colorimetric detection ammonium root of high stable of the present invention detects ammonium root, without complicated point
Desorption device, can direct naked eye recognition detection；
5. determinand without being carried out any pre-processing by detection reagent of the invention, easy to operate, popularization is facilitated to answer
With.
Detailed description of the invention
Fig. 1 is that the concentration of thymol blue of the present invention and tetrabutylammonium hydroxide (TBAH) in ultra-pure water solution is respectively
107 μM and 308nM, the uv-visible absorption spectra spectrogram of front and back is reacted with 10mM ammonium root, wherein illustration is camera shooting
Reaction front and back reagent color change photo；
Fig. 2 is that concentration of the thymol blue of the present invention in reagent is fixed as 107 μM, tetrabutylammonium hydroxide (TBAH) it is dense
After degree takes 61.6nM-308nM, the prepared reagent of different tetrabutylammonium hydroxide (TBAH) concentration to react with 10mM ammonium root
Uv-visible absorption spectra spectrogram；
Fig. 3 be using tetrabutylammonium hydroxide (TBAH) reagent additional amount as abscissa, the absorption value at 435nm is vertical
Coordinate, fitting can obtain exponential curve；
Fig. 4 is that the concentration of tetrabutylammonium hydroxide of the present invention (TBAH) in reagent is fixed as 308nM, thymol blue it is dense
Degree is when successively taking 2.14 μM -107 μM, reagent reacted with 1M ammonium root after uv-visible absorption spectra spectrogram.
Fig. 5 be using thymol blue reagent additional amount as abscissa, absorption value 435nm at is ordinate, and fitting can
Obtain linearity curve；
Fig. 6 is that the concentration of thymol blue of the present invention and tetrabutylammonium hydroxide (TBAH) in ultra-pure water solution is respectively
107 μM and 308nM, gained uv-visible absorption spectra spectrogram after being reacted with the ammonium root of 1 μM of -9mM；
Fig. 7 is that the absorption value using ammonium root concentration as abscissa, at 435nm is ordinate, and fitting can obtain exponential curve；
Fig. 8 is with ammonium root concentration (3 μM -10 μM) for abscissa, and the absorption value at 435nm is ordinate, and fitting can obtain line
Linearity curve；
Fig. 9 is that the concentration of thymol blue of the present invention and tetrabutylammonium hydroxide (TBAH) in ultra-pure water solution is respectively
107 μM and 308nM, gained camera shoots picture after reacting with the ammonium root of 1 μM of -9mM.
Specific embodiment
Below by specific embodiment, the present invention is described further, but the present invention is not limited to these embodiments.
Embodiment 1
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, uses liquid-transfering gun
The 0.1g/L thymol blue aqueous solution of 5mL is measured, the 40% of 10 times of the ultrapure water dilution of 20 μ L is in the tetrabutylammonium hydroxide of water
(TBAH) aqueous solution is stirred with 5mL ultrapure water to being uniformly mixed, and mixing time 10min obtains thymol blue and tetrabutylammonium hydrogen
Amine-oxides (TBAH) in aqueous solution concentration be respectively 107 μM He 308nM blue detection reagent；
Configured detection reagent measurement 3mL is placed in quartz colorimetric utensil, the 1M ammonium root titer prepared is added
30 μ L carry out uv-visible absorption spectra scanning with ultraviolet-visible spectrophotometer, and spectrogram such as Fig. 1 institute of front and back is added in ammonium root
Show, spectrogram can be seen that the absorption peak being located at 595nm after reaction and drastically reduce before and after being reacted by comparison, and go out at 435nm
Show apparent absorption peak, has directly been taken pictures (as shown in Fig. 1 illustration) to the reagent of reaction front and back, comparison reaction front and back reagent
Reagent from navy blue has become glassy yellow after photo can be seen that reaction, illustrates to have detected ammonium root.
Embodiment 2
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 9 glass
Glass bottle is separately added into the 0.1g/L thymol blue aqueous solution and 5mL ultrapure water of 5mL with liquid-transfering gun, then measures 4 μ L, 6 μ respectively
L, 8 μ L, 10 μ L, 12 μ L, 14 μ L, 16 μ L, 18 μ L and 20 μ L have diluted the 40% of 10 times in the TBAH aqueous solution of water, are added 9
In vial, stirring is to being uniformly mixed, and mixing time 20min, obtaining thymol blue molar concentration is 107 μM and tetrabutylammonium hydrogen
Amine-oxides (TBAH) molar concentration be 61.6nM, 92.4nM, 123.2nM, 154nM, 184.8nM, 215.6nM, 246.4nM,
The blue detection reagent of 277.2nM and 308nM；
Configured detection reagent measurement 3mL is placed in quartz colorimetric utensil, the 1M ammonium root standard water prepared is added
30 μ L of solution carries out uv-visible absorption spectra scanning, different tetrabutylammonium hydroxide with ultraviolet-visible spectrophotometer
(TBAH) the spectrogram result after the reagent detection same concentrations ammonium root of concentration is as shown in Fig. 2, as can be seen from the figure: with the tetrabutyl
The increase of ammonium hydroxide (TBAH) concentration, the absorption value after reaction at 435nm gradually increase, and more obvious can be found out by Fig. 3:
With the increase of tetrabutylammonium hydroxide (TBAH) additional amount, the absorption peak strength at 435nm is in exponential increase.
Embodiment 3
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 17
10mL volumetric flask, with liquid-transfering gun be added with ultrapure water dilute 10 times 40% in water tetrabutylammonium hydroxide (TBAH) it is water-soluble
20 μ L of liquid, then measure respectively 100 μ L, 200 μ L, 400 μ L, 600 μ L, 800 μ L, 1mL, 1.2mL, 1.4mL, 1.6mL, 1.8mL,
The 0.1g/L thymol blue aqueous solution of 2mL, 2.5mL, 3mL, 3.5mL, 4mL, 4.5mL and 5mL is added in 17 volumetric flasks, with super
Pure water constant volume shakes up, and the time is 30min to get being 308nM and thymol blue to tetrabutylammonium hydroxide (TBAH) molar concentration
Molar concentration is 2.14 μM, 4.28 μM, 8.56 μM, 12.84 μM, 17.12 μM, 21.4 μM, 25.68 μM, 29.596 μM, 38.52 μ
M, 42.8 μM, 53.5 μM, 64.2 μM, 74.9 μM, 85.6 μM, 96.3 μM and 107 μM of blue detection reagent；
Configured detection reagent measurement 3mL is placed in quartz colorimetric utensil, the 1M ammonium root standard water prepared is added
30 μ L of solution carries out uv-visible absorption spectra scanning, the examination of different thymol blue concentration with ultraviolet-visible spectrophotometer
Agent detects the spectrogram result after same concentrations ammonium root as shown in figure 4, as can be seen from the figure: with the increase of thymol blue concentration,
It is located at the absorption value at 435nm after reaction to gradually increase, more obvious can be found out by Fig. 5: with the increasing of thymol blue additional amount
Add, the increase in a linear relationship of the absorption peak strength at 435nm.
Embodiment 4
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 400 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 100mL is titrated to 200mL with ultrapure water mixing, it is dense to obtain thymol blue mole by mixing time 15min
The detection reagent that degree is 107 μM and tetrabutylammonium hydroxide (TBAH) molar concentration is 308nM；
Configured detection reagent measurement 3mL is placed in quartz colorimetric utensil, the various concentration ammonium root prepared is added
30 μ L of standard aqueous solution, the surveyed absorption spectrum of ultraviolet-visible spectrophotometer after different ammonium root concentration are added as shown in fig. 6,
As can be seen from the figure: as the absorption peak strength that the raising of ammonium root concentration is located at 435nm is gradually increased, and by the quasi- of Fig. 7
Closing curve more obvious can find out: with the raising of ammonium root concentration, absorption peak strength at 435nm with ammonium root concentration increasing
Add and have exponent relation increase, when ammonium root concentration is 3 μM -10 μM, the absorption peak strength at 435nm is with ammonium root concentration
Increase and increase (as shown in Figure 8) in good linear relationship, linear equation can obtain y=6.02174 × 10-4x+
0.00938, limit calculation equation according to detection: detection limit=3 σ/K, wherein σ is used ultraviolet-visible spectrophotometer
Standard deviation, the present invention used in ultraviolet-visible spectrophotometer standard deviation=1.59463 × 10-4(n=15), K is quasi-
Close slope of a curve, i.e. K=6.02174 × 10-4, the detection for being computed this reagent is limited to 51nM.
Embodiment 5
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 400 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 100mL is titrated to 200mL with ultrapure water mixing, it is dense to obtain thymol blue mole by mixing time 25min
The detection reagent that degree is 107 μM and tetrabutylammonium hydroxide (TBAH) molar concentration is 308nM；
Configured detection reagent measurement 1mL is placed in the centrifuge tube that capacity is 2mL, it is dense to add the difference prepared
10 μ L of ammonium root standard aqueous solution is spent, the photo after the reaction of various concentration ammonium root is shot in light box is as shown in figure 9, from figure
It can be seen that prepared reagent is limited to 10 μM for the naked eye recognition detection of ammonium root.
Embodiment 6
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 400 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 2mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 308nM for 2.14 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro (NH is wiped with sampling paper4)3PO4After solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center,
This it appears that: sampling paper center quickly can become glassy yellow from dark blue blue, it was demonstrated that quick-fried containing non-standard in object to be checked
Fried raw material ammonium salt.
Embodiment 7
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 80 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol blue with liquid-transfering gun
Then aqueous solution 100mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 61.6nM for 107 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro NH is wiped with sampling paper4HCO3After solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, it can
Will become apparent from: sampling paper center quickly can become glassy yellow from dark blue blue, it was demonstrated that explode in object to be checked containing non-standard
Raw material ammonium salt.
Embodiment 8
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 400 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 50mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 308nM for 53.5 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro NH is wiped with sampling paper4After F solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, it can be with
Will become apparent from: sampling paper center quickly can become glassy yellow from dark blue blue, it was demonstrated that contain non-standard explosive in object to be checked
Raw material ammonium salt.
Embodiment 9
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 200 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 100mL is titrated to 200mL with ultrapure water mixing, it is dense to obtain thymol blue mole by mixing time 15min
The detection reagent that degree is 107 μM and tetrabutylammonium hydroxide (TBAH) molar concentration is 154nM；
Micro NH is wiped with sampling paper4After Cl solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, it can
Will become apparent from: sampling paper center quickly can become glassy yellow from dark blue blue, it was demonstrated that explode in object to be checked containing non-standard
Raw material ammonium salt.
Embodiment 10
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 400 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 5mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 308nM for 5.35 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro KNO is wiped with sampling paper3After solid residue, 1-2 drop detection reagent, sampling is added dropwise at sampling paper center
Paper does not have any color change, it was demonstrated that without containing non-standard explosion raw material ammonium salt in object to be checked.
Embodiment 11
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 20 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol blue with liquid-transfering gun
Then aqueous solution 100mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 15.4nM for 107 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro KClO is wiped with sampling paper3After solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, adopts
Sample paper does not have any color change, it was demonstrated that without containing non-standard explosion raw material ammonium salt in object to be checked.
Embodiment 12
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 40 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol blue with liquid-transfering gun
Then aqueous solution 10mL is titrated to 200mL, mixing time 15min with ultrapure water mixing, obtaining thymol blue molar concentration is
10.7 μM are the detection reagent of 30.8nM with tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro NaNO is wiped with sampling paper3After solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, adopts
Sample paper does not have any color change, it was demonstrated that without containing non-standard explosion raw material ammonium salt in object to be checked.
Embodiment 13
At room temperature, weighing 100mg thymol blue, which is dissolved in 1L ultrapure water, obtains 0.1g/L thymol blue aqueous solution, takes 200mL
Volumetric flask is added 40% in the 100 μ L of tetrabutylammonium hydroxide (TBAH) aqueous solution of water and prepared thymol with liquid-transfering gun
Then blue aqueous solution 25mL is titrated to 200mL with ultrapure water mixing, mixing time 15min obtains thymol blue molar concentration
The detection reagent for being 77nM for 21.75 μM and tetrabutylammonium hydroxide (TBAH) molar concentration；
Micro NaNO is wiped with sampling paper2After solid residue, 1-2 drop detection reagent is added dropwise at sampling paper center, adopts
Sample paper does not have any color change, it was demonstrated that without containing non-standard explosion raw material ammonium salt in object to be checked.
Although above embodiments describe the present invention, it should be appreciated that in the premise without prejudice to spirit of the invention
Under, ammonium root detection of this reagent in other fields is equally applicable.Reagent component ratio in the present invention can be transferred, and this
A little change also belongs to the scope of the present invention.
Claims (1)
1. a kind of reagent of the quick colorimetric detection ammonium root of high stable, it is characterised in that the reagent be by chemical reagent thymol blue,
Tetrabutylammonium hydroxide and solvent are formulated for ultrapure water, in which:
The concentration of tetrabutylammonium hydroxide in the solution is 61.6 nM-308 nM；
The concentration of thymol blue in the solution is 2.14 μM -107 μM；
Tetrabutylammonium hydroxide and thymol blue are dissolved in ultrapure water by molar concentration, stirred evenly, mixing time 10-
30 min are to get the reagent for arriving the quick colorimetric detection ammonium root of high stable.
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