CN103743737B - A method of F- is detected based on aluminum-eriochrome cyanine R color development systems - Google Patents
A method of F- is detected based on aluminum-eriochrome cyanine R color development systems Download PDFInfo
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Abstract
The invention discloses one kind detecting F based on aluminium chromium cyanines R color development systems‑Method, this method includes the research of color development system and each anion chromogenic reaction, color development system and the influence of influence, measuring temperature to chromogenic reaction of each anion absorption spectrum, minute to chromogenic reaction, measures influence of the acid-base value to chromogenic reaction, draws standard curve, carries out recovery test to known aggregate sample.The present invention utilizes aluminium chromium cyanines R color development systems, reduces interference；Measurement for inorganic soluble content of fluoride ion in industrial wastewater is simple and efficient to handle, can identify that color change determines whether fluorine ion is exceeded by bore hole；Content of fluoride ion is 1 × 10‑4~3 × 10‑ 4It is in a linear relationship within the scope of mol/L, quantitative analysis can be carried out, stability is good, and accuracy is high；The present invention is pollution-free, is conducive to environmental protection.
Description
Technical field
The invention belongs to field of chemical detection, more particularly to one kind being based on aluminum-eriochrome cyanine R color development systems bore hole in aqueous solution
Identification and detection F-Method.
Background technology
Fluorine is one of the essential trace elements of the human body, it is distributed widely in soil, water and animals and plants in the form of fluorine ion
In body.Suitable fluorine is to promoting the growth of tooth and bone to play an important roll, but excessive intake fluorine, can generate danger to human body
Evil causes the fluorine such as " glaze dental plaque " or bone calcium metabolism disorder calm.Therefore to F-Detection not only human life science study
There is critical role in field, is also hot spot of people's attention in Environmental Chemistry and medicine etc..However develop at present a variety of
F-Its identification process of ion transducer is carried out in organic phase or half water phase mostly, this significantly limits it to F-Ion is known
The application range that do not study.
Invention content
The invention discloses one kind detecting F based on aluminum-eriochrome cyanine R color development systems-Method, it is intended to solve to have developed at present
A variety of its identification process of F- ion transducers are carried out in organic phase or half water phase mostly, significantly limit it to F-Ion
The problem of application range of Study of recognition.
The invention is realized in this way a kind of detecting F based on aluminum-eriochrome cyanine R color development systems-Method, it is described based on aluminium-
Chromium cyanines R color development systems detect F-Method include the following steps：
Step 1: the research of color development system and each anion chromogenic reaction, pipettes pre-prepared chromophoric solution, respectively
KF, Na is added2CO3、NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr aqueous solution, solution colour by blue become
For aubergine, then main body is KF；
Step 2: color development system and each anion absorption spectrum, a series of colour developings are prepared with the identical method of same step 1
The aqueous solution of system and different anions so that the concentration of various anion sodium salts is 2 × 10-3MolL-1, in room temperature item
It is scanned absorption spectrum in 200 to 800 nanometer ranges with Cary50 types ultraviolet-uisible spectrophotometer under part, is ginseng with water
Than；
Step 3: influence of the minute to chromogenic reaction, to former color development system solution and contains F-The color development system of ion
Absorbance is measured in different time sections, the influence with search time to chromogenic reaction, the time interval in different time periods
It is 1 hour, 2 hours, 5 hours, 8 hours；
Step 4: influence of the measuring temperature to chromogenic reaction, former color development system solution in step 3 and contain F-Ion
Color development system after standing 50 minutes, respectively at developing the color ten minutes at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, measures absorbance；
Step 5: measuring influence of the acid-base value to chromogenic reaction, inspection is investigated by the way that different amounts of NaOH or HCl solution is added
Color developing effect of the survey system under different pH conditions；
Step 6: being 1 × 10 to fluorinion concentration-4mol/L、1.5×10-4mol/L、2.0×10-4mol/L、2.5×
10-4mol/L、 3×10-4mol/L、4×10-4The standard solution of mol/L carries out chromogenic assay, draws standard curve；
Step 7: carrying out recovery test to known aggregate sample.
Further, the research of the color development system and each anion chromogenic reaction is as follows：It pipettes in advance
The Al standard solution 30ml of prepared 5.4ug/ml, 2 × 10-4The bromine of chromium cyanines R solution 20ml, 0.1000mol/L of mol/L
It is mixed to change six methylene, the four ammonium buffer solution 20ml that dodecyl trimethylamine solution 20ml, 0.5000mol/L and PH are 5~7
Conjunction is configured to chromophoric solution；4ml developing solutions are pipetted respectively in a series of 10ml colorimetric cylinders, then are separately added into 2ml solution concentrations
It is KF, Na of 0.0100mol/L2CO3、NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr aqueous solution, and
10ml scales are settled to distilled water, are shaken up, stand 50 minutes, color of observation color development system in the presence of different anions
Variation.
Further, the specific method is as follows for influence of the measurement acid-base value to chromogenic reaction：
As PH ＜ 4.5, all solution colours become pink, no identification, and as pH ＞ 7, all anion are molten
Liquid begins to change into faint yellow, and only as 5 ＜ pH ＜ 7, blue is presented in developing solution and other anion solutions, and fluorine ion is added
Pink is presented in solution, achievees the purpose that Selective recognition, so selecting 5.5≤pH≤6.5 for optimum detection environment.
Further, influence of the measuring temperature to chromogenic reaction, when temperature is in 10 DEG C and 20 DEG C, absorbance is maximum,
When temperature is higher than 30 DEG C, absorbance starts to be substantially reduced.
Effect summarizes
The present invention passes through the research of color development system and each anion chromogenic reaction, color development system and each anion absorption light
Spectrum, influence, measuring temperature influence to chromogenic reaction of the minute to chromogenic reaction measure shadow of the acid-base value to chromogenic reaction
Ring, draw standard curve and to known aggregate sample carry out recovery test researches show that aluminum-eriochrome cyanine R color development systems in water phase
To F-The color developing effect of selectivity and bore hole identification with height, can be applied to following two aspect：The detection of water quality, Al marks
Quasi- solution (5.4ug/ml) 30ml, chromium cyanines R solution (2 × 10-4mol/L) 20ml, bromination dodecyl trimethylamine solution
(0.1000mol/L) 20ml, six times four ammonium buffer solution of methylene (0.5000mol/L, PH are 5~7) 20ml is hybridly prepared into
Chromophoric solution；It takes the developing solution 1.5mL prepared in 10mL colorimetric cylinders, adds 8mL water samples to be measured, constant volume is observed after ten minutes
Solution colour changes in colorimetric cylinder, and solution colour becomes aubergine by blue, illustrates F in water body to be measured-Content is exceeded (to be more than
10mg/L)；If/solution colour illustrates F in water body to be measured without significant change-Content is not exceeded.F in water-Assay：Yu Yi
According to developing solution 3.6ml in serial 10ml colorimetric cylinders, prepare liquid 1.6ml is then with water constant volume, to a series of standard of fluorine ions
Solution carries out chromogenic assay, the results showed that, content of fluoride ion is 1 × 10-4~3 × 10-4It is in a linear relationship within the scope of mol/L, it returns
Yield is good, can be used for F in water sample and toothpaste-Assay.
The present invention's detects F based on aluminum-eriochrome cyanine R color development systems-Method have the beneficial effect that：
(1) selectivity is good, and using aluminum-eriochrome cyanine R color development systems, Common Anions will not be with Al3+Coordination, experiment interference compared with
It is small.
(2) present invention is simple and efficient to handle for the measurement of inorganic soluble content of fluoride ion in industrial wastewater, can pass through
Bore hole identification color change determines whether fluorine ion is exceeded.
(3) content of fluoride ion of the invention is 1 × 10-4~3 × 10-4It is in a linear relationship within the scope of mol/L, it can be determined
Amount analysis, stability is good, and accuracy is high.
(4) pollution-free, be conducive to environmental protection.
Description of the drawings
Fig. 1 is provided in an embodiment of the present invention based on aluminum-eriochrome cyanine R color development systems detection F-Method flow chart.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Fig. 1 shows that the present invention's detects F based on aluminum-eriochrome cyanine R color development systems-Method flow, this as shown in the figure hair
It is bright to be achieved in that a kind of aluminum-eriochrome cyanine R color development systems that are based on detect F-The laboratory apparatus that uses of method include：Ultraviolet-can
See absorption spectrometer (Cary50), 1cm quartz colorimetric utensils；
Experiment reagent includes：Domain is thought in the Al standard solution for the 1000 μ g/mL that State Standard Matter Research Centre provides, Shanghai
The chromium cyanines R (ECR) that Chemical Industry Science Co., Ltd provides, six methines, four ammonium that Tianjin Deng Feng Chemical Companies provide,
The bromination dodecyl trimethyl ammonium (DTAB) that fine chemistry industry research institute provides is recovered in Tianjin, and anion used is that analysis is pure
Corresponding sodium salt, solvent is homemade distilled water.
One kind detecting F based on aluminum-eriochrome cyanine R color development systems-Method include the following steps：
S101：The research of color development system and each anion chromogenic reaction, pipettes pre-prepared chromophoric solution, adds respectively
Enter KF, Na2CO3、 NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr aqueous solution, solution colour becomes from blue
Aubergine, then main body is KF；
S102：Color development system and each anion absorption spectrum prepare a series of developing bodies with the identical method of same step 1
The aqueous solution of system and different anions so that the concentration of various anion sodium salts is 2 × 10-3mo1·L-1, in room temperature condition
It is lower to be scanned absorption spectrum in 200 to 800 nanometer ranges with Cary50 types ultraviolet-uisible spectrophotometer, it is ginseng with water
Than；
S103：Influence of the minute to chromogenic reaction to former color development system solution and contains F-The color development system of ion exists
Absorbance, the influence with search time to chromogenic reaction are measured in different time sections, the different time sections time interval is 1 small
When, 2 hours, 5 hours, 8 hours；
S104：Influence of the measuring temperature to chromogenic reaction, former color development system solution in step 3 and contains F-Ion is shown
Color system after standing 50 minutes, respectively at developing the color ten minutes at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, measures absorbance；
S105：Influence of the acid-base value to chromogenic reaction is measured, detection is investigated by the way that different amounts of NaOH or HCl solution is added
Color developing effect of the system under different pH conditions；
S106：It is 1 × 10 to fluorinion concentration-4mol/L、1.5×10-4mol/L、2.0×10-4mol/L、2.5×10- 4mol/L、3×10-4mol/L、4×10-4The standard solution of mol/L carries out chromogenic assay, draws standard curve；
S107：Recovery test is carried out to known aggregate sample.
Further, the research of color development system and each anion chromogenic reaction is as follows in the S101：It moves
Take pre-prepared 5.4ug/ml Al standard solution 30ml, 2 × 10-4Chromium cyanines R solution 20ml, 0.1000mol/L of mol/L
Bromination dodecyl trimethylamine solution 20ml, 0.5000mol/L and PH be 5~7 six methylene, four ammonium buffer solution
20ml is hybridly prepared into chromophoric solution；4ml developing solutions are pipetted respectively in a series of 10ml colorimetric cylinders, then to be separately added into 2ml molten
Liquid concentration is KF, Na of 0.0100mol/L2CO3、NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr it is water-soluble
Liquid is used in combination distilled water to be settled to 10ml scales, shakes up, and stands 50 minutes, and observation color development system is in the presence of different anions
Color change；
Further, influence of the acid-base value to chromogenic reaction is measured in S105, and the specific method is as follows：
As PH ＜ 4.5, all solution colours become pink, no identification.And as pH ＞ 7, all anion are molten
Liquid begin to change into it is faint yellow, also without identification.Only as 5 ＜ pH ＜ 7, blue is presented in developing solution and other anion solutions, adds
Pink is presented in the solution for entering fluorine ion, achievees the purpose that Selective recognition.So selecting H≤6.5 5.5≤p for optimum detection
Environment.
Further, influence of the measuring temperature of S104 to chromogenic reaction, when temperature is at 10 DEG C~20 DEG C, absorbance is maximum,
When temperature is higher than 30 DEG C, absorbance is substantially reduced.Select temperature condition for room temperature (20 DEG C).
In the presence of alkyl front three amine cation surfactant, when PH is in 5.5~6.5 ranges, to developing body
The CO of equivalent is added in system3 2-, Cl-, Ac-, SO4 2-, SO3 2-, NO3 -, NO2 -, Br-Aqueous solution when, developing solution color and absorb light
Spectrum has no significant change, illustrates that the color development system does not have obvious effect to these types of anion, under room temperature aluminium and chromium cyanines R shapes
At stable blue complex, after fluorine ion is added, due to competitive substitution, fluorine ion and Al3+In conjunction with the colourless of formation stabilization
Complex, solution colour are become the red of chromium cyanines R itself from blue, and conspicuousness variation also occurs for ultra-violet absorption spectrum, to real
Now to the identification and detection of fluorine ion in aqueous solution.
Due to aluminum-eriochrome cyanine R color development systems in water phase to F-The colour developing effect of selectivity and bore hole identification with height
Fruit, therefore the system can be applied to following two aspect：The detection of water quality, Al standard solution (5.4ug/ml) 30ml, chromium cyanines R solution
(2 × 10-4mol/L) 20ml, bromination dodecyl trimethylamine solution (0.1000mol/L) 20ml, six four ammonium of methylene bufferings
Solution (0.5000mol/L, pH are 5~7) 20ml is hybridly prepared into chromophoric solution.Take the developing solution 1.5mL prepared in 10mL ratios
Colour tube adds 8mL water samples to be measured, and constant volume is observed solution colour in colorimetric cylinder and changed after ten minutes, and solution colour is by blue
Become aubergine, illustrates F in water body to be measured-Content is exceeded (being more than 10mg/L).If/solution colour illustrates without significant change
F in water body to be measured-Content is not exceeded.F in water-Assay：According to developing solution 3.6ml in a series of 10ml colorimetric cylinders, wait for
Liquid 1.6ml is surveyed then with water constant volume, chromogenic assay is carried out to a series of standard solution of fluorine ions, the results showed that, fluorine ion contains
Amount is 1 × 10-4~3 × 10-4In a linear relationship within the scope of mol/L, the rate of recovery is good, can be used for F in water sample and toothpaste-Containing measurement
It is fixed.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not
It needs to pay the various modifications or changes that performing creative labour can be made and still fall within the protection scope of the present invention.
Claims (3)
1. one kind detecting F based on aluminum-eriochrome cyanine R color development systems-Method, which is characterized in that it is described based on aluminum-eriochrome cyanine R developing bodies
System detection F-Method include the following steps：
Step 1: the research of color development system and each anion chromogenic reaction, pipettes pre-prepared chromophoric solution, is separately added into
KF、Na2CO3、NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr aqueous solution, solution colour becomes purple from blue
Red, then main body is KF；
Step 2: color development system and each anion absorption spectrum, a series of color development systems are prepared with the identical method of same step 1
With the aqueous solution of different anions so that the concentration of various anion sodium salts is 2 × 10-3mol·L-1, under room temperature
It is scanned absorption spectrum in 200 to 800 nanometer ranges with Cary50 types ultraviolet-uisible spectrophotometer, using water as reference；
Step 3: influence of the minute to chromogenic reaction, to former color development system solution and contains F-The color development system of ion is in difference
Absorbance, the influence with search time to chromogenic reaction are measured in period, the time interval in different time periods is 1 small
When, 2 hours, 5 hours, 8 hours；
Step 4: influence of the measuring temperature to chromogenic reaction, former color development system solution in step 3 and contain F-The developing body of ion
System after standing 50 minutes, respectively at developing the color ten minutes at 10 DEG C, 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, measures absorbance；
Step 5: measuring influence of the acid-base value to chromogenic reaction, detection body is investigated by the way that different amounts of NaOH or HCl solution is added
Tie up to the color developing effect under different pH conditions；
Step 6: being 1 × 10 to fluorinion concentration-4mol/L、1.5×10-4mol/L、2.0×10-4mol/L、2.5×10- 4mol/L、3×10-4mol/L、4×10-4The standard solution of mol/L carries out chromogenic assay, draws standard curve；
Step 7: carrying out recovery test to known aggregate sample；
The research of the color development system and each anion chromogenic reaction is as follows：It pipettes pre-prepared
The Al standard solution 30ml of 5.4ug/ml, 2 × 10-4The bromination dodecyl of chromium cyanines R solution 20ml, 0.1000mol/L of mol/L
Six methylene, the four ammonium buffer solution 20ml that trimethylamine solution 20ml, 0.5000mol/L and pH are 5~7 is hybridly prepared into aobvious
Color solution；4ml developing solutions are pipetted respectively in a series of 10ml colorimetric cylinders, then are separately added into 2ml solution concentrations and are
KF, Na of 0.0100mol/L2CO3、NaAc、Na2SO4、Na2SO3、NaNO3、NaNO2, NaCl, NaBr aqueous solution, distillation is used in combination
Water is settled to 10ml scales, shakes up, and stands 50 minutes, color change of observation color development system in the presence of different anions.
2. detecting F based on aluminum-eriochrome cyanine R color development systems as described in claim 1-Method, which is characterized in that the measurement
The specific method is as follows for influence of the acid-base value to chromogenic reaction：
As pH ＜ 4.5, all solution colours become pink, no identification, and as pH ＞ 7, all anion solutions are opened
Beginning becomes faint yellow, and only as 5 ＜ pH ＜ 7, blue is presented in developing solution and other anion solutions, and the solution of fluorine ion is added
Pink is presented, achievees the purpose that Selective recognition, so selecting 5.5≤pH≤6.5 for optimum detection environment.
3. detecting F based on aluminum-eriochrome cyanine R color development systems as described in claim 1-Method, which is characterized in that the measurement
Influence of the temperature to chromogenic reaction, when temperature is in 10 DEG C and 20 DEG C, absorbance is maximum, and when temperature is higher than 30 DEG C, absorbance is opened
Beginning is substantially reduced.
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| CN105758829B (en) * | 2015-11-20 | 2018-07-17 | 河南理工大学 | The preparation method of the nanocomposite of fluorine ion in a kind of quick detection water phase |
| CN114088693A (en) * | 2021-11-16 | 2022-02-25 | 益诺思生物技术南通有限公司 | Simulated radioactivity18F-labeled cold labeling method and kit |
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