CN106645056A - Method for detecting barium ions in drinking water - Google Patents
Method for detecting barium ions in drinking water Download PDFInfo
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- CN106645056A CN106645056A CN201611008667.1A CN201611008667A CN106645056A CN 106645056 A CN106645056 A CN 106645056A CN 201611008667 A CN201611008667 A CN 201611008667A CN 106645056 A CN106645056 A CN 106645056A
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- drinking water
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- barium
- fluorescence probe
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
Abstract
The invention discloses a method for detecting barium ions in drinking water. A reagent containing a fluorescent probe T serves as a fluorometric reagent, to-be-tested drinking water is added into the fluorometric reagent, the fluorometric reagent is excited through laser with a fixed wavelength, fluorescence emission spectrum intensity change values delta F before and after the fluorometric reagent is added into the to-be-tested drinking water are observed, and the barium ions in the drinking water can be detected. The method has the advantages of being low in analysis cost, simple to operate, sensitive and rapid.
Description
Technical field
The invention belongs to chemical analysis field, and in particular to a kind of detection method of barium in drinking water ion.
Background technology
Barium is a kind of slightly glossiness silvery white alkaline-earth metal, and barium compound species is various, and conventional has barium chloride, carbonic acid
Barium, barium sulfate and barium hydroxide etc..Barium compound is widely used in pigment, steel quenching, ceramics and glass industry.And with barium
The extensive application of compound, is consequently increased in production process to the baric waste water of environmental emission, discarded object, accumulation in the environment
A certain degree of pollution will be caused, threatens the health of the mankind, soluble barium to cause acute poisoning, alimentary canal occur will stimulate disease
Shape, Diagnostic value, uncomfortable in chest, palpitaition etc..200～300mg of oral barium chloride can be poisoned, can causing death during 800～1000mg.State
Standard committee of family and the Ministry of Public Health combine what is issued《Standards for drinking water quality》(GB 5749-2006) to the barium in drinking water from
The content of son has done barium ions in relevant regulations, i.e. drinking water, and, used as unconventional toxicological parameters, its highest permission content is
0.7mg/L。
At present, the analysis method of barium ions mainly adopts absorption/emission spectrum, chromatography of ions, inductively coupled plasma
Atomic emission spectrometry and inductivity coupled plasma mass spectrometry technology etc..These method degrees of accuracy and sensitivity are higher, but need
The instrument of costliness and the detection technique personnel of specialty, it is relatively costly.Fluorescent molecular probe, due to high sensitivity, testing into
This cheap, sample treatment and simple to operate, assay method is quick and enjoys favor the advantages of real-time detection.Therefore, one is designed
The fluorescence detection method for planting simple, sensitive, quick barium in drinking water ion is very necessary.
The content of the invention
It is an object of the present invention to provide a kind of detection method of barium in drinking water ion.The present invention has analysis cost
Relatively low, simple to operate, sensitive and quick the characteristics of.
Technical scheme：A kind of detection method of barium in drinking water ion, is with the reagent containing fluorescence probe T
As fluorometric reagent, and drinking water to be measured is added in fluorometric reagent, then by the LASER Excited Fluorescence reagent of fixed wave length,
And observe fluorescence emission spectrum Strength Changes value Δ F of the fluorometric reagent before and after drinking water to be measured is added, you can in drinking water
Barium ions detected.
The detection method of aforesaid barium in drinking water ion, methods described comprises the steps：
(1) fluorescence probe solution is prepared：Fluorescence probe T is taken, is dissolved with HCl solution, you can obtain the standard of fluorescence probe T
Solution；
(2) measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, to fix excitation wavelength 501nm
Carry out fluorescence emission spectrum measure, and draw the change curve of the fluorescence intensity at the wavelength for inspiring；
(3) spectrofluorimetry：The fluorescence under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Intensity of emission spectra changing value Δ F, you can the barium ions in drinking water is detected.
The detection method of aforesaid barium in drinking water ion, methods described comprises the steps：
(1) fluorescence probe solution is prepared：Accurately weigh the quaternary melon rings of 25.04mg ten (tQ [14]) and 4.80mg thiazole oranges
(TO), dissolve and be settled to 100mL with the HCl/water solution of pH=2, you can obtain the standard liquid of fluorescence probe T；
(2) measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, then with the HCl solution of pH=2
Constant volume is carried out, after placing 10-20 minutes, to fix excitation wavelength 501nm fluorescence emission spectrum measure is carried out, and drafting is inspired
The wavelength at fluorescence intensity change curve；
(3) spectrofluorimetry：The fluorescence under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Intensity of emission spectra changing value Δ F, you can the barium ions in drinking water is detected.
The detection method of aforesaid barium in drinking water ion, the molecular formula of the fluorescence probe T is：C84H84N56O28@
C20H17N2S。
The detection method of aforesaid barium in drinking water ion, the ten quaternarys melon ring is 2 with the mol ratio of thiazole orange:1.
The detection method of aforesaid barium in drinking water ion, the molar concentration of the standard liquid of the fluorescence probe T is 1.0
×10-4mol/L。
The detection method of aforesaid barium in drinking water ion, in the step (3), the method for spectrofluorimetry is as follows：
When the fluorescence emission spectrum Strength Changes Δ F under correspondence 587nm before and after drinking water to be measured is added in fluorescence probe solution is larger,
Then show to contain barium ions in drinking water to be measured, the fluorescence before and after drinking water to be measured is added in fluorometric reagent under corresponding 587nm
When intensity of emission spectra changes delta F is less, then show not containing barium ions in drinking water to be measured.
The detection method of aforesaid barium in drinking water ion, in the step (3), the method for spectrofluorimetry is as follows：
Fluorescence emission spectrum Strength Changes Δ F before and after drinking water to be measured is added in fluorescence probe solution under correspondence 587nm more than ±
When 10%, then show to contain barium ions in drinking water to be measured, before and after drinking water to be measured is added in fluorometric reagent under corresponding 587nm
Fluorescence emission spectrum Strength Changes Δ F be less than ± 10% when, then show in drinking water to be measured do not contain barium ions.
Beneficial effects of the present invention：
1st, the fluorescent molecular probe in the present invention, because with high sensitivity, testing cost is cheap, sample treatment and operation
Simply, assay method is quick, real-time detection the advantages of and enjoy favor.Therefore the design method of the present invention is to Ba in drinking water2+
Fluorescence probe with high sensitivity, high selectivity has stronger scientific research meaning and actual application value.
2nd, the present invention compared with prior art, with obvious beneficial effect, as can be known from the above technical solutions：The present invention is base
Can make the fluorescence of thiazole orange that enhanced sensitivity occur so as to form super molecular complex fluorescence probe T in ten quaternary melon rings, when visiting in fluorescence
Ba is added in pin T2+Afterwards, Ba2+Probe T is destroyed so as to form new compound, fluorescence probe is quenched again, utilize this
The fluorescent switch effect of super molecular compound is planted, so as to a kind of Ba for setting up2+Detection method, the method cost is lower, operation
It is simpler.
3rd, in fluorometric reagent of the invention, the fluorescence probe T of individualism, fixed excitation wavelength 501nm, slit 10nm,
Fluorescence intensity level is strong at fluorescence emission wavelengths 587nm during voltage 650v, Ba2+Unstressed configuration spectral quality, adds in probe T and contains
Ba2+Solution after, solution fluorescence emission spectrum correspondence 587nm at fluorescent emission intensity substantially reduce, it is acid water-soluble with probe T
Interfering material (Li that may be present is added in liquid+, Na+, K+, Mg2+, Ca2+, Hg2+, Co2+, Ni2+, Cu2+, Cd2+, Pb2+, Zn2+,
Al3+, Fe3+, Fe2+) afterwards contrast fluorescent emission intensity experiment show that the fluorescence system has certain selectivity.
4th, Ba provided by the present invention2+Detection method compared with traditional inductance coupled plasma-atomic emission spectrometry and electricity
The detection techniques such as sense coupled plasma mass spectrometry technology are more quick, simple, sensitive.
Further to prove effect of the invention, applicant has done following experiment：
First, impact of the barium ions to the fluorescence signal of fluorometric reagent
Drinking water is taken, with 0.2 μm of water phase membrane filtration, adds a small amount of acid regulation to make the pH=2 of water sample as prepare liquid, inspection
Water sample is surveyed, does not find there is the presence of barium ions in water sample；The volumetric flask for taking 10mL is some, on the basis of this, using standard plus
Enter method and be separately added into the standard liquid containing barium ions, then make the concentration of barium ions in volumetric flask be distributed on 1.5 with pure water constant volume
～4.5 × 10-6In the range of mol/L, the fluorescence probe T solution 2mL of pH=2 are then respectively adding, then with the HCl/water of pH=2
Solution constant volume (volume of water sample >=50%), shakes up, and room temperature is placed after 10-20min, and fixed excitation wavelength 501nm carries out fluorescence and sends out
Spectroscopic assay is penetrated, standard recovery rate is tested according to IUPAC law regulations, then detect and calculate adding for the solution in each bottle
Enter the fluorescence emission spectrum Strength Changes value Δ F under correspondence 587nm before and after fluorometric reagent.
Testing result is as shown in Figure 2：It can be seen that after barium ions is added in fluorescence probe solution, fluorescence
Intensity of emission spectra there occurs and be widely varied that Δ F is larger for changing value, it was demonstrated that fluorescence signal there occurs quenching effect, meanwhile, with
The increase of barium ions concentration, quenching effect is more obvious.
2nd, the impact of barium ions and other metal ions to the fluorescence signal of fluorescence probe solution
Drinking water is taken, with 0.2 μm of water phase membrane filtration, adds a small amount of acid regulation to make the pH=2 of water sample as prepare liquid, inspection
Water sample is surveyed, does not find there is the presence of barium ions in water sample；The volumetric flask for taking 10mL is some, on the basis of this, using standard plus
Enter method and add the standard liquid containing barium ions in one bottle thereto, be then separately added into in other volumetric flasks and comprise only other certain
One metal ion species (Li+, Na+, K+, Mg2+, Ca2+, Hg2+, Co2+, Ni2+, Cu2+, Cd2+, Pb2+, Zn2+, Al3+, Fe3+, Fe2+)
Solution, the concentration of metal ions is consistent with barium ions concentration, is then respectively adding the fluorescence probe T solution 2mL of pH=2,
Then with HCl/water solution constant volume (volume of water sample >=50%) of pH=2, shake up, room temperature is placed after 10-20min, fixed excitation wave
Long 501nm carries out fluorescence emission spectrum measure, and standard recovery rate is tested according to IUPAC law regulations, then draws out fluorescence spectrum
The change curve of intensity, experimental result as shown in figure 3, as can be seen from Figure 3 in the presence of it there are other ions in solution, no
The probe can be affected to Ba2+Detection, be to illustrate that the probe has preferable anti-interference.
3rd, interference--free experiments
(1) preparation of the HCl/water solution of pH=2：
The 6M HCl solutions of 1.33mL are accurately pipetted in the volumetric flask of 1000mL, redistilled water constant volume is used, is configured to
The HCl/water solution of pH=2；
(2) preparation of fluorescence probe T standard liquids：
The quaternary melon rings of 25.04mg ten (tQ [14]) and 4.80mg thiazole oranges (TO) are accurately weighed, the HCl/water with pH=2 is molten
Liquid dissolves and is settled to 100mL.It is 2 that ten quaternary melon rings are obtained with thiazole orange molar concentration rate:1st, molar concentration be 1.0 ×
10-4The fluorescence probe T solution of mol/L；
(3)Ba(ClO4)2·2H2The preparation of O standard liquids：
Accurately weigh 26.14mg Ba (ClO4)2·2H2O, with the HCl/water solution of pH=2 10ml, molar concentration are configured to
For 1.0 × 10-2The Ba of mol/L2+Standard liquid；
(4) preparation of interfering ion solution：
Specpure each metal ion species (perchlorate) standard items are weighed respectively, and respectively with the HCl/water solution of pH=2
Concentration is configured to for 1.00 × 10-2The solution of mol/L；
(5) drafting of calibration curve：
10,10ml volumetric flasks are taken, per bottle adds after the μ L of 1.0 × 10-4mol/L fluorescence probe T solution 400, accurate respectively
Add 0,4.0,8.0,12.0,16.0,20.0,24.0,28.0,32.0,36.0,40.0 μ L, 1.0 × 10-2mol/LBa2+Standard
Solution, with the HCl/water solution of pH=2 scale is settled to, and is shaken up, and room temperature is placed after 10-20min, and fixed excitation wavelength 501nm is entered
Row fluorescence emission spectrum is determined, with Ba2+Concentration be abscissa, with correspondence 587nm under fluorescence emission spectral intensity changing value
Δ F (adds Ba2+Before with addition Ba2+Difference afterwards) draw calibration curve for ordinate；
(6) interfering ion is determined：
In the probe T solution for having configured add pH=2 HCl/water solution, make solution middle probe T concentration be 4.00 ×
10-6mol·L-1, the standard liquid for having configured is added, add and determine after standard liquid probe T to be the fluorescence at 587nm in wavelength
Intensity level.Again respectively to probe T-Ba2+The interfering ion solution for having configured of equivalent is added in mixed solution, then detection is added
The change of fluorescence intensity level in front and back.As shown in Figure 3, test result indicate that probe T detection Ba2+Fluorescence intensity be substantially not subject to
The impact that other ions coexist.
Description of the drawings
Fig. 1 is fluorescence spectrums of the fluorescence probe T in the presence of different metal ions；
Fig. 2 is fluorescence probe T solution fluorescence spectroscopic methodology detections Ba2+Canonical plotting (excitation wavelength is 501nm, slit
10nm, voltage 650v)；
Fig. 3 coexistent metallic ions detect Ba to probe T2+Fluorescence intensity affect.
Specific embodiment
Embodiments of the invention：
Embodiment 1：A kind of detection method of barium in drinking water ion, comprises the steps：
(1) fluorescence probe solution is prepared：Accurately weigh the quaternary melon rings of 25.04mg ten (tQ [14]) and 4.80mg thiazole oranges
(TO), dissolve and be settled to 100mL with the HCl/water solution of pH=2, you can obtain mol ratio for 2:1st, molar concentration be 1.0 ×
10-4(molecular formula is the fluorescence probe T of mol/L：C84H84N56O28@C20H17N2S standard liquid)；
(2) measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, then with the HCl solution of pH=2
Constant volume is carried out, after placing 15 minutes, to fix excitation wavelength 501nm fluorescence emission spectrum measure is carried out, and draw what is inspired
The change curve of the fluorescence intensity at the wavelength；
(3) spectrofluorimetry：The fluorescence under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Intensity of emission spectra changing value Δ F, the fluorescent emission before and after drinking water to be measured is added in fluorescence probe solution under corresponding 587nm
When spectral intensity changes delta F is equal to ± 20%, then show to contain barium ions in drinking water to be measured, it is to be measured when adding in fluorometric reagent
When fluorescence emission spectrum Strength Changes Δ F before and after drinking water under correspondence 587nm is equal to ± 5%, then in showing drinking water to be measured
Without barium ions.
Embodiment 2：A kind of detection method of barium in drinking water ion, comprises the steps：
(1) fluorescence probe solution is prepared：Accurately weigh the quaternary melon rings of 25.04mg ten (tQ [14]) and 4.80mg thiazole oranges
(TO), dissolve and be settled to 100mL with the HCl/water solution of pH=2, you can obtain mol ratio for 2:1st, molar concentration be 1.0 ×
10-4(molecular formula is the fluorescence probe T of mol/L：C84H84N56O28@C20H17N2S standard liquid)；
(2) measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, then with the HCl solution of pH=2
Constant volume is carried out, after placing 10 minutes, to fix excitation wavelength 501nm fluorescence emission spectrum measure is carried out, and draw what is inspired
The change curve of the fluorescence intensity at the wavelength；
(3) spectrofluorimetry：The fluorescence under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Intensity of emission spectra changing value Δ F, the fluorescent emission before and after drinking water to be measured is added in fluorescence probe solution under corresponding 587nm
When spectral intensity changes delta F is equal to ± 10%, then show to contain barium ions in drinking water to be measured, it is to be measured when adding in fluorometric reagent
When fluorescence emission spectrum Strength Changes Δ F before and after drinking water under correspondence 587nm is equal to ± 10%, then in showing drinking water to be measured
Without barium ions.
Embodiment 3：A kind of detection method of barium in drinking water ion, comprises the steps：
(1) fluorescence probe solution is prepared：Accurately weigh the quaternary melon rings of 25.04mg ten (tQ [14]) and 4.80mg thiazole oranges
(TO), dissolve and be settled to 100mL with the HCl/water solution of pH=2, you can obtain mol ratio for 2:1st, molar concentration be 1.0 ×
10-4(molecular formula is the fluorescence probe T of mol/L：C84H84N56O28@C20H17N2S standard liquid)；
(2) measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, then with the HCl solution of pH=2
Constant volume is carried out, after placing 20 minutes, to fix excitation wavelength 501nm fluorescence emission spectrum measure is carried out, and draw what is inspired
The change curve of the fluorescence intensity at the wavelength；
(3) spectrofluorimetry：The fluorescence under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Intensity of emission spectra changing value Δ F, the fluorescent emission before and after drinking water to be measured is added in fluorescence probe solution under corresponding 587nm
When spectral intensity changes delta F is equal to ± 50%, then show to contain barium ions in drinking water to be measured, it is to be measured when adding in fluorometric reagent
When fluorescence emission spectrum Strength Changes Δ F before and after drinking water under correspondence 587nm is equal to 0, then show not contained in drinking water to be measured
Barium ions.
Claims (8)
1. a kind of detection method of barium in drinking water ion, it is characterised in that：It is using the reagent containing fluorescence probe T as fluorescence
Reagent, and drinking water to be measured is added in fluorometric reagent, then by the LASER Excited Fluorescence reagent of fixed wave length, and observe glimmering
Fluorescence emission spectrum Strength Changes value Δ F of the light reagent before and after drinking water to be measured is added, you can to the barium ions in drinking water
Detected.
2. the detection method of barium in drinking water ion according to claim 1, it is characterised in that methods described includes as follows
Step：
（1）Prepare fluorescence probe solution：Fluorescence probe T is taken, is dissolved with HCl solution, you can the standard for obtaining fluorescence probe T is molten
Liquid；
（2）The measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, is carried out with fixing excitation wavelength 501nm
Fluorescence emission spectrum is determined, and draws the change curve of the fluorescence intensity at the wavelength for inspiring；
（3）Spectrofluorimetry：The fluorescent emission under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Spectral intensity changing value Δ F, you can the barium ions in drinking water is detected.
3. the detection method of barium in drinking water ion according to claim 2, it is characterised in that methods described includes as follows
Step：
（1）Prepare fluorescence probe solution：Accurately weigh the quaternary melon rings of 25.04 mg ten (tQ [14]) and 4.80mg thiazole oranges（TO）,
100 mL are dissolved and are settled to the HCl/water solution of pH=2, you can obtain the standard liquid of fluorescence probe T；
（2）The measure of fluorescence spectrum：Drinking water to be measured is added in fluorescence probe solution, is then carried out with the HCl solution of pH=2
Constant volume, after placing 10-20 minutes, to fix excitation wavelength 501nm fluorescence emission spectrum measure is carried out, and draw inspire should
The change curve of the fluorescence intensity at wavelength；
（3）Spectrofluorimetry：The fluorescent emission under correspondence 587nm before and after drinking water to be measured is added in calculating fluorescence probe solution
Spectral intensity changing value Δ F, you can the barium ions in drinking water is detected.
4. the detection method of the barium in drinking water ion according to Claims 2 or 3, it is characterised in that：The fluorescence probe T
Molecular formula be：C84H84N56O28@C20H17N2S。
5. the detection method of barium in drinking water ion according to claim 4, it is characterised in that：The ten quaternarys melon ring with
The mol ratio of thiazole orange is 2:1.
6. the detection method of barium in drinking water ion according to claim 4, it is characterised in that：The fluorescence probe T's
The molar concentration of standard liquid is 1.0 × 10-4mol/L。
7. the detection method of the barium in drinking water ion according to Claims 2 or 3, it is characterised in that the step（3）
In, the method for spectrofluorimetry is as follows：Fluorescence before and after drinking water to be measured is added in fluorescence probe solution under corresponding 587nm
When intensity of emission spectra changes delta F is larger, then show to contain barium ions in drinking water to be measured, when adding drink to be measured in fluorometric reagent
With the fluorescence emission spectrum Strength Changes Δ F under correspondence 587nm before and after water it is less when, then show in drinking water to be measured not baric from
Son.
8. the detection method of barium in drinking water ion according to claim 7, it is characterised in that the step（3）In, it is glimmering
The method of light spectrum analysis is as follows：Fluorescent emission before and after drinking water to be measured is added in fluorescence probe solution under corresponding 587nm
When spectral intensity changes delta F is more than ± 10%, then show to contain barium ions in drinking water to be measured, it is to be measured when adding in fluorometric reagent
When fluorescence emission spectrum Strength Changes Δ F before and after drinking water under correspondence 587nm is less than ± 10%, then in showing drinking water to be measured
Without barium ions.
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| CN109652062B (en) * | 2018-12-25 | 2021-07-13 | 贵州大学 | Fluorescent probe T and preparation and application thereof |
| CN109738412A (en) * | 2019-03-05 | 2019-05-10 | 贵州大学 | A kind of detection method of Aluminium in Drinking Water, iron, chromium, mercury, europium, thulium and ytterbium ion |
| CN114018880A (en) * | 2021-10-22 | 2022-02-08 | 杭州食疗晶元生物科技有限公司 | Method for identifying purified water and natural mineral water based on endogenous active intermediate |
| CN114018880B (en) * | 2021-10-22 | 2024-02-27 | 杭州食疗晶元生物科技有限公司 | Method for identifying purified water and natural mineral water based on endogenous active intermediate |
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