CN109632783A - The new opplication of indoles chloride - Google Patents
The new opplication of indoles chloride Download PDFInfo
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- CN109632783A CN109632783A CN201910029888.4A CN201910029888A CN109632783A CN 109632783 A CN109632783 A CN 109632783A CN 201910029888 A CN201910029888 A CN 201910029888A CN 109632783 A CN109632783 A CN 109632783A
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses indoles chloride, i.e. 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3- trimethyl -3H- indoles chlorides survey the new opplication in platinum in spectrophotometry.When the compound is applied to spectrophotometry survey platinum as organic complexing agent, the preparation of solution is mainly comprised the steps that, draw standard curve, sample measurement.Wherein sample measurement includes: Specimen eliminating, complex reaction, liquid-liquid extraction, absorbance measurement.Measuring method provided by the invention can avoid saturated absorption area and the platinum ion absorption band of near ultraviolet, and rapidly, complexing product is stablized for colour developing, it is anti-interference strong, there is good selectivity to platinum, it is safe and harmless, it is environmental-friendly, it can be used for environmental water sample, model water sample, the separation and concentration of glass Trace Amounts of Platinum and detection.
Description
Technical field
The invention belongs to the new applications of known compound, more specifically to 2- [2- [4- [(2- cyano ethyl)-first
Base-amino]-phenyl]-vinyl] the application of -1,3,3- trimethyl -3H- indoles chloride in spectrophotometry survey platinum.
Background technique
The application of platinum mainly also has more application in environment and biological field, jewelry and nm regime.In addition, platinum is in light
It learns in material industry and also plays huge effect, because it is the basic melting container of optical glass.It is melted in platinum crucible
Phosphate laser glass can make glass have high optical quality and uniformity, and platinum is with platinum ion and platinum grain field trash
Form enter in glass become impurity.With the improvement of technique, platinum is controlled as the content of impurity in ppm magnitude, but
It is still to be able to greatly influence the lasing efficiency of glass and the consistency of performance.It is big to advise with the development of high field laser physics
The construction of mode laser part needs higher performance and the consistent laser glass of performance height, it is therefore desirable to carry out strictly to impurity
Control and monitoring.Their influences to laser glass performance of quantitative analysis are conducive to the detection of platinum ion.Except phosphate laser
Outside glass, the civilian glass of platinum equipment is touched in the melting process such as fluorphosphate glass, germanate glass, tellurate glass
Platinum impurity is all introduced to a certain extent.At this stage, complicated composition and the low platinum content of glass sample are the masters that platinum detects
Want problem.The measuring method of platinum content has in the prior art: spectrophotometry, atomic absorption method, atomic fluorescence method, atomic emissions
Spectroscopic methodology and mass spectrography etc..Since instrument and equipment is simple and easy to get, analysis cost is low, spectrophotometry is most common method.
Common complexing agent is stannous chloride and thiosemicarbazide compound in spectrophotometry at present, but these methods are all
Have a respective drawback: solution acidic is too strong, severe reaction conditions, complicated for operation, toxic solvent endanger environment etc..From cyanine dyes
Since being found, the hot spot that scholars pay close attention to just has been become with its unique advantage.Itself have molar extinction coefficient big, maximum
The advantages such as absorption and launch wavelength are long, light-wave energy is low, and its is maximum the disadvantage is that unstable under illumination.Recently as new-type
The appearance of cyanine dyes and its derivative molecular, application has been extended to biology, medicine and energy field, such as solar battery, light
Photodynamic therapy (PDT), DNA sequencing, pH probe etc.；At the same time, also there is comparable application in traditional chemical analysis field.
It is larger steady with light in the research of element determination, being all difficult to take into account maximum absorption wavelength as complexing agent using cyanine dyes at present
Qualitative two conditions, thus it is how restricted in this application.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the complexing agent used when surveying platinum for spectrophotometry is mentioned
It can guarantee that maximum absorption wavelength is larger under the premise of good light stability for one kind, while can accurately and effectively measure in sample
Platinum content and environmental-friendly cyanine dyes, the invention discloses 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-benzene
Base]-vinyl] the application of -1,3,3- trimethyl -3H- indoles chloride in spectrophotometry survey platinum.It is organic in the present invention
Complexing agent belongs to one kind of hemicyanine dye, is under the jurisdiction of cyanine dyes major class.
It is the specific technical solution of the present invention below:
2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1 with following structural formula (I),
3,3- trimethyl -3H- indoles chloride surveys the application in platinum in spectrophotometry.
Above-mentioned organic complexing agent can pass through commercially available compound, CAS 12217-48-0 known to being.
Further, above-mentioned application the following steps are included:
A, the preparation of solution: 10mgL-1Pt (IV) standard solution: by be added deionized water, be by concentration
1000mg·L-1Pt (IV) standard solution dilution, obtain 10mgL-1Pt (IV) standard solution；Enveloping agent solution: it weighs
2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3- trimethyl -3H- indoles chloride
34.40mg adds deionized water to be settled to 100mL, shakes up, and obtains 1 × 10-3mol·L-1Enveloping agent solution；
B, draw standard curve: taking 10 centrifuge tubes, be separately added into 0,0.1,0.2,0.3,0.4,0.5,0.6,0.7,
0.8, the 10mgL of 0.9mL-1Pt (IV) standard solution, and sequentially add 0.5mL0.5molL-1H2SO4Solution,
1.0mL0.01mol·L-1KI solution and 0.3mL1 × 10-3mol·L-1Enveloping agent solution, be settled to deionized water
5mL shakes up, and stands 1min.It is eventually adding 5mL extractant, separates organic phase after extracting 1min.Obtain Pt (IV) concentration difference
For 0,0.2,0.4,0.6,0.8,1.0,1.2,1.4,1.6,1.8mgL-1Extract liquor.The extract liquor for being 0 with Pt (IV) concentration
The extinction of remaining extract liquor is successively tested according to ultraviolet-uisible spectrophotometer operating instruction at 510-540nm for reference
Degree, using the concentration of platinum ion in extract liquor as abscissa, ordinate is absorbance value, draws standard curve.Wherein, in KI solution
Include 0.2wt% sodium ascorbate.
C, sample measures: specifically comprising the steps of
(1) Specimen eliminating: the resolution acid of 2-10ml being added into sample to be tested, sets heating on electric hot plate and clears up to Mao Bai
Cigarette is added deionized water constant volume to 30-50ml after catching up with acid, obtains digestion solution.
(2) in the digestion solution obtained to step (1), it is molten that dilute sulfuric acid, potassium iodide and complexing agent complex reaction: are sequentially added
Liquid is added deionized water constant volume to 5-10ml, shakes up and stand 1min.Wherein, 0.2wt% sodium ascorbate is included in KI solution.
(3) liquid-liquid extraction: the extractant that 5-10ml is added in the solution obtained to (2) is extracted, after by organic phase point
From obtaining extract liquor；
(4) absorbance measurement: using Pt (IV) concentration be 0 solution as reference, the determination step (3) at 510-540nm
The absorbance of the extract liquor arrived, and according to the content of standard curve calculating platinum.
In above-mentioned steps B and step C- (3), sour one in concentrated nitric acid, concentrated phosphoric acid, hydrofluoric acid, concentrated hydrochloric acid of resolution
Kind is a variety of.
In above-mentioned steps C- (1), the extractant is any one of ethyl acetate, butyl acetate, dimethylbenzene.
2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3- front three provided by the invention
Base -3H- indoles chloride surveys the application in platinum in spectrophotometry, can be used for environmental water sample, model water sample, glass Trace Amounts of Platinum
Separation and concentration and detection.
Compared with the prior art, the invention has the following advantages:
1, compared to the existing cyanine dyes as complexing agent, there is the complexing agent in the present invention maximum absorption wave to grow up,
The high advantage of photostability can avoid saturated absorption area and the platinum ion absorption band of near ultraviolet.
2, rapidly, the chromogenic reaction of complexing agent and platinum in the present invention can quickly complete at room temperature for colour developing, show after 1min
Color is basicly stable.
3, the complexing product stability in the present invention is high, and after liquid-liquid extraction separation, extract liquor can at least stablize 6h.
4, measuring method provided by the invention is anti-interference strong, has good selectivity to platinum.Concurrent in complicated substrate
Matter interference is more serious, and can be effectively reduced ion interference using the method for liquid-liquid separation after complexing.
5, agents useful for same is safe and harmless and dosage is small, to operator and environmental-friendly.
Detailed description of the invention
Fig. 1 is the platinum Gradient Absorption curve graph of the embodiment of the present invention.
Fig. 2 is the platinum Working calibration curve of the embodiment of the present invention.In Fig. 2, abscissa is the dense of platinum ion in extract liquor
Degree, ordinate is the absorbance value obtained using the extract liquor that Pt (IV) concentration is 0 as reference；Using a length of 1cm ratio of light path
Color ware；In standard curve, y=0.3343x-0.0056, R2=0.9973.
Specific embodiment
Below with reference to embodiment, the invention will be further elaborated, but should not be limited the scope of the invention with this.
The embodiment of the present invention is as follows:
Using the platinum of trace in spectrophotometry laser glass sample.Complexing agent uses 2- [2- [4- [(2- cyano second
Base)-Methyl-amino]-phenyl]-vinyl] -1,3,3- trimethyl -3H- indoles chlorides, TCL production, purchased from Chinese reagent
Net；Ultraviolet-uisible spectrophotometer selects PerkinElmer Lambda 950UV-VIS-NIR, wave-length coverage 400-650nm.
A, the preparation of solution:
10mg·L-1Pt (IV) standard solution: take appropriate 1000mgL-1Pt (IV) standard solution (Macklin is raw
Produce), deionized water is added, dilution obtains 10mgL-1Pt (IV) standard solution.
Enveloping agent solution: 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-second of precise 34.40mg
Alkenyl] -1,3,3- trimethyl -3H- indoles chlorides, add deionized water to be settled to 100mL, shake up, obtains 1 × 10-3mol·L-1
Enveloping agent solution.
B, standard curve is drawn:
Take 10 centrifuge tubes, number consecutively 0#, 1#, 2#, 3#, 4#, 5#, 6#, 7#, 8#, 9#, pipette 0 respectively, 0.1,
0.2, the 10mgL of 0.3,0.4,0.5,0.6,0.7,0.8,0.9mL-1Pt (IV) standard solution, and sequentially add
0.5mL0.5mol·L-1H2SO4Solution, 1.0mL0.01molL-1KI solution (including 0.2wt% sodium ascorbate) and
0.3mL1×10-3mol·L-1Enveloping agent solution, be settled to 5mL with deionized water, shake up stand 1min.It is eventually adding 5mL
Ethyl acetate separates organic phase after extracting 1min.At this point, in 10 centrifuge tubes the concentration of Pt (IV) be respectively 0,0.2,0.4,
0.6、0.8、1.0、1.2、1.4、1.6、1.8mg·L-1。
By 0# sample be reference, according to ultraviolet-uisible spectrophotometer operating instruction successively test 0#, 1#, 2#, 3#, 4#,
The absorbance of 5#, 6#, 7#, 8#, 9#, absorbance curve such as Fig. 1 are averaged, and draw mark for each sample retest five times
Directrix curve such as Fig. 2.
C, sample measures:
(1) Specimen eliminating: weighing 0.2-0.4g laser glass powder sample in micro-wave diminishing pot, addition 4mL concentrated phosphoric acid,
8mL concentrated nitric acid clears up 40min at 180 DEG C in microwave dissolver；In heating evaporation on electric hot plate to Mao Bai after having cleared up
Cigarette is added deionized water after cooling and is settled to 40mL, obtains digestion solution.
(2) it complex reaction: takes 1mL digestion solution in centrifuge tube, and sequentially adds 0.5mL0.5molL-1H2SO4It is molten
Liquid, 1.0mL0.01molL-1KI solution (including 0.2wt% sodium ascorbate) and 0.3mL1 × 10-3mol·L-1Complexing
Agent solution is settled to 5mL with deionized water, shakes up and stands 1min.
(3) liquid-liquid extraction: 5mL ethyl acetate being added into obtained solution, and after extracting 1min, organic phase is separated.
(4) absorbance measurement: with reagent blank (0#) for reference, the absorbance value of sample is measured, standard curve meter is utilized
The content of point counting analysis platinum.
The result that the result and inductively coupled plasma body atomic absorption spectrography (AAS) that this method measures obtain is compared
Right, the two is consistent, when illustrating to be measured the platinum in laser glass, using method provided by the invention obtain the result is that
Reliably.
Working principle of the present invention:
Table 1 is complexing agent of the present invention and comparison of other cyanine dyes complexing agents on maximum absorption wavelength and photostability.
The maximum absorption wavelength of complexing agent of the present invention can avoid platinum ion (Pt at 530nm4+) absorption band (350-430nm).
In addition, 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3- trimethyl -3H-
Complex reaction colour developing occurs in weak acidic medium for indoles chloride and platinum and iodide ion, and the molar ratio for generating complex compound is 2:1:
6.The chromogenic reaction can be carried out quickly at room temperature, color stability after placement 1min, after liquid-liquid extraction, placed 6h and surveyed immediately
Fixed absorbance value difference is only 0.002, and system illustrates color development system in organic phase at least still in relatively stable state
6h can be stablized.Liquid-liquid extraction is because of 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3-
Trimethyl -3H- indoles chloride is to exist in water phase with the state of cation, is not easily accessible organic phase.And it is deposited in platinum and iodine
In case, platinum and iodine preferential reaction become stable complex anion group, anion radical further with the network of cationic state
Mixture, which combines, to be generated macromolecular and rapidly enters organic phase.Table 2 be the present invention allows ion interference multiple, iodide ion and network
The double selection of mixture makes this process of most of ion pairs noiseless, illustrates that detection method provided by the invention has very well platinum
Selectivity.
Table 1
| Solvent | Maximum absorption wavelength (nm) | Stability | |
| Astrafloxin FF | DMF | 556 | It is sensitive to pH |
| MPVTI | Toluene | 430 | Photostability is poor |
| Complexing agent of the present invention | Ethyl acetate | 530 | Light is stable, pH range is big |
Table 2
| Interfering ion | It accommodates multiple (molar ratio of interfering ion and platinum ion) |
| Alkali metal, alkaline-earth metal, Al (III) | 1000 |
| Ni(II),Co(II),Zn(II),Sn(II),Mn(II),Cr(III),Cd(II) | 500 |
| Cu(II),Fe(III) | >10,<100 |
| Pb(II),Hg(II) | <10 |
Claims (5)
1. the 2- [2- [4- [(2- cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3 with following structural formula (I),
3- trimethyl -3H- indoles chloride surveys the application in platinum in spectrophotometry.
2. application according to claim 1, which comprises the following steps:
A, the preparation of solution: 10mgL-1Pt (IV) standard solution: by be added deionized water, by concentration be 1000mgL-1
Pt (IV) standard solution dilution, obtain 10mgL-1Pt (IV) standard solution；Enveloping agent solution: 2- [2- [4- [(2- is weighed
Cyano ethyl)-Methyl-amino]-phenyl]-vinyl] -1,3,3- trimethyl -3H- indoles chloride 34.40mg, add deionization
Water is settled to 100mL, shakes up, and obtains 1 × 10-3mol·L-1Enveloping agent solution；
B, draw standard curve: taking 10 centrifuge tubes, be separately added into 0,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,
The 10mgL of 0.9mL-1Pt (IV) standard solution, and sequentially add 0.5mL0.5molL-1H2SO4Solution,
1.0mL0.01mol·L-1KI solution and 0.3mL1 × 10-3mol·L-1Enveloping agent solution, be settled to deionized water
5mL shakes up, and stands 1min；It is eventually adding 5mL extractant, separates organic phase after extracting 1min, obtains Pt (IV) concentration difference
For 0,0.2,0.4,0.6,0.8,1.0,1.2,1.4,1.6,1.8mgL-1Extract liquor；The extract liquor for being 0 with Pt (IV) concentration
The extinction of remaining extract liquor is successively tested according to ultraviolet-uisible spectrophotometer operating instruction at 510-540nm for reference
Degree, using the concentration of platinum ion in extract liquor as abscissa, ordinate is absorbance value, draws standard curve；Wherein, in KI solution
Include 0.2wt% sodium ascorbate；
C, sample measures: specifically comprising the steps of
(1) Specimen eliminating: the resolution acid of 2-10ml being added into sample to be tested, sets heating resolution on electric hot plate and catches up with to Mao Baiyan
Deionized water constant volume is added after acid to 30-50ml, obtains digestion solution；
(2) complex reaction: in the digestion solution obtained to step (1), dilute sulfuric acid, potassium iodide and enveloping agent solution is sequentially added, is added
Enter deionized water constant volume to 5-10ml, shakes up and stand 1min；Wherein, 0.2wt% sodium ascorbate is included in KI solution；
(3) liquid-liquid extraction: in the solution obtained to (2) be added 5-10ml extractant extracted, after organic phase is separated,
Obtain extract liquor；
(4) absorbance measurement: using Pt (IV) concentration be 0 solution as reference, determination step (3) obtains at 510-540nm
The absorbance of extract liquor, and according to the content of standard curve calculating platinum.
3. application according to claim 2, which is characterized in that resolution acid described in step B and step C- (3) is dense nitre
One of acid, concentrated phosphoric acid, hydrofluoric acid, concentrated hydrochloric acid are a variety of.
4. application according to claim 2, which is characterized in that extractant described in step C- (1) is ethyl acetate, second
Any one of acid butyl ester, dimethylbenzene.
5. a kind of claim 1-4 it is any it is described apply environmental water sample, model water sample, glass Trace Amounts of Platinum separation and concentration with
Application in detection.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111948196A (en) * | 2020-07-16 | 2020-11-17 | 中国科学院上海光学精密机械研究所 | Method for detecting platinum ion content in solution through visual colorimetry |
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