CN103411956A - Method for rapidly detecting iodate by surface enhanced Raman spectroscopy and application of method - Google Patents
Method for rapidly detecting iodate by surface enhanced Raman spectroscopy and application of method Download PDFInfo
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- CN103411956A CN103411956A CN2013103694946A CN201310369494A CN103411956A CN 103411956 A CN103411956 A CN 103411956A CN 2013103694946 A CN2013103694946 A CN 2013103694946A CN 201310369494 A CN201310369494 A CN 201310369494A CN 103411956 A CN103411956 A CN 103411956A
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- paranitroanilinum
- azanol
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- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 20
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 37
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 29
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005859 coupling reaction Methods 0.000 claims abstract description 15
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003651 drinking water Substances 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract 4
- 229940005654 nitrite ion Drugs 0.000 claims abstract 3
- 239000000523 sample Substances 0.000 claims description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 29
- 235000012206 bottled water Nutrition 0.000 claims description 16
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 claims description 14
- -1 nitrite anions Chemical class 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 229940005633 iodate ion Drugs 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 230000002708 enhancing effect Effects 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 4
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 4
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 4
- 229940124530 sulfonamide Drugs 0.000 claims description 4
- 238000004451 qualitative analysis Methods 0.000 claims description 3
- 238000004445 quantitative analysis Methods 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 229950000244 sulfanilic acid Drugs 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 abstract description 11
- 230000008878 coupling Effects 0.000 abstract description 8
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000006149 azo coupling reaction Methods 0.000 abstract 1
- 235000020188 drinking water Nutrition 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 239000013535 sea water Substances 0.000 description 12
- 235000002639 sodium chloride Nutrition 0.000 description 12
- 238000004611 spectroscopical analysis Methods 0.000 description 11
- 150000002500 ions Chemical class 0.000 description 7
- 239000000975 dye Substances 0.000 description 6
- ICIWUVCWSCSTAQ-UHFFFAOYSA-N iodic acid Chemical compound OI(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-N 0.000 description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 5
- 230000005284 excitation Effects 0.000 description 5
- 239000011630 iodine Substances 0.000 description 5
- 229910052740 iodine Inorganic materials 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000002452 interceptive effect Effects 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 0 *c(cc1)ccc1[N-] Chemical compound *c(cc1)ccc1[N-] 0.000 description 3
- 239000000987 azo dye Substances 0.000 description 3
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 3
- 235000006666 potassium iodate Nutrition 0.000 description 3
- 239000001230 potassium iodate Substances 0.000 description 3
- 229940093930 potassium iodate Drugs 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- NDANYAAFYIQLDE-UHFFFAOYSA-N Cc1cccc2c1C=C=C2 Chemical compound Cc1cccc2c1C=C=C2 NDANYAAFYIQLDE-UHFFFAOYSA-N 0.000 description 1
- 206010067997 Iodine deficiency Diseases 0.000 description 1
- 206010044278 Trace element deficiency Diseases 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明涉及表面增强拉曼光谱快速检测碘酸根的方法及应用。碘酸根自身的拉曼信号很弱，SERS信号也很弱，碘酸根将羟胺氧化为亚硝酸根，在酸性或弱碱性条件下亚硝酸根离子与重氮-偶合试剂生成偶合染料，偶合染料的SERS信号强，通过SERS测定偶合染料的量间接对碘酸根进行定性和定量检测。本发明采用Au/SiO2作为SERS基底材料，二氧化硅壳层提高了增强粒子的稳定性，使结果重复性更好。本方法适用于食盐、饮用水、环境等复杂样品中碘酸根的快速测定，具有简单、快速（约2min），适用于现场检测，有利于推广使用等优点。
The invention relates to a method for rapidly detecting iodate by surface-enhanced Raman spectroscopy and an application thereof. The Raman signal of iodate itself is very weak, and the SERS signal is also very weak. The iodate oxidizes hydroxylamine to nitrite, and the nitrite ion and the diazo-coupling reagent generate a coupling dye under acidic or weakly alkaline conditions. The coupling dye The SERS signal is strong, and the amount of the coupled dye is determined by SERS to indirectly detect the iodate radical qualitatively and quantitatively. The invention adopts Au/SiO 2 as the SERS base material, and the silicon dioxide shell layer improves the stability of the reinforced particle, so that the repeatability of the result is better. This method is suitable for the rapid determination of iodate in complex samples such as salt, drinking water, and the environment. It has the advantages of being simple and fast (about 2 minutes), suitable for on-site detection, and conducive to popularization and use.
Description
Technical field
The present invention relates to the method for Surface enhanced raman spectroscopy fast detecting iodate, relate in particular to method and the application thereof of Surface enhanced raman spectroscopy fast detecting iodate, be applicable to the mensuration of iodate in the complex samples such as salt, potable water and environment.
Background technology
Iodine is a kind of important trace element, and iodine deficiency is the important public health problem in the whole world, particularly for child and conceived women.Address this problem at present the best way and in salt, add exactly iodate.Therefore the content of studying the Iodine Content In Iodized Salt acid group has very important significance for the quality and the quality control that guarantee salt.
The traditional detection method of iodate has multiple, and the detection method of recent domestic report mainly contains titrimetry, gas chromatography, high performance liquid chromatography, chromatography of ions, spectrum and mass spectrum etc.But these methods exist process loaded down with trivial details, consuming time, be not easy to the deficiencies such as Site Detection.Therefore foundation simply, the iodate detection method has important meaning fast.
Summary of the invention
Loaded down with trivial details, consuming time and be not easy to the deficiencies such as Site Detection in order to solve conventional iodine acid group detection method process.The invention provides the method for a kind of Surface enhanced raman spectroscopy (SERS) fast detecting iodate, and the application in iodate mensuration in the complex samples such as salt, potable water and environment.
Principle of the present invention: the Raman signal of iodate self is very weak, and the SERS signal is also very weak, therefore can not directly measure iodate by SERS.Iodate is oxidized to nitrite anions by azanol, nitrite anions generates diazonium-coupling product with diazonium-coupling reagent under acid condition, this product self Raman signal is stronger, and the SERS of this product is enhanced, using this coupling product as the probe of iodate, iodate is carried out to indirectly quantitative and qualitative analysis measure by measuring coupling product.
In order to realize the foregoing invention purpose, the present invention has adopted following Surface enhanced raman spectroscopy fast detecting iodate method, it is characterized in that: Surface enhanced raman spectroscopy fast detecting iodate method, it is characterized in that: make iodate in testing sample that azanol is oxidized to nitrite anions, nitrite anions and diazo reagent and azo reagent generate diazonium-para-dye under acid condition, using this diazonium-para-dye as probe molecule, indirectly iodate is carried out to quantitative and qualitative analysis mensuration by measuring diazonium-para-dye.
As preferred version, the iodate ion in said method in testing sample is converted into nitrite anions by azanol, is that nitrite anions and paranitroanilinum and hydrochloride naphthodiamide generate red diazonium-para-dye under acid condition.
Specifically, above-mentioned quilitative method comprises the following steps:
A, get the iodate solution of variable concentrations in centrifuge tube, add azanol to generate nitrite anions, add again diazo reagent, be mixed evenly and make it that diazo-reaction occur, after add and the azo reagent of diazo reagent with equimolar ratio, be mixed evenly and make it that coupling reaction occur, reactant liquor is placed 1min, obtains diazonium-para-dye;
B, get certain volume a step gained reactant liquor in sample hose, then add the enhancing mix particles of equal volume even, directly with the portable Raman instrument of DeltaNu, detect;
C, measure and draw out the corresponding Surface enhanced raman spectroscopy figure of different content iodate solution;
D, measure testing sample, add azanol to generate nitrite anions, add again diazo reagent, be mixed evenly and make it that diazo-reaction occur, after add and the azo reagent of diazo reagent with equimolar ratio, be mixed evenly and make it that coupling reaction occur, reactant liquor is placed 1min, obtains diazonium-para-dye; Add the enhancing mix particles of equal volume even, directly with the Raman instrument, detect the Surface enhanced raman spectroscopy of this sample, to sample, carry out qualitative according to the Raman shift in step c gained Raman spectrogram.
As further quilitative method, described diazo reagent is the paranitroanilinum hydrochloric acid solution; Described azo reagent is the hydrochloride naphthodiamide aqueous solution; Described step c also comprises and draws out 1138cm
-1The peak area of Raman shift place-iodate ion content standard curve; Described steps d also comprises according to 1138cm
-1The peak area of Raman shift place-iodate ion content standard opisometer is calculated the content of iodate in sample.
Specifically, described concentration of hydrochloric acid solution is 0.1-3.0mol L
-1Described azanol concentration is 0.001-3.0mol L
-1The concentration of hydrochloric acid solution of described paranitroanilinum is 0.001-1.0mol L
-1The concentration of aqueous solution of described hydrochloride naphthodiamide is 0.001-1.0mol L
-1.
Described centrifuge tube volume is 1mL.
Described sample hose is the 1mL glass tube.
It is 100:(0.1～3.0 that described iodate solution adds volume and the ratio that adds volume of the hydrochloric acid solution of azanol and paranitroanilinum): (0.1～3.0); It is 100:(0.1～3.0 that described testing sample adds the hydrochloric acid solution of volume and azanol and paranitroanilinum to add the ratio of volume): (0.1～3.0).
Described iodate solution can be selected potassium iodate solution.
As possibility, diazo reagent can be paranitroanilinum, sulfanilamide (SN) and sulfanilic acid etc., and azo reagent can be diphenylamine and hydrochloride naphthodiamide etc.
Described enhancing particle is Au/SiO
2Nano sol, wherein Au/SiO
2For the Au nanoparticle surface, be coated with the core-shell type structure of silica shell, described enhancing particle can be also A g Nano sol or Au Nano sol etc.
Described Raman instrument excitation wavelength is 785nm; Laser power: 60mv; Sweep time: 1s.
Be respectively 1098,1138 for Raman shift qualitatively, 1381 and 1426cm
-1For quantitative Raman shift, be 1138cm
-1, wherein 1098 is C-NO
2Stretching vibration, 1138cm
-1For C-N=N stretching vibration, 1381cm
-1C-C stretching vibration in phenyl ring, 1426cm
-1For the N=N stretching vibration.
The present invention also provides the application of Surface enhanced raman spectroscopy fast detecting iodate method iodate content in measuring salt, potable water or environment.
By above-mentioned steps, can find, method and the application thereof of surface-enhanced Raman fast detecting iodate of the present invention, have the advantages such as simple, quick, is applicable to Site Detection, is conducive to promote the use of etc.And the degree of depth that color is produced in coupling becomes positive correlation with the concentration of iodate ion, namely iodate ion concentration is larger, and color is darker, can to iodate content in sample, estimate by the change color of visual inspection reaction system.
The accompanying drawing explanation:
Below in conjunction with the drawings and specific embodiments, this experiment is elaborated:
Fig. 1 is Raman and the SERS figure of iodate and diazonium-coupling product,
Wherein, a is 0.05mg L
-1Iodate coupling product SERS; B is 1000mg L
-1Iodate coupling product Raman figure; C is 1000mg L
-1Iodate SERS; D is 1000mg L
-1Iodate Raman figure;
Fig. 2 is the SERS figure of the corresponding coupling product of variable concentrations iodate, wherein, and iodate concentration (a-g): 0,0.010,0.030,0.050,0.075,0.10and0.13mg L
-1
Fig. 3 is 1138cm
-1The peak area of Raman shift place-iodate content standard curve.
Embodiment
The method of SERS fast detecting iodate of the present invention and application thereof are based on following chemical reaction:
2IO
3 -+3NH
2OH→3NO
2 -+3H
++2I
-+3H
2O
The final color that generates azo dyes be redness, and the degree of depth of its color becomes positive correlation with the concentration of iodate ion, and namely iodate ion concentration is larger, and color is darker.This azo dyes very easily is adsorbed on the enhancing particle surface, obtains Surface enhanced raman spectroscopy, the content of the amount indirect determination iodate by measuring azo dyes.
The embodiment of SERS fast detecting iodate method of the present invention and application thereof is as follows, but content of the present invention is not limited to this fully.
Iodate in embodiment 1SERS fast detecting salt
1.1 key instrument and reagent:
The portable Raman instrument of DeltaNu Inspector, electronic balance;
The iodate standard solution: precision takes the Potassiumiodate of 0.0122g dry 24h in baking oven, with ultrapure water, dissolves and moves in the 100mL volumetric flask, and be diluted to scale, and being mixed with concentration is 100mg L
-1The Potassiumiodate storing solution, 4 ℃ of preservations, be diluted to desired concn before use; Azanol (0.02mol L
-1) take the 0.1389g azanol, be dissolved in the 100mL aqueous solution, put in brown bottle and mix, 4 ℃ of preservations; Paranitroanilinum (0.02mol L
-1): take the 0.2762g paranitroanilinum, be dissolved in 100mL hydrochloric acid solution (1mol L
-1) in, after mixing, put in brown bottle 4 ℃ of preservations; Hydrochloride naphthodiamide (0.02mol L
-1): take the 0.5183g hydrochloride naphthodiamide, be dissolved in the 100mL aqueous solution, put in brown bottle and mix, 4 ℃ of preservations; Au/SiO
2: Au NPs radius 55nm, SiO
2Shell thickness 1-2nm.Experimental water is ultrapure water.
1.2 sample preparation:
Take 0.25g iodized salt (being accurate to 0.0001g) in the 25mL volumetric flask, add the 15-20mL ultrapure water, shake up, be settled to 25mL.For the mark-on salt sample, analyzing, is 100mg L by 25 μ L concentration
-1Iodate join in the 10mL salt sample, mix, mark-on concentration is 25 μ g g
-1.
1.3 the drafting of typical curve
Compound concentration is 0.0075,0.010,0.030,0.050,0.075,0.10and0.13mg L respectively
-1Iodate solution, get above-mentioned solution 200 μ L successively in the 2mL centrifuge tube, adds hydroxylamine solution 2 μ L, after mixing, adds paranitroanilinum hydrochloric acid solution 2 μ L, after mixing, continues to add hydrochloride naphthodiamide solution 2 μ L, after standing 1min.Get isopyknic above-mentioned reactant liquor and Au/SiO
2In sample hose, mix, with DeltaNu Raman instrument direct-detection, excitation wavelength 785nm, sweep time: 1s; Drawn 1138cm
-1Raman shift place peak area-iodate ion content standard curve, be shown in Fig. 3.
1.4 the mensuration of interfering ion
The effects multiple common kation and negative ion to 0.1mg L
-1The interference that iodate is measured, result is as shown in table 1.As add peak area (1138cm after interfering ion
-1) RSD in ± 10%, be considered as the mensuration that this ion does not disturb iodate.As can be seen here, this method has good practicality to the mensuration of iodate.
Table 1
1.5 the mensuration of salt sample:
Measure the above-mentioned salt solution of 200 μ L, add hydroxylamine solution 2 μ L, after mixing, add the paranitroanilinum of 2 μ L and the hydrochloride naphthodiamide of 2 μ L, after mixing, after standing 1min.Get isopyknic above-mentioned reactant liquor and Au/SiO
2In sample hose, mix, with DeltaNu Raman instrument, detect, excitation wavelength: 785nm, sweep time: 1s, read 1138cm
-1The peak area of Raman shift place, substitution 1138cm
-1The peak area of Raman shift place-iodate content standard curve, calculate the content of Iodine in Table Salt acid group.The content that calculates the Iodine in Table Salt acid group is 39.33 ± 1.69 μ g g
-1, after mark-on, the content of iodate is 66.12 ± 2.31 μ g g
-1, recovery of standard addition is 107.1%.
Iodate in embodiment 2SERS fast detecting bottled water
In this application, the key instrument of using and reagent, the drafting of typical curve and the mensuration of interfering ion are identical with embodiment 1.
2.1 the processing of bottled water sample:
Measure the bottled water of certain volume, obtain the bottled water sample.Then by this bottled water sample preparation mark-on concentration, be 0.020mg L
-1Mark-on bottled water sample.
2.2 the mensuration of bottled water sample:
Get bottled water sample and the mark-on bottled water sample of 200 μ L, add 2 μ L hydroxylamine solutions, after mixing, add the paranitroanilinum of 2 μ L and the hydrochloride naphthodiamide of 2 μ L, after mixing, after standing 1min.Get isopyknic above-mentioned reactant liquor and Au/SiO
2In sample hose, mix, with DeltaNu Raman instrument, detect, excitation wavelength: 785nm, sweep time: 1s, read 1138cm
-1The peak area of Raman shift place, substitution 1138cm
-1The peak area of Raman shift place-iodate content standard curve, calculate the content of iodate in bottled water.This method does not detect the existence of iodate in the bottled water sample, and after mark-on, the content of iodate is 0.022 ± 0.001mg L
-1, recovery of standard addition is 109.1%.
Iodate in embodiment 3SERS fast detecting seawater
In this application, the key instrument of using and reagent, the drafting of typical curve and the mensuration of interfering ion are identical with embodiment 1.
3.1 the processing of seawater sample:
Measure the seawater of certain volume, after filtration, obtain seawater sample.Then by this seawater sample preparation mark-on concentration, be 0.020mg L
-1The mark-on seawater sample.
3.2 the mensuration of seawater sample:
Get seawater sample and the mark-on seawater sample of 200 μ L,, add 2 μ L hydroxylamine solutions, after mixing, add the paranitroanilinum of 2 μ L and the hydrochloride naphthodiamide of 2 μ L, after mixing, after standing 1min.Get isopyknic above-mentioned reactant liquor and Au/SiO
2In sample hose, mix, with DeltaNu Raman instrument, detect, excitation wavelength: 785nm, sweep time: 1s, read 1138cm
-1The peak area of Raman shift place, substitution 1138cm
-1The peak area of Raman shift place-iodate content standard curve, calculate the content of iodate in seawater.This method does not detect the existence of iodate in seawater sample, and after mark-on, the content of iodate is 0.017 ± 0.001mg L
-1, recovery of standard addition is 86.2%.
Be more than the application of SERS fast detecting iodate of the present invention in salt, bottled water and seawater moderate sample, can find out from embodiment, the method for this mensuration iodate of the present invention has the advantages such as simple, quick.
Those skilled in the art will be appreciated that, above embodiment illustrates the present invention, not as the restriction to invention, as long as in connotation scope of the present invention, all will drop in claim scope of the present invention variation, the sex change of the above embodiment.
Claims (10)
1. Surface enhanced raman spectroscopy fast detecting iodate method, it is characterized in that: iodate is oxidized to nitrite anions by azanol, nitrite ion and diazo reagent and azo reagent reacting generate diazonium-para-dye under acid condition, using this diazonium-para-dye as probe molecule, indirectly the iodate root is carried out to quantitative and qualitative analysis mensuration by measuring diazonium-para-dye.
2. method according to claim 1, it is characterized in that: at first iodate is oxidized to nitrite anions by azanol, and nitrite ion and paranitroanilinum and hydrochloride naphthodiamide generate red diazonium-para-dye under acid condition.
3. method according to claim 1 is characterized in that comprising the following steps:
A, get the iodate solution of variable concentrations in centrifuge tube, add azanol, after mixing, add diazo reagent, be mixed evenly and make it that diazo-reaction occur, after add and the azo reagent of diazo reagent with equimolar ratio, be mixed evenly and make it that coupling reaction occur, reactant liquor is placed 1min, obtains diazonium-para-dye;
B, get certain volume a step gained reactant liquor in sample hose, then add the enhancing mix particles of equal volume even, directly with the portable Raman instrument of DeltaNu, detect;
C, measure and draw out the corresponding Surface enhanced raman spectroscopy figure of different content iodate solution;
D, measure testing sample, add azanol to generate nitrite anions, add again diazo reagent, be mixed evenly and make it that diazo-reaction occur, after add and the azo reagent of diazo reagent with equimolar ratio, be mixed evenly and make it that coupling reaction occur, reactant liquor is placed 1min, obtains diazonium-para-dye; Add the enhancing mix particles of equal volume even, directly with the Raman instrument, detect the Surface enhanced raman spectroscopy of this sample, to sample, carry out qualitative according to the Raman shift in step c gained Raman spectrogram.
4. method according to claim 3, it is characterized in that: described diazo reagent is the paranitroanilinum hydrochloric acid solution; Described azo reagent is the aqueous solution of hydrochloride naphthodiamide; Described step c also comprises and draws out 1138cm
-1The peak area of Raman shift place-iodate ion content standard curve; Described steps d also comprises according to 1138cm
-1The peak area of Raman shift place-iodate ion content standard opisometer is calculated the content of iodate in sample.
5. method according to claim 4, is characterized in that: be 0.1-3.0mol L be used to the concentration of hydrochloric acid solution of preparing the paranitroanilinum hydrochloric acid solution
-1Azanol concentration is 0.001-3.0mol L
-1The concentration of hydrochloric acid solution of paranitroanilinum is 0.001-1.0mol L
-1The concentration of aqueous solution of described hydrochloride naphthodiamide is 0.001-1.0mol L
-1.
6. method according to claim 5, it is characterized in that: it is 100:(0.1～3.0 that described iodate solution adds volume and the ratio that adds volume of the hydrochloric acid solution of azanol and paranitroanilinum): (0.1～3.0); It is 100:(0.1～3.0 that described testing sample adds the hydrochloric acid solution of volume and azanol and paranitroanilinum to add the ratio of volume): (0.1～3.0).
7. method according to claim 1, diazo reagent can be paranitroanilinum, sulfanilamide (SN) and sulfanilic acid etc., azo reagent can be diphenylamine and hydrochloride naphthodiamide etc.
8. detection method according to claim 2, it is characterized in that: described enhancing particle is Au/SiO
2Nano sol, wherein Au/SiO
2For the Au nanoparticle surface, be coated with the core-shell type structure of silica shell, described enhancing particle can be also the Nano sols such as Ag Nano sol or Au etc.
9. detection method according to claim 4 is characterized in that: for Raman shift qualitatively, be respectively 1098,1138,1381 and 1426cm
-1For quantitative Raman shift, be 1138cm
-1, wherein 1098 is C-NO
2Stretching vibration, 1138cm
-1For C-N=N stretching vibration, 1381cm
-1C-C stretching vibration in phenyl ring, 1426cm
-1For the N=N stretching vibration.
10. the application of the arbitrary described Surface enhanced raman spectroscopy fast detecting iodate method of claim 1～9 iodate content in measuring salt, potable water or environment.
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| CN2013103694946A CN103411956A (en) | 2013-08-22 | 2013-08-22 | Method for rapidly detecting iodate by surface enhanced Raman spectroscopy and application of method |
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| CN2013103694946A CN103411956A (en) | 2013-08-22 | 2013-08-22 | Method for rapidly detecting iodate by surface enhanced Raman spectroscopy and application of method |
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Cited By (9)
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| CN103868907A (en) * | 2014-01-24 | 2014-06-18 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing silica-coated surface-enhanced raman marker nanoparticles |
| CN104165881A (en) * | 2014-08-25 | 2014-11-26 | 广西师范大学 | Method for measuring IO3<-> by utilizing surface-enhanced Raman scattering spectrums |
| CN104777148A (en) * | 2015-04-17 | 2015-07-15 | 华东理工大学 | Method for rapidly detecting total protein in milk |
| CN105259158A (en) * | 2015-11-13 | 2016-01-20 | 暨南大学 | Surface enhanced Raman scattering immunochromatography test paper strip and preparation method and application |
| CN105372222A (en) * | 2014-08-22 | 2016-03-02 | 中国科学院生态环境研究中心 | Detection method of divalent heavy metal |
| CN108279228A (en) * | 2018-05-04 | 2018-07-13 | 山东理工大学 | A method of utilizing acetate ion concentration in the Raman spectroscopy acid solution of the silica dioxide granule containing methylene blue |
| CN111175241A (en) * | 2020-03-09 | 2020-05-19 | 薛原 | High-precision urine iodine detection method |
| CN114685311A (en) * | 2020-12-29 | 2022-07-01 | 华中师范大学 | An azo aromatic compound and its application and a reagent for enhancing Raman scattering signal |
| CN116148410A (en) * | 2022-12-23 | 2023-05-23 | 苏州大学 | A kind of SERS base material that can be used for continuous TLC detection and its preparation method and application |
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| CN103868907A (en) * | 2014-01-24 | 2014-06-18 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing silica-coated surface-enhanced raman marker nanoparticles |
| CN105372222A (en) * | 2014-08-22 | 2016-03-02 | 中国科学院生态环境研究中心 | Detection method of divalent heavy metal |
| CN104165881A (en) * | 2014-08-25 | 2014-11-26 | 广西师范大学 | Method for measuring IO3<-> by utilizing surface-enhanced Raman scattering spectrums |
| CN104165881B (en) * | 2014-08-25 | 2017-01-18 | 广西师范大学 | Method for measuring IO3 by utilizing surface-enhanced Raman scattering spectrums |
| CN104777148A (en) * | 2015-04-17 | 2015-07-15 | 华东理工大学 | Method for rapidly detecting total protein in milk |
| CN105259158A (en) * | 2015-11-13 | 2016-01-20 | 暨南大学 | Surface enhanced Raman scattering immunochromatography test paper strip and preparation method and application |
| CN108279228A (en) * | 2018-05-04 | 2018-07-13 | 山东理工大学 | A method of utilizing acetate ion concentration in the Raman spectroscopy acid solution of the silica dioxide granule containing methylene blue |
| CN108279228B (en) * | 2018-05-04 | 2020-12-08 | 山东理工大学 | A kind of method that utilizes the Raman spectrum of silica particle containing methylene blue to measure acetate ion concentration in acidic solution |
| CN111175241A (en) * | 2020-03-09 | 2020-05-19 | 薛原 | High-precision urine iodine detection method |
| CN111175241B (en) * | 2020-03-09 | 2020-09-18 | 刘宇娜 | High-precision urine iodine detection method |
| CN114685311A (en) * | 2020-12-29 | 2022-07-01 | 华中师范大学 | An azo aromatic compound and its application and a reagent for enhancing Raman scattering signal |
| CN114685311B (en) * | 2020-12-29 | 2024-06-04 | 华中师范大学 | Azo aromatic compound, application thereof and reagent for enhancing Raman scattering signal |
| CN116148410A (en) * | 2022-12-23 | 2023-05-23 | 苏州大学 | A kind of SERS base material that can be used for continuous TLC detection and its preparation method and application |
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