CN112666151A - Method for rapidly, qualitatively and quantitatively analyzing trace bromide ions - Google Patents
Method for rapidly, qualitatively and quantitatively analyzing trace bromide ions Download PDFInfo
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- CN112666151A CN112666151A CN202110123684.4A CN202110123684A CN112666151A CN 112666151 A CN112666151 A CN 112666151A CN 202110123684 A CN202110123684 A CN 202110123684A CN 112666151 A CN112666151 A CN 112666151A
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- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 31
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000010931 gold Substances 0.000 claims abstract description 34
- 229910052737 gold Inorganic materials 0.000 claims abstract description 34
- 239000002105 nanoparticle Substances 0.000 claims abstract description 30
- 238000001514 detection method Methods 0.000 claims abstract description 29
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 12
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 12
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910001414 potassium ion Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 3
- 229940006460 bromide ion Drugs 0.000 description 7
- 238000004659 sterilization and disinfection Methods 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 4
- 229910052794 bromium Inorganic materials 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- -1 Bromine ions Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- GATVIKZLVQHOMN-UHFFFAOYSA-N Chlorodibromomethane Chemical compound ClC(Br)Br GATVIKZLVQHOMN-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 description 2
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 2
- DIKBFYAXUHHXCS-UHFFFAOYSA-N bromoform Chemical compound BrC(Br)Br DIKBFYAXUHHXCS-UHFFFAOYSA-N 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 241001131796 Botaurus stellaris Species 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000002535 acidifier Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- FMWLUWPQPKEARP-UHFFFAOYSA-N bromodichloromethane Chemical compound ClC(Cl)Br FMWLUWPQPKEARP-UHFFFAOYSA-N 0.000 description 1
- 229950005228 bromoform Drugs 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000007674 genetic toxicity Effects 0.000 description 1
- 231100000025 genetic toxicology Toxicity 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for rapidly detecting and analyzing trace bromide ions, which specifically comprises the following steps: (1) preparing gold nanoparticle sol by using chloroauric acid solution to form an SERS enhanced substrate; (2) bromide ions are strongly adsorbed on the surface of the gold nanoparticle sol by forming Au-Br bonds; (3) adding high-concentration inorganic salt to induce gold nanoparticle sol to agglomerate; (4) performing Raman spectrum detection to locate at 178cm‑1Performing qualitative and quantitative detection on bromide ions in the sample to be detected by taking the characteristic Raman peaks of the Au-Br as the reference; the method provided by the invention can realize qualitative and quantitative detection of trace bromide ions in the water body, and has the advantages of simplicity, convenience, rapidness, low cost, high stability and the like.
Description
Technical Field
The invention belongs to the technical field of detection methods of non-metal ions in aqueous solution, and particularly relates to a method for rapidly, qualitatively and quantitatively analyzing trace bromide ions.
Background
Bromine ions widely exist in natural water and cannot harm human beings under normal conditions, but the content of the bromine ions in drinking water is too high, so that a brominated disinfection by-product with higher concentration can be generated in the disinfection process, the by-product has obvious carcinogenicity and genetic toxicity to the human body, and the toxicity of the brominated disinfection by-product is dozens of times of that of the chlorinated disinfection by-product. The limit value of bromate is 10ug/L, the limit values of bromodichloromethane, dibromochloromethane and bromoform brominated disinfection byproducts are 60 mug/L, 100 mug/L and 100 mug/L respectively, and the sum of the ratio of the measured concentration of each compound in the compounds to the limit values of the compounds is not more than 1. Effectively reducing the content of bromide ions in inlet water of an ozone oxidation or disinfection process in the process of treating drinking water, and having important practical significance for controlling the formation of bromate and brominated disinfection byproducts.
In the prior art, bromine ion detection methods include atomic absorption spectrometry, atomic fluorescence method, inductively coupled plasma mass spectrometry and the like, but the methods have the defects of expensive equipment, complex operation, long detection time, incapability of on-line monitoring and the like, and limit the wide application of the methods. Therefore, exploring a simple, fast, economical, efficient and on-line bromine detection method has become one of the important research directions in the fields of food, health and environmental analysis nowadays.
Chinese patent No. 201310403419.7 discloses a method for measuring bromide ion content in bittern by gas chromatography, which comprises selecting acidifying agent, derivatizing agent and oxidant for sample pretreatment, and measuring bromide ion content by hydrogen flame ion detector in gas chromatograph, wherein organic saturated ketones can rapidly generate substitution reaction with elementary bromine under catalysis of acid, reaction is balanced in a certain time, and bromide ketone compound is generated quantitatively.
The SERS method has the advantages of simplicity and convenience in operation, high sensitivity, low detection cost, high analysis speed and the like, and has great application potential in various fields such as environmental monitoring, biological analysis and detection, food science and the like. Some currently disclosed SERS methods for detecting bromide ions in water mainly focus on qualitative detection of bromide ions in water, lack of research on bromide ion detection sensitivity, and restrict application and popularization of the SERS method for detecting trace bromide ions.
Disclosure of Invention
In order to solve the problems of complex detection method, long time consumption, incapability of on-line detection and the like of the bromide ions in the water body in the prior art, the invention provides a method for quickly, qualitatively and quantitatively analyzing the trace bromide ions, which can realize convenient, quick, low-cost, high-sensitivity and high-stability detection of the bromide ions in the environment.
The technical scheme of the invention is as follows:
a method for rapidly detecting and analyzing trace bromide ions specifically comprises the following steps:
(1) preparing gold nanoparticle sol by using chloroauric acid solution to form an SERS enhanced substrate;
(2) bromide ions in the water are strongly adsorbed on the surface of the gold nanoparticle sol by forming Au-Br bonds;
(3) adding high-concentration inorganic salt to induce the gold nanoparticle sol to agglomerate to form a solution to be detected;
(4) performing Raman spectrum detection on the solution to be detected to be 178cm-1And qualitatively and quantitatively detecting the bromide ions in the sample to be detected by taking the characteristic Raman peaks of the Au-Br as the reference.
Further, the particle size of the gold nano-ions in the gold nanoparticle sol in the step (1) is adjustable within the range of 15-150 nm.
Further, the high-concentration inorganic salt in the step (3) is a halogen salt solution with sodium and potassium ions as cations and with a concentration of 0.5-3M.
Further, the specific method for detecting the raman spectrum in (4) is as follows: and putting the gold nanoparticle sol into a 96-hole plate, adding a solution containing bromide ions to be monitored, finally adding a high-concentration inorganic salt solution to form a mixed solution to be detected, and then putting the mixed solution into a Raman spectrometer for detection.
Further, the high-concentration inorganic salt and the gold nanoparticle sol are added according to the volume ratio of 1: 1; the solution containing bromide ions and the gold nanoparticle sol are added according to the volume ratio of 10: 1.
The invention has the beneficial effects that:
(1) the SERS method for rapidly detecting and analyzing the trace bromide ions, provided by the invention, simultaneously explores the detection sensitivity of the trace bromide ionsThe lowest detectable concentration is 10-7And M can be used for quantitative and qualitative detection of trace bromide ions in the water body.
(2) The SERS method provided by the invention has the advantages of simplicity, convenience, rapidness, low cost, high stability and the like for detecting trace bromide ions in water, and meanwhile, the portable Raman spectrometer is convenient for on-line monitoring and has potential market value.
Drawings
Fig. 1 is a raman spectrum corresponding to bromide ions of different concentrations in a bromide ion detection method established in an embodiment disclosed in the present invention;
FIG. 2 is a graph of Bromide SERS signal intensity as a function of concentration, as established in the disclosed example.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific examples, which are given by way of illustration only and are not to be construed as limiting the invention; unless otherwise specified, the reagent raw materials used in the following examples are biochemical reagent raw materials which are conventionally commercially available or commercially available, and the laboratory instruments used are laboratory conventional instruments, and unless otherwise specified, the methods and apparatuses used in the following examples are those conventionally used in the art.
Preparation of reagents:
sodium bromide (analytically pure) and sodium sulfate (analytically pure) are all produced by chemical reagents of national drug group limited; polystyrene 96 well plates for detection (Corning, usa);
preparing an instrument:
example 1 detection method of Bromide ions in Water
A method for rapidly detecting and analyzing trace bromide ions specifically comprises the following steps:
(1) preparing gold nanoparticle sol to form an SERS enhanced substrate, wherein the particle size of gold nanoparticles in the gold nanoparticle sol is within the range of 15-150 nm;
(2) bromide ions are strongly adsorbed on the surface of the gold nanoparticle sol by forming Au-Br bonds;
(3) adding high-concentration inorganic salt to induce gold nanoparticle sol to agglomerate; wherein the high-concentration inorganic salt is a halogen salt solution with the concentration of 0.5-3M and taking sodium and potassium ions as cations;
(4) performing Raman spectrum detection on the solution to be detected to be 178cm-1And qualitatively and quantitatively detecting the bromide ions in the sample to be detected by taking the characteristic Raman peaks of the Au-Br as the reference.
Further, the preparation method of the gold nanoparticle sol in the step (1) comprises the following steps: placing 50mL of 0.06% (m/v) chloroauric acid solution into a 100mL double-mouth round-bottom flask, continuously stirring the solution at the rotating speed of 1500r/min, heating to boil for 3-5min, rapidly adding 3mL of 1% (m/v) trisodium citrate solution, gradually changing the solution from golden yellow to colorless to wine red, keeping boiling for 15min, stopping heating, stirring and cooling to room temperature to prepare gold sol, transferring the gold sol into a 50mL centrifuge tube, and storing in a refrigerator at 4 ℃ for storage.
Further, the principle of bromine ion adsorption on the surface of the gold nanoparticle sol in the step (2) is as follows:
further, the specific method for detecting the raman spectrum in the step (4) is as follows: placing the gold nanoparticle sol in a 96-hole plate, adding a solution containing bromide ions to be monitored, finally adding a sodium sulfate solution to form a mixed solution to be detected, and then placing the mixed solution in a Raman spectrometer for detection; adding the sodium sulfate solution and the gold nanoparticle sol according to the volume ratio of 1: 1; adding the solution containing bromide ions and the gold nanoparticle sol according to the volume ratio of 10: 1.
Example 2 Bromide ion detection sensitivity test
First, the concentrations were 1M and 10M, respectively-1M、10-2M、10-3M、10-4M、10-5M、10-6M、10-7M、10-8M、10-9M sodium bromide solutions with different concentration gradients are shaken by hand and mixed evenly;
secondly, preparing gold nanoparticle sol according to the method in example 1 to form an SERS enhancing substrate;
then, taking 20 mu L of gold nanoparticle sol, adding the gold nanoparticle sol into a 96-well plate, respectively taking 200 mu L of sodium bromide solutions with different concentrations as detection samples, adding the detection samples into the 96-well plate, and finally adding the high-concentration inorganic salt into the 96-well plate by selecting 20 mu L of sodium sulfate solution to form a mixed solution to be detected;
finally, the mixed solution to be tested is placed in a Raman spectrometer to obtain a Raman diagram as shown in figure 1 at 178cm-1Is a characteristic Raman peak of bromide ion with a lowest detectable concentration of 10-7And M, performing qualitative and quantitative analysis on the bromide ions in the sample to be detected.
Referring to FIG. 2, it can be seen that when the concentration of bromide ions in the water is 10-5～10-4And when M is used, the intensity of the SERS signal of the bromide ion is strongest, and the detection effect is most obvious.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. A method for rapidly detecting and analyzing trace bromide ions specifically comprises the following steps:
(1) preparing gold nanoparticle sol by using chloroauric acid solution to form an SERS enhanced substrate;
(2) bromide ions in the water are strongly adsorbed on the surface of the gold nanoparticle sol by forming Au-Br bonds;
(3) adding high-concentration inorganic salt to induce the gold nanoparticle sol to agglomerate to form a solution to be detected;
(4) performing Raman spectrum detection on the solution to be detected to be 178cm-1Left and right Au-Br teAnd qualitatively and quantitatively detecting the bromide ions in the sample to be detected by taking the characteristic Raman peak as a reference.
2. The method for rapidly detecting and analyzing the trace bromide ions according to claim 1, which is characterized in that: the particle size of gold nano ions in the gold nano particle sol in the step (1) is adjustable within the range of 15-150 nm.
3. The method for rapidly detecting and analyzing the trace bromide ions according to claim 1, which is characterized in that: and (3) the high-concentration inorganic salt is a halogen salt solution with the concentration of 0.5-3M and taking sodium and potassium ions as cations.
4. The method for rapidly detecting and analyzing the trace bromide ions according to claim 1, which is characterized in that: the specific method for detecting the Raman spectrum in the step (4) is as follows: and putting the gold nanoparticle sol into a 96-hole plate, adding a solution containing bromide ions to be monitored, finally adding a high-concentration inorganic salt solution to form a mixed solution to be detected, and then putting the mixed solution into a Raman spectrometer for detection.
5. The method for rapidly detecting and analyzing the trace bromide ions according to claim 4, wherein the method comprises the following steps: the high-concentration inorganic salt solution and the gold nanoparticle sol are added according to the volume ratio of 1: 1; the solution containing bromide ions and the gold nanoparticle sol are added according to the volume ratio of 10: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166817A (en) * | 2021-11-22 | 2022-03-11 | 国网福建省电力有限公司 | Method for rapidly, qualitatively and quantitatively analyzing trace chloride ions |
| CN114184592A (en) * | 2021-11-24 | 2022-03-15 | 厦门大学 | Electronegative molecule SERS detection method based on electronegative SERS substrate |
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