CN112557146A - Method for measuring content of amino PEG (polyethylene glycol) -coated nano iron oxide - Google Patents
Method for measuring content of amino PEG (polyethylene glycol) -coated nano iron oxide Download PDFInfo
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- CN112557146A CN112557146A CN202011589830.4A CN202011589830A CN112557146A CN 112557146 A CN112557146 A CN 112557146A CN 202011589830 A CN202011589830 A CN 202011589830A CN 112557146 A CN112557146 A CN 112557146A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 title claims abstract description 15
- 239000002202 Polyethylene glycol Substances 0.000 title abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 title abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 41
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052742 iron Inorganic materials 0.000 claims abstract description 27
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- -1 iron ions Chemical class 0.000 claims abstract description 18
- 239000012488 sample solution Substances 0.000 claims abstract description 14
- 238000002835 absorbance Methods 0.000 claims abstract description 13
- 239000012085 test solution Substances 0.000 claims abstract description 12
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000523 sample Substances 0.000 claims abstract description 11
- 239000007974 sodium acetate buffer Substances 0.000 claims abstract description 10
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims abstract description 10
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000012086 standard solution Substances 0.000 claims abstract description 6
- 238000000209 wet digestion Methods 0.000 claims abstract description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 230000001079 digestive effect Effects 0.000 claims description 3
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000005728 strengthening Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000007865 diluting Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
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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
-
- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the content of amino PEG (polyethylene glycol) -coated nano ferric oxide, which comprises the following steps: digesting the sample by a wet digestion method to eliminate interference of organic solvents and other organic matters; reducing the iron ions into ferric ions by using hydroxylamine hydrochloride test solution; adjusting the pH value of the solution by using an acetic acid-sodium acetate buffer solution; developing iron ions by using phenanthroline test solution to obtain a sample solution; performing the same operation by using iron ion standard solutions with different concentrations to obtain a linear solution; detecting the absorbance of the sample solution and the linear solution by using an ultraviolet spectrophotometer; taking the concentration of the iron ion standard solution and the absorbance of the linear solution as a linear equation; and calculating the iron ion concentration of the sample solution according to a linear equation and the absorbance of the sample solution. The invention digests the sample, converts iron into an inorganic state, eliminates the interference of an organic solvent, and improves the detection accuracy by using the method as a linear equation.
Description
Technical Field
The invention relates to a method for measuring the content of amino PEG (polyethylene glycol) -coated nano ferric oxide, belonging to the technical field of analysis and detection.
Background
When an ultraviolet spectrophotometer is used for detecting the content of the amino PEG-coated nano iron oxide, the accuracy of the determination is not high due to factors such as incomplete iron ion digestion, interference of an organic solvent and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the method for measuring the content of the amino PEG-coated nano ferric oxide, so that the interference of an organic solvent is eliminated, and the detection accuracy is improved.
In order to solve the technical problem, the invention provides a method for measuring the content of amino PEG-coated nano ferric oxide, which comprises the following steps:
digesting the sample by a wet digestion method to eliminate interference of organic solvents and other organic matters;
reducing the iron ions into ferric ions by using hydroxylamine hydrochloride test solution;
adjusting the pH value of the solution by using an acetic acid-sodium acetate buffer solution;
developing iron ions by using phenanthroline test solution to obtain a sample solution;
performing the same operation by using iron ion standard solutions with different concentrations to obtain a linear solution;
detecting the absorbance of the sample solution and the linear solution by using an ultraviolet spectrophotometer;
taking the concentration of the iron ion standard solution and the absorbance of the linear solution as a linear equation;
and calculating the iron ion concentration of the sample solution according to a linear equation and the absorbance of the sample solution.
Preferably, the wet digestion method is: adding concentrated nitric acid into the sample, uniformly mixing, adding concentrated sulfuric acid, gradually strengthening fire, keeping a micro-boiling state, and continuously adding concentrated nitric acid dropwise until the solution is transparent and does not turn black; when the solution becomes deep, adding nitric acid immediately; after the solution is not blackened any more, heating is continued for a few minutes until dense white smoke is emitted, and at the moment, the digestive juice is clear and transparent.
Preferably, in the initial reaction stage, the volume ratio of the sample, the concentrated nitric acid and the concentrated sulfuric acid is 1: 20: 10.
preferably, the volume ratio of the hydroxylamine hydrochloride test solution to the acetic acid-sodium acetate buffer solution is 1: 1.
Preferably, the pH value of the solution is adjusted to 2-9 by using an acetic acid-sodium acetate buffer solution.
Preferably, the concentration of the phenanthroline test solution is 0.15%.
Preferably, the absorbance of the sample solution and the linear solution is measured with an ultraviolet spectrophotometer at a wavelength of 510 nanometers.
The invention achieves the following beneficial effects: the method digests the sample, converts iron into an inorganic state, eliminates the interference of an organic solvent, ensures that hydroxylamine hydrochloride and iron completely react, uses an acetic acid-sodium acetate buffer solution to adjust the pH value, eliminates the error of the color development strength of the phenanthroline solution and iron ions under different pH conditions, and improves the detection accuracy by using the method as a linear equation.
Drawings
FIG. 1 is a linear equation diagram of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Preparation of a required solution:
dilute hydrochloric acid: 234ml of hydrochloric acid is taken and diluted to 1000ml by adding water, thus obtaining the compound. The liquid containing HC1 should be 9.5-10.5%.
Dilute nitric acid: taking 105ml of nitric acid, adding water to dilute to 1000ml, and obtaining the nitric acid. The liquid contains HN 03-10.5%
Acetic acid-sodium acetate buffer (ph 4.6): dissolving sodium acetate 5.4g in water 50ml, adjusting pH to 4.6 with glacial acetic acid, and diluting with water to 100 ml.
Hydroxylamine hydrochloride test solution: 3.5g of hydroxylamine hydrochloride is taken and dissolved into 100ml by adding 60 percent ethanol, thus obtaining the product.
0.15% of phenanthroline: 0.15g of the product is taken and diluted to 100ml by water, and the product is prepared immediately after use.
The method for measuring the content of the amino PEG coated nano ferric oxide comprises the following steps:
(1) taking a standard iron solution, diluting the standard iron solution into a solution containing 0.05mg/ml, 0.1mg/ml, 0.15mg/ml, 0.2mg/ml and 0.25mg/ml of iron, precisely measuring 1ml, adding 1ml of dilute hydrochloric acid into a 50ml volumetric flask, carrying out water bath at 80 ℃ for 5min, adding 5ml of hydroxylamine hydrochloride test solution, and shaking up; then adding 5ml acetic acid-sodium acetate buffer salt (pH 4.6) and 2ml0.15% o-phenanthroline for color development, diluting with water to scale, measuring absorbance at 510nm wavelength, calculating linear regression equation by using iron concentration and absorbance, and the correlation coefficient (r) should not be less than 0.99. (see FIG. 1)
(2) Precisely measuring 1mL of a sample to be tested, putting the sample into a 100mL Kjeldahl bottle, adding 20 mL of concentrated nitric acid, carefully and uniformly mixing, adding 10 mL of concentrated sulfuric acid, gradually adding strong fire, keeping a slightly boiling state, and continuously adding the concentrated nitric acid dropwise until the solution is transparent and does not turn black. Nitric acid is added immediately whenever the solution becomes dark, otherwise the digestion will be incomplete. And after the solution is not blackened any more, continuing heating for a plurality of minutes until dense white smoke is emitted, and clarifying and transparent the digestive juice at the moment. After the digest had cooled down, it was carefully diluted with water and transferred to the volumetric flask, while the Kjeldahl flask was washed with water, the wash was incorporated into the volumetric flask and diluted to the mark. An additional 1ml of the solution diluted to about 0.2mg/ml iron was taken and the iron ion concentration was calculated as a linear equation, operating with a standard iron solution.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for measuring the content of amino PEG coated nano ferric oxide is characterized by comprising the following steps:
digesting the sample by a wet digestion method to eliminate interference of organic solvents and other organic matters;
reducing the iron ions into ferric ions by using hydroxylamine hydrochloride test solution;
adjusting the pH value of the solution by using an acetic acid-sodium acetate buffer solution;
developing iron ions by using phenanthroline test solution to obtain a sample solution;
performing the same operation by using iron ion standard solutions with different concentrations to obtain a linear solution;
detecting the absorbance of the sample solution and the linear solution by using an ultraviolet spectrophotometer;
taking the concentration of the iron ion standard solution and the absorbance of the linear solution as a linear equation;
and calculating the iron ion concentration of the sample solution according to a linear equation and the absorbance of the sample solution.
2. The method for measuring the content of the amino PEG coated nano iron oxide according to claim 1, wherein the wet digestion method comprises the following steps: adding concentrated nitric acid into the sample, uniformly mixing, adding concentrated sulfuric acid, gradually strengthening fire, keeping a micro-boiling state, and continuously adding concentrated nitric acid dropwise until the solution is transparent and does not turn black; when the solution becomes deep, adding nitric acid immediately; after the solution is not blackened any more, heating is continued for a few minutes until dense white smoke is emitted, and at the moment, the digestive juice is clear and transparent.
3. The method for measuring the content of the amino PEG coated nano ferric oxide according to claim 2, wherein in the initial reaction stage, the volume ratio of the sample, the concentrated nitric acid and the concentrated sulfuric acid is 1: 20: 10.
4. the method for measuring the content of the amino PEG-coated nano ferric oxide according to claim 1, wherein the volume ratio of the hydroxylamine hydrochloride test solution to the acetic acid-sodium acetate buffer solution is 1: 1.
5. The method for measuring the content of the amino PEG-coated nano ferric oxide according to claim 1, wherein the pH of the solution is adjusted to 2-9 by acetic acid-sodium acetate buffer solution.
6. The method for measuring the content of the amino PEG-coated nano ferric oxide according to claim 1, wherein the concentration of the phenanthroline test solution is 0.15%.
7. The method for measuring the content of the amino PEG coated nano ferric oxide according to claim 1, characterized in that an ultraviolet spectrophotometer is used for detecting the absorbance of the sample solution and the linear solution at the wavelength of 510 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011589830.4A CN112557146A (en) | 2020-12-28 | 2020-12-28 | Method for measuring content of amino PEG (polyethylene glycol) -coated nano iron oxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011589830.4A CN112557146A (en) | 2020-12-28 | 2020-12-28 | Method for measuring content of amino PEG (polyethylene glycol) -coated nano iron oxide |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006317247A (en) * | 2005-05-12 | 2006-11-24 | Wako Pure Chem Ind Ltd | Iron concentration measuring method |
| CN102565045A (en) * | 2011-12-28 | 2012-07-11 | 新疆众和股份有限公司 | Determination method of trace iron in aluminum-containing phosphoric acid solution and aluminum masking agent therefor |
| CN104422665A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Method for detecting content of phosphorus and iron in LiFePO4/C composite material |
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2020
- 2020-12-28 CN CN202011589830.4A patent/CN112557146A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006317247A (en) * | 2005-05-12 | 2006-11-24 | Wako Pure Chem Ind Ltd | Iron concentration measuring method |
| CN102565045A (en) * | 2011-12-28 | 2012-07-11 | 新疆众和股份有限公司 | Determination method of trace iron in aluminum-containing phosphoric acid solution and aluminum masking agent therefor |
| CN104422665A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Method for detecting content of phosphorus and iron in LiFePO4/C composite material |
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| 夏玉宇: "《化验员实用手册》", 31 March 1999, 化学工业出版社 * |
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Application publication date: 20210326 |