CN113092399A - Standard substance for ultraviolet visible region wavelength calibration and preparation method and application thereof - Google Patents
Standard substance for ultraviolet visible region wavelength calibration and preparation method and application thereof Download PDFInfo
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- CN113092399A CN113092399A CN202110363326.0A CN202110363326A CN113092399A CN 113092399 A CN113092399 A CN 113092399A CN 202110363326 A CN202110363326 A CN 202110363326A CN 113092399 A CN113092399 A CN 113092399A
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- Prior art keywords
- ultraviolet
- standard substance
- wavelength calibration
- visible region
- oxide
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- 239000000126 substance Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title abstract description 20
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 48
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims abstract description 28
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 13
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002835 absorbance Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 28
- 238000001514 detection method Methods 0.000 description 16
- 238000004090 dissolution Methods 0.000 description 12
- 239000013307 optical fiber Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 4
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001954 samarium oxide Inorganic materials 0.000 description 1
- 229940075630 samarium oxide Drugs 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940075624 ytterbium oxide Drugs 0.000 description 1
Images
Classifications
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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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- 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
- G01N2001/2893—Preparing calibration standards
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/127—Calibration; base line adjustment; drift compensation
Abstract
The invention provides a standard substance for ultraviolet and visible region wavelength calibration, a preparation method and an application thereof, wherein the standard substance for ultraviolet and visible region wavelength calibration comprises, by weight, 20-80 parts of holmium oxide, 6-24 parts of neodymium oxide and an acid solution. The standard substance for ultraviolet visible region wavelength calibration provided by the invention has the advantages of wide application range, wide wavelength coverage range, narrower half width of an absorption peak, more accurate peak positioning and conveniently adjustable absorbance.
Description
Technical Field
The invention belongs to the field of standard substances, particularly relates to a standard substance for ultraviolet visible region wavelength calibration, a preparation method and application thereof, and particularly relates to a standard substance for ultraviolet visible region wavelength calibration with a wide application range, a preparation method and application thereof.
Background
At present, wavelength indication errors of an ultraviolet visible light region can be calibrated only by combining holmium oxide solution/holmium oxide filter and praseodymium-neodymium filter for common use, but the peak shape of an absorption peak of the filter is poor, the absorbance cannot be accurately controlled, and the uncertainty cannot meet the requirements of a high-end ultraviolet visible spectrophotometer.
CN105911008B discloses a method for measuring wavelength indicating errors of an ultraviolet-visible spectrophotometer, which can effectively solve the problem of measuring any wavelength indicating error of the ultraviolet-visible spectrophotometer. The method comprises the steps that the wavelength of the optical fiber spectrometer is calibrated, light emitted by an ultraviolet visible spectrophotometer is converged to a light guide inlet of 1-branch 7-path optical fibers after being reflected by a reflector of a 90-degree corner lighting device and condensed by a convex lens, and then the light is guided into the optical fiber spectrometer through the 1-branch 7-path optical fibers; the vertical position of the 90-degree corner lighting device in the cuvette groove is adjusted to enable the spectral energy value of the optical fiber spectrometer to be maximum, the hollow connecting rod is fixed in the pressing cap through screwing the screw, light emitted by the ultraviolet and visible spectrophotometer is guided into the optical fiber spectrometer through the 90-degree corner lighting device and 1-branch 7-path optical fibers for measurement, the difference between the wavelength value of the ultraviolet and visible spectrophotometer and the wavelength peak value measured by the optical fiber spectrometer is a wavelength indication value error, and the method is stable and reliable and high in measurement precision.
The existing calibration method for ultraviolet and visible spectrophotometry needs to combine different filters, and has poor calibration effect. Therefore, how to provide a standard substance with good calibration effect and convenient use becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a standard substance for ultraviolet visible region wavelength calibration and a preparation method and application thereof, and particularly provides a standard substance for ultraviolet visible region wavelength calibration with a wide application range and a preparation method and application thereof. The standard substance for ultraviolet visible region wavelength calibration provided by the invention has the advantages of wide application range, wide wavelength coverage range, narrower half width of an absorption peak, more accurate peak positioning and conveniently adjustable absorbance.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a standard substance for ultraviolet and visible wavelength calibration, which comprises, by weight, 20-80 parts of holmium oxide, 6-24 parts of neodymium oxide and an acid solution.
The holmium oxide may be present in an amount of 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts, etc., and the neodymium oxide may be present in an amount of 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, etc., but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical ranges are also applicable.
Compared with the traditional method for calibrating the solution and the optical filter in a matched manner, the method has the advantages that the holmium oxide and the neodymium oxide are uniformly dispersed and are closer to the actual sample for daily detection, the influence of the matrix effect on the calibration result can be effectively reduced, the calibration steps are saved, and the cost is lower; the application range is wide, and the method can be applied to ultraviolet-visible spectrophotometers with different resolutions; meanwhile, the wavelength coverage range is wide, and the calibration can be carried out between 200 and 900 nm; the half width of an absorption peak is narrower, the peak positioning is more accurate, the uncertainty is lower, and the absorbance can be conveniently adjusted.
Preferably, the standard substance for ultraviolet and visible wavelength calibration comprises 30-50 parts of holmium oxide, 10-14 parts of neodymium oxide and an acid solution in parts by weight.
Preferably, the acid comprises perchloric acid and/or sulfuric acid.
Preferably, the mass fraction of acid in the acid solution is 8-12%.
Preferably, the concentration of the holmium oxide is 20-80 g/L.
Preferably, the concentration of the holmium oxide is 30-50 g/L.
Preferably, the concentration of the neodymium oxide is 6-24 g/L.
Preferably, the concentration of the neodymium oxide is 10-14 g/L.
The acid content may be 8%, 9%, 10%, 11%, 12%, etc., the holmium oxide concentration may be 20g/L, 30g/L, 40g/L, 50g/L, 60g/L, 70g/L, 80g/L, etc., and the neodymium oxide concentration may be 6g/L, 8g/L, 10g/L, 12g/L, 14g/L, 16g/L, 18g/L, 20g/L, 22g/L, 24g/L, etc., but is not limited to the above-listed values, and other values not listed in the above-mentioned range of values are also applicable.
In a second aspect, the present invention provides a method for preparing the standard substance for ultraviolet-visible wavelength calibration as described above, the method comprising the steps of: mixing and stirring holmium oxide, neodymium oxide and an acid solution to obtain the standard substance for wavelength calibration in the ultraviolet and visible region.
In a third aspect, the present invention also provides the use of the standard substance for ultraviolet-visible wavelength calibration as described above for calibrating an ultraviolet-visible spectrophotometer.
Compared with the prior art, the invention has the following beneficial effects:
compared with the traditional method for calibrating the solution and the optical filter in a matched manner, the method has the advantages that the holmium oxide and the neodymium oxide are uniformly dispersed and are closer to the actual sample for daily detection, the influence of the matrix effect on the calibration result can be effectively reduced, the calibration steps are saved, and the cost is lower; the application range is wide, and the method can be applied to ultraviolet-visible spectrophotometers with different resolutions; meanwhile, the wavelength coverage range is wide, and the calibration can be carried out between 200 and 900 nm; the half width of an absorption peak is narrower, the peak positioning is more accurate, the uncertainty is lower, and the absorbance can be conveniently adjusted.
Drawings
FIG. 1 shows the results of detection of a standard substance for ultraviolet-visible wavelength calibration provided in example 1;
FIG. 2 is the result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in example 2;
FIG. 3 shows the results of detection of a standard substance for ultraviolet-visible wavelength calibration provided in example 3;
FIG. 4 shows the results of detection of a standard substance for ultraviolet-visible wavelength calibration provided in example 4;
FIG. 5 shows the results of detection of a standard substance for ultraviolet-visible wavelength calibration provided in example 5;
FIG. 6 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 1;
FIG. 7 is a result of detection of the standard substance for ultraviolet-visible wavelength calibration provided in comparative example 2;
FIG. 8 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 3;
FIG. 9 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 4;
FIG. 10 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 5;
FIG. 11 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 6;
FIG. 12 is a result of detection of a standard substance for ultraviolet-visible wavelength calibration provided in comparative example 7;
fig. 13 is a result of detection of a certain commercially available holmium oxide filter provided in comparative example 8;
fig. 14 is a result of detection of a commercially available praseodymium neodymium filter provided in comparative example 9.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a standard substance for ultraviolet and visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 40g of holmium oxide and 12g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Example 2
The embodiment provides a standard substance for ultraviolet and visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 50g of holmium oxide and 10g of neodymium oxide in 8% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Example 3
The embodiment provides a standard substance for ultraviolet and visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 30g of holmium oxide and 14g of neodymium oxide in a perchloric acid solution with the mass fraction of 12%, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Example 4
The embodiment provides a standard substance for ultraviolet and visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 80g of holmium oxide and 60g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Example 5
The embodiment provides a standard substance for ultraviolet and visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 20g of holmium oxide and 24g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 1
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 10g of holmium oxide and 30g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 2
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 90g of holmium oxide and 3g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 3
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 52g of holmium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet-visible region wavelength calibration.
Comparative example 4
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 52g of neodymium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 5
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and dissolving 52g of ytterbium oxide in 10 mass percent perchloric acid solution, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 6
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 52g of cerium oxide in 10% perchloric acid solution by mass fraction, and after complete dissolution, metering the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 7
The comparative example provides a standard substance for ultraviolet visible region wavelength calibration, and the preparation method comprises the following steps:
and (3) dissolving 52g of samarium oxide in a perchloric acid solution with the mass fraction of 10%, and after complete dissolution, fixing the volume to 1L to obtain the standard substance for ultraviolet visible region wavelength calibration.
Comparative example 8
Certain commercially available holmium oxide filters.
Comparative example 9
A praseodymium neodymium filter is commercially available.
And (3) performance testing:
testing an instrument: uv-vis spectrophotometer, manufacturer: agilent, model number CARY6000 i.
The testing steps are as follows:
1. the uv-vis spectrophotometer was preheated for 30 minutes.
2. A scan setup is performed. (spectral bandwidth: 2nm, scanning range: 200-
3. And (6) correcting an air baseline.
4. And (4) putting the solution to be detected into a cuvette, and putting the cuvette into a sample chamber for scanning.
5. And obtaining a corresponding scanning spectrogram.
The standard substances and filters provided in examples 1 to 5 and comparative examples 1 to 9 were examined, and the results are shown in FIGS. 1 to 14.
As can be seen from the figure, the standard substance for ultraviolet visible region wavelength calibration provided by the invention can cover the range of 200-900nm, can complete large-range calibration at one time, does not need to replace the calibration material for many times, and reduces the calibration steps; comparing example 1 with comparative examples 8-9, it can be seen that, compared with the prior art, the standard substance for ultraviolet visible region wavelength calibration provided by the invention has lower absorbance, can be suitable for the calibration of ultraviolet visible spectrophotometers with different resolutions, and meanwhile, the half width of the absorption peak is narrower, the peak positioning is more accurate, and the uncertainty is lower; comparing example 1 with comparative examples 3-7, it can be found that the invention covers the calibration range of 200-900nm by compounding and combining holmium oxide and neodymium oxide, can meet the calibration requirements of different ranges, and has significant advantages.
The applicant states that the present invention is illustrated by the above examples to show the standard substance for ultraviolet and visible wavelength calibration of the present invention, and the preparation method and application thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. The standard substance for ultraviolet and visible wavelength calibration is characterized by comprising 20-80 parts by weight of holmium oxide, 6-24 parts by weight of neodymium oxide and an acid solution.
2. The standard substance for ultraviolet-visible wavelength calibration as set forth in claim 1, wherein the standard substance for ultraviolet-visible wavelength calibration comprises 30 to 50 parts by weight of holmium oxide, 10 to 14 parts by weight of neodymium oxide, and an acid solution.
3. The standard substance for ultraviolet-visible wavelength calibration according to claim 1 or 2, wherein the acid comprises perchloric acid and/or sulfuric acid.
4. The standard substance for ultraviolet-visible wavelength calibration as set forth in any one of claims 1 to 3, wherein the acid solution has an acid mass fraction of 8 to 12%.
5. The standard substance for ultraviolet-visible wavelength calibration as set forth in any one of claims 1 to 4, wherein the holmium oxide has a concentration of 20 to 80 g/L.
6. The standard substance for ultraviolet-visible wavelength calibration as set forth in any one of claims 1 to 5, wherein the holmium oxide has a concentration of 30 to 50 g/L.
7. The standard substance for ultraviolet-visible wavelength calibration according to any one of claims 1 to 6, wherein the concentration of the neodymium oxide is 6 to 24 g/L.
8. The standard substance for ultraviolet-visible wavelength calibration according to any one of claims 1 to 6, wherein the concentration of the neodymium oxide is 10 to 14 g/L.
9. A method for preparing a standard substance for ultraviolet-visible wavelength calibration according to any one of claims 1 to 8, comprising the steps of: mixing and stirring holmium oxide, neodymium oxide and an acid solution to obtain the standard substance for wavelength calibration in the ultraviolet and visible region.
10. Use of the standard substance for ultraviolet-visible wavelength calibration according to any one of claims 1 to 8 for calibrating an ultraviolet-visible spectrophotometer.
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