Near-infrared wavelength standard substance and preparation method thereof
Patent Information
- Application Number
- CN202311247189.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-26
- Publication Date
- 2026-10-30
- Estimated Expiration
- 2043-09-26
AI Technical Summary
该标物是将稀土元素和聚苯乙烯融合在一起制成的滤光片用以弥补SRM 2035b以及GBW(E)130551从2000～2600nm处的吸收峰，但聚苯乙烯在近红外取的吸收峰形并不理想，导致此滤光片在近红外区的峰形欠佳难以精准定位峰值波长
[0037]1、本发明提供的近红外波长标准物质可以完整覆盖近红外光区(900-2600nm)，并且吸收峰的半峰宽较玻璃滤光片更窄，峰定位更准确；
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Figure CN117309803B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of infrared detection technology, specifically relating to a near-infrared wavelength standard substance and its preparation method. Background Technology
[0002] Near-infrared (NIR) light is electromagnetic radiation falling between the visible and mid-infrared regions. Different literatures define its wavelength range differently, but the American Society for Testing and Materials (ASTM) specifies it as 780–2526 nm. Each specific NIR spectrometer has an effective spectral range, which depends primarily on the instrument's optical path design, detector type, and light source. The wavelength range of NIR spectrometers is typically divided into two segments: the short-wavelength NIR spectral region of 700–1100 nm and the long-wavelength NIR spectral region of 1100–2500 nm.
[0003] Since the first commercial near-infrared spectrometer was introduced in 1954, researchers have actively promoted and used this spectroscopic technology in various fields. During this period, a large number of experiments were conducted to analyze the absorption bands of various substances in the near-infrared region. At the same time, by combining the results of the mid-infrared material composition characteristic absorption spectrum analysis, the experimental observation results were compared with the theoretical calculation results, which can more accurately analyze the near-infrared overtone and combination absorption spectra of many substances.
[0004] The near-infrared spectral region coincides with the absorption regions of the combination frequencies and overtones of the vibrations of hydrogen-containing groups (OH, NH, CH) in organic molecules. By scanning the near-infrared spectrum of a sample, characteristic information of hydrogen-containing groups in organic molecules in the sample can be obtained. Moreover, the near-infrared spectroscopy technique for analyzing samples has advantages such as being convenient, fast, efficient, accurate, and low-cost. It does not damage the sample, consume chemical reagents, or pollute the environment. Therefore, this technique is increasingly favored by many people.
[0005] However, near-infrared spectroscopy suffers from problems such as wide spectral bandwidth, severe peak overlap, and weak absorption signals. It is difficult to find standard materials with sharp absorption peaks and abundant absorption peaks in the near-infrared spectral range to calibrate the wavelength in the near-infrared region.
[0006] Currently, the most commonly used standard reference material internationally is SRM 2035b from the National Institute of Standards and Technology (NIST). This standard reference material has peak wavelengths of 975.8 nm, 1075.6 nm, 1151.5 nm, 1222.2 nm, 1366.8 nm, 1469.1 nm, and 1945.7 nm. This standard reference material is an absorption filter made using the absorption of rare earth elements in the near-infrared region. However, due to the absorption characteristics of rare earth elements, the measurement range cannot be extended to around 2500 nm.
[0007] Currently, commonly used near-infrared wavelength standard materials in China include:
[0008] GBW(E)130446 has peak wavelengths of 1016.4nm, 1364.8nm, 1717.4nm, 1981.2nm, and 2291.3nm. This standard is an interference filter, with each filter corresponding to a single peak wavelength, resulting in a total of five wavelength values. The number of wavelength points is relatively small, and the peak wavelength stability of the interference filter is not very good. Furthermore, the peak wavelength of the interference filter changes with the incident angle of the incident light, making it easy to obtain poor test results if the test cannot be performed under conditions of perpendicular incident parallel light. At the same time, the calibration instrument is cumbersome to use, requiring repeated operation and filter changes.
[0009] GBW(E)130551 has peak wavelengths of 1068.3 nm, 1220.5 nm, 1362.9 nm, 1464.6 nm, 1524.0 nm, and 1939.0 nm. This standard is similar to NIST's SRM 2035b, being an absorption filter made using the absorption of rare earth elements in the near-infrared region, and its characteristics are also similar to SRM 2035b.
[0010] GBW(E)130550 has near-infrared peak wavelengths of 1228.3 nm, 1364.9 nm, 1679.6 nm, 1906.2 nm, 1948.1 nm, 2135.4 nm, 2253.6 nm, and 2537.2 nm. This standard is a filter made by fusing rare earth elements and polystyrene to compensate for the absorption peaks of SRM 2035b and GBW(E)130551 in the 2000–2600 nm range. However, the absorption peak shape of polystyrene in the near-infrared region is not ideal, resulting in poor peak shape and difficulty in accurately locating the peak wavelength in the near-infrared region of this filter.
[0011] Therefore, developing a solution standard substance for calibration wavelengths that can cover the near-infrared region, and whose absorption peaks have a narrower half-width, more accurate peak positioning, and superior peak shape and number, is a key research focus in this field. Summary of the Invention
[0012] To address the shortcomings of existing technologies, the present invention aims to provide a near-infrared wavelength standard material and its preparation method.
[0013] To achieve this objective, the present invention employs the following technical solution:
[0014] In a first aspect, the present invention provides a near-infrared wavelength standard material, characterized in that the raw materials of the near-infrared wavelength standard material include a solute and a solvent; the solute is a halogenated phenol, and the solvent is a halogenated olefin.
[0015] Preferably, the halogenated phenol includes monohalogen substitution, dihalogen substitution, trihalogen substitution, tetrahalogen substitution, or pentahalogen substitution.
[0016] Preferably, the halogenated phenol is trihalogenated.
[0017] Preferably, the halogen in the halophenol includes any one or a combination of at least two of fluorine, chlorine, or bromine.
[0018] Preferably, the halogen in the halogenated phenol is chlorine.
[0019] Preferably, the halogenated phenol is 2,4,5-trichlorophenol.
[0020] Preferably, the halogenated olefin includes monohalogen substitution, dihalogen substitution, trihalogen substitution, or tetrahalogen substitution.
[0021] Preferably, the olefin in the haloolefin is ethylene.
[0022] Preferably, the halogen in the haloolefin includes any one or a combination of at least two of fluorine, chlorine, or bromine.
[0023] Preferably, the halogen in the haloolefin is chlorine.
[0024] Preferably, the haloolefin is tetrachloroethylene.
[0025] Preferably, the half-width at half maximum (WHM) of the near-infrared wavelength standard material is ≤12nm, for example, it can be 11nm, 10nm, 9nm, 8nm, etc.
[0026] Preferably, the peak wavelength uncertainty of the near-infrared wavelength standard material is ≤0.5nm, for example, it can be 0.45nm, 0.4nm, 0.35nm, 0.3nm, 0.25nm, 0.2nm, 0.15nm, 0.1nm, etc.
[0027] Preferably, the wavelength range of the near-infrared wavelength standard material is 900-2600nm, for example, it can be 1000nm, 1100nm, 1200nm, 1300nm, 1400nm, 1500nm, 1600nm, 1700nm, 1800nm, 1900nm, 2000nm, 2100nm, 2200nm, 2300nm, 2400nm, 2500nm, etc.
[0028] Preferably, the scanning spectrum of the near-infrared wavelength standard material includes 11 characteristic peaks.
[0029] Preferably, the peak wavelengths of the 11 characteristic peaks are 991-993nm (e.g., 991.2nm, 991.4nm, 991.6nm, 991.8nm, etc.), 1239-1240nm (e.g., 1239.2nm, 1239.4nm, 1239.6nm, 1239.8nm, etc.), and 1448-1449nm (e.g., 1448.2nm, 1448.4nm, etc.). 1448.6nm, 1448.8nm, etc.), 1658-1659nm (e.g., 1658.2nm, 1658.4nm, 1658.6nm, 1658.8nm, etc.), 1958-1959nm (e.g., 1958.2nm, 1958.4nm, 1958.6nm, 1958.8nm, etc.), 2027-2028nm (e.g., 2027... 2027.2nm, 2027.4nm, 2027.6nm, 2027.8nm, etc.), 2069-2070nm (e.g., 2069.2nm, 2069.4nm, 2069.6nm, 2069.8nm, etc.), 2119-2120nm (e.g., 2119.2nm, 2119.4nm, 2119.6nm, 2119.8nm, etc.), 2411-2412n m (e.g., 2411.2nm, 2411.4nm, 2411.6nm, 2411.8nm, etc.), 2434-2435nm (e.g., 2434.2nm, 2434.4nm, 2434.6nm, 2434.8nm, etc.), 2540-2541nm (e.g., 2540.2nm, 2540.4nm, 2540.6nm, 2540.8nm, etc.).
[0030] Preferably, the peak wavelengths of the 11 characteristic peaks are 992.0 nm, 1239.1 nm, 1448.8 nm, 1658.2 nm, 1958.2 nm, 2027.7 nm, 2069.5 nm, 2119.3 nm, 2411.1 nm, 2434.4 nm, and 2540.9 nm.
[0031] In a second aspect, the present invention provides a method for preparing a near-infrared wavelength standard substance as described in the first aspect, the method comprising: dissolving a solute in a solvent, the resulting solution being the near-infrared wavelength standard substance.
[0032] Preferably, the preparation method includes: dissolving 2,4,5-trichlorophenol in tetrachloroethylene to obtain the near-infrared wavelength standard material.
[0033] Preferably, the concentration of 2,4,5-trichlorophenol in the near-infrared wavelength standard material is 0.13-0.15 g / mL, for example, it can be 0.135 g / mL, 0.14 g / mL, 0.145 g / mL, etc., preferably 0.14 g / mL.
[0034] The near-infrared wavelength standard material provided by this invention needs to be permanently sealed by heat fusion in a specially designed cuvette. This permanent sealing solves the problem of the toxicity and volatility of organic solutions. Furthermore, because organic solutions are volatile during heat sealing and have low flash and ignition points, the cuvette is specially designed with a layer of quartz at the mouth and a capillary hole in the center. The solution is injected through a syringe needle, which greatly reduces the evaporation of the solution during the sealing process and solves the problem of flammability caused by solution evaporation during heat sealing.
[0035] The numerical range described in this invention includes not only the point values listed above, but also any point values within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values included in the range.
[0036] Compared with the prior art, the present invention has the following beneficial effects:
[0037] 1. The near-infrared wavelength standard material provided by this invention can completely cover the near-infrared light region (900-2600nm), and the half-width of the absorption peak is narrower than that of the glass filter, and the peak positioning is more accurate.
[0038] 2. Compared with existing standard materials, the near-infrared wavelength standard material provided by this invention has more characteristic peaks and better peak shapes, which can meet the requirements of high-end instrument performance evaluation, analytical method evaluation, and quality control of biological, food, pharmaceutical, chemical products and cosmetics. Attached Figure Description
[0039] Figure 1 The image shows the appearance of the sealed near-infrared wavelength standard material in Example 1.
[0040] Figure 2 The absorption spectrum of the near-infrared standard material prepared in Example 1 at wavelengths of 900-2600 nm.
[0041] Figure 3 The absorption spectrum of NIST SRM2035b at wavelengths of 900-2600 nm;
[0042] Figure 4 The absorption spectrum of GBW(E)130550 at wavelengths of 900-2600 nm is shown. Detailed Implementation
[0043] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.
[0044] The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not limited to those elements and may also include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.
[0045] "Optional" or "any one" means that the matter or event described thereafter may or may not occur, and the description includes both the possibility that the event will occur and the possibility that the event will not occur.
[0046] The indefinite articles “a” and “an” preceding an element or component of this invention do not impose any limitation on the quantity (i.e., number of times) of the element or component. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers only to the singular form.
[0047] The terms "one embodiment," "some embodiments," "exemplary," "specific example," or "some examples," etc., used in this invention refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the invention. In this document, the illustrative expressions of the above terms are not necessarily directed at the same embodiment or example.
[0048] The reagents or instruments used in the following examples are from the following sources:
[0049] 2,4,5-Trichlorophenol: Purchased from Sinopharm Chemical Reagent Co., Ltd., CAS: 95-95-4;
[0050] Tetrachloroethylene: Purchased from Sinopharm Chemical Reagent Co., Ltd.;
[0051] NIST SRM2035b: The spectrum is derived from the standard substance certificate published on the NIST website.
[0052] GBW(E)130550: Purchased from the National Standard Material Resource Sharing Platform and produced by the National Institute of Metrology, China.
[0053] Example 1
[0054] This embodiment provides a near-infrared wavelength standard substance, and the preparation method of the near-infrared wavelength standard substance includes the following steps:
[0055] Accurately weigh 7g of 2,4,5-trichlorophenol, dissolve it in tetrachloroethylene, stir, and after it is completely dissolved, make up to 50mL. Inject the solution into a cuvette and heat-seal it permanently to obtain the near-infrared wavelength standard material.
[0056] The appearance of the sealed near-infrared wavelength standard material is shown in the figure below. Figure 1 As shown.
[0057] Test Example 1
[0058] Testing conditions: Agilent CARY 5000 UV-Vis-NIR spectrophotometer, fixed spectral bandwidth of 2nm, scanning interval of 1nm, 6 scans, and the average value after interpolation was taken as the result. Ambient temperature 22℃, relative humidity 63%;
[0059] Test sample: Near-infrared wavelength standard material prepared in Example 1, GBW(E)130550;
[0060] Detection results: The absorption spectrum of the near-infrared standard material prepared in Example 1 at wavelengths of 900-2600 nm is shown below. Figure 2 As shown in the figure, abundant absorption peaks are relatively evenly distributed in the wavelength range from 900nm to 2600nm, with sharp peak shapes. By performing cubic spline interpolation on 5 points near the maximum wavelength of each peak, with a total of 80 interpolations, the peak wavelengths obtained after interpolation are 992.0nm, 1239.1nm, 1448.8nm, 1658.2nm, 1958.2nm, 2027.7nm, 2069.5nm, 2119.3nm, 2411.1nm, 2434.4nm, and 2540.9nm.
[0061] The absorption spectrum of NIST SRM2035b at wavelengths of 900-2600 nm is as follows: Figure 3 As shown, the spectrum is derived from the standard material certificate published on the NIST website. The standard material is an absorption filter made by utilizing the absorption of rare earth elements in the near-infrared region. However, due to the absorption characteristics of rare earth elements, the measurement range cannot be extended to around 2500 nm.
[0062] The absorption spectrum of GBW(E)130550 at wavelengths of 900-2600nm is as follows: Figure 4 As shown, the absorption peak shape of polystyrene in the standard material in the near-infrared region is not ideal, which makes it difficult to accurately locate the peak wavelength in the near-infrared region due to the poor peak shape of this filter.
[0063] As shown in the figure, the peak shape and number of peaks in the 900-2600nm wavelength absorption spectrum of the near-infrared standard material prepared in Example 1 are superior to those of NIST SRM2035b and GBW(E)130550.
[0064] The applicant declares that the present invention is illustrated by the above embodiments, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of the raw materials used in the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims
1. A near-infrared wavelength standard material, characterized in that, The raw materials for the near-infrared wavelength standard material include a solute and a solvent; the solute is a halogenated phenol, and the solvent is a halogenated olefin. The halogenated phenol is 2,4,5-trichlorophenol; The haloolefin is tetrachloroethylene; The concentration of the 2,4,5-trichlorophenol is 0.13-0.15 g / mL; The near-infrared wavelength standard material has 11 characteristic peaks in its scanning spectrum.
2. The near-infrared wavelength standard material according to claim 1, characterized in that, The full width at half maximum (FWHM) of the near-infrared wavelength standard material is ≤12 nm.
3. The near-infrared wavelength standard material according to claim 1, characterized in that, The peak wavelength uncertainty of the near-infrared wavelength standard material is ≤0.5 nm.
4. The near-infrared wavelength standard material according to claim 1, characterized in that, The wavelength range of the near-infrared wavelength standard material is 900-2600 nm.
5. The near-infrared wavelength standard material according to claim 1, characterized in that, The peak wavelengths of the 11 characteristic peaks are 991-993 nm, 1239-1240 nm, 1448-1449 nm, 1658-1659 nm, 1958-1959 nm, 2027-2028 nm, 2069-2070 nm, 2119-2120 nm, 2411-2412 nm, 2434-2435 nm, and 2540-2541 nm.
6. The near-infrared wavelength standard material according to claim 5, characterized in that, The peak wavelengths of the 11 characteristic peaks are 992.0 nm, 1239.1 nm, 1448.8 nm, 1658.2 nm, 1958.2 nm, 2027.7 nm, 2069.5 nm, 2119.3 nm, 2411.1 nm, 2434.4 nm, and 2540.9 nm.
7. A method for preparing a near-infrared wavelength standard material as described in any one of claims 1-6, characterized in that, The preparation method includes: 2,4,5-Trichlorophenol was dissolved in tetrachloroethylene to obtain the near-infrared wavelength standard material; The concentration of 2,4,5-trichlorophenol in the near-infrared wavelength standard material is 0.13-0.15 g / mL.
8. The preparation method according to claim 7, characterized in that, The concentration of 2,4,5-trichlorophenol in the near-infrared wavelength standard material is 0.14 g / mL.
Citation Information
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Improvements relating to the treatment of textiles for protection against biologicalattack
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