Quantitative element detection method for sodium pyroantimonate product
By establishing a standard curve using X-ray fluorescence spectroscopy, the problem of time-consuming sodium pyroantimonate detection was solved, enabling rapid and accurate quantitative elemental detection, simplifying the detection steps and reducing errors.
Patent Information
- Application Number
- CN202511583896.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-31
- Publication Date
- 2026-02-17
AI Technical Summary
Existing methods for detecting sodium pyroantimonate are time-consuming and complex, making it difficult to quickly and accurately quantify elements such as antimony, iron, sodium, lead, and arsenic in products.
X-ray fluorescence spectrometry was used to detect sodium pyroantimonate products by preparing standards, establishing standard curves, calculating concentrations using the gravimetric method, and combining X-ray fluorescence spectrometry analysis.
It enables rapid and accurate quantitative detection of different elements in sodium pyroantimonate products, shortens detection time, simplifies procedures, reduces errors, and is environmentally friendly.
Smart Images
Figure CN121540741A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical detection technology, and in particular to a method for quantitative elemental detection of sodium pyroantimonate products. Background Technology
[0002] Sodium pyroantimonate is an inorganic antimony compound, commonly represented by the molecular formula NaSb(OH)6. It is a safe, stable, and easily processed carrier for antimony. Antimony plays a specific role in many industrial processes, such as clarification in the glass and ceramics industry and catalysis in the production of polyethylene terephthalate. Directly using metallic antimony or other antimony compounds is neither safe nor convenient; sodium pyroantimonate, in its stable salt form, allows for the safe and uniform addition of antimony to various materials.
[0003] In actual industrial production of sodium pyroantimonate, due to the influence of raw material sources and production processes, it is almost impossible for sodium pyroantimonate to achieve 100% purity. It usually contains some impurity elements, such as arsenic, lead, iron, and sodium. The content of these elements directly affects the grade and application fields of sodium pyroantimonate products, thus necessitating elemental analysis. Current technologies for the detection of sodium pyroantimonate generally employ chemical analysis methods. Total antimony content is determined using a cerium sulfate standard titration solution, and iron content is determined using an o-phenanthroline spectrophotometric method. The detection of other elements is time-consuming and complex, requiring nearly two days to complete the overall analysis. Therefore, there is an urgent need for a rapid and accurate method for the quantitative detection of elements in sodium pyroantimonate products. Summary of the Invention
[0004] The main objective of this invention is to propose a method for quantitative elemental detection of sodium pyroantimonate products, aiming to solve the problem of long detection time in existing methods.
[0005] To achieve the above objectives, this invention proposes a method for quantitative elemental detection of sodium pyroantimonate products, comprising: Provide standard samples, which include antimony, iron, sodium, lead, and arsenic. The standard samples were analyzed by X-ray fluorescence spectroscopy to obtain standard curves for antimony, iron, sodium, lead, and arsenic. The sodium pyroantimonate product was tested by X-ray fluorescence spectroscopy, and the contents of antimony, iron, sodium, lead, and arsenic in the sodium pyroantimonate product were determined according to the standard curve.
[0006] Preferably, the standard includes antimony trioxide, ferric oxide, sodium carbonate, lead oxide, and arsenic trioxide.
[0007] Preferably, the standard comprises, by mass percentage: 57.5%–61.2% antimony trioxide, 0.005%–0.12% ferric oxide, 20.2%–22.2% sodium carbonate, 0.02%–1.8% lead oxide, and 0.01%–1.5% arsenic trioxide.
[0008] Preferably, the standard includes boric acid.
[0009] Preferably, the standard comprises 17.23% to 17.98% boric acid by mass percentage.
[0010] Preferably, the standard product includes a first sub-standard product, a second sub-standard product, a third sub-standard product, a fourth sub-standard product, a fifth sub-standard product, a sixth sub-standard product, a seventh sub-standard product, an eighth sub-standard product, and a ninth sub-standard product; By mass percentage, the first sub-standard comprises 57.5% antimony trioxide, 0.005% ferric oxide, 21.9% sodium carbonate, 1.8% lead oxide, 1% arsenic trioxide, and 17.795% boric acid; The second sub-standard comprises 57.8% antimony trioxide, 0.1% ferric oxide, 21.1% sodium carbonate, 1.6% lead oxide, 1.5% arsenic trioxide, and 17.9% boric acid; The third sub-standard comprises 58% antimony trioxide, 0.06% ferric oxide, 22% sodium carbonate, 0.8% lead oxide, 1.28% arsenic trioxide, and 17.86% boric acid. The fourth sub-standard comprises 58.9% antimony trioxide, 0.09% ferric oxide, 22.2% sodium carbonate, 0.1% lead oxide, 0.81% arsenic trioxide, and 17.9% boric acid. The fifth sub-standard comprises 59.5% antimony trioxide, 0.12% ferric oxide, 21.5% sodium carbonate, 0.6% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid. The sixth sub-standard comprises 60.7% antimony trioxide, 0.008% ferric oxide, 21.3% sodium carbonate, 0.012% lead oxide, 0.1% arsenic trioxide, and 17.88% boric acid. The seventh sub-standard comprises 60.8% antimony trioxide, 0.04% ferric oxide, 20.7% sodium carbonate, 0.6% lead oxide, 0.04% arsenic trioxide, and 17.82% boric acid. The eighth sub-standard comprises 61.2% antimony trioxide, 0.01% ferric oxide, 21% sodium carbonate, 0.02% lead oxide, 0.01% arsenic trioxide, and 17.76% boric acid. The ninth sub-standard comprises 61.2% antimony trioxide, 0.02% ferric oxide, 20.2% sodium carbonate, 0.3% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid.
[0011] Preferably, the standard is prepared by powder compression.
[0012] Preferably, the method for preparing the standard includes the steps of: providing a plastic ring, placing the standard in the plastic ring, and performing tableting.
[0013] Preferably, the particle size of the standard is less than 0.1 mm.
[0014] Preferably, the pressure of the tableting process is 20-40 t, and the holding time of the tableting process is 10-30 s.
[0015] The technical solution of this invention uses known standard substances and a gravimetric method to calculate the corresponding concentrations or proportions. A standard curve is established using X-ray fluorescence spectroscopy. Based on this standard curve, sodium pyroantimonate products are detected using X-ray fluorescence spectroscopy, enabling simultaneous, rapid, and accurate quantitative detection of different elements in the sodium pyroantimonate product. Compared with existing chemical analysis methods, the required time is significantly reduced; no additional testing reagents are needed, making it environmentally friendly; the overall detection method is simple and reduces errors caused by human measurement. Attached Figure Description
[0016] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.
[0017] Figure 1 A schematic flowchart of the elemental quantitative detection method for sodium pyroantimonate products provided by the present invention; Figure 2 The standard curve obtained by X-ray fluorescence spectroscopy analysis of the standard provided in this invention.
[0018] The objectives, features, and advantages of this invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation
[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0020] It should be noted that if the embodiments of the present invention involve directional indicators (such as up, down, left, right, front, back, etc.), the directional indicators are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indicators will also change accordingly.
[0021] Furthermore, if the embodiments of this invention involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the use of "and / or" or "and / or" throughout the text implies three parallel solutions. For example, "A and / or B" includes solution A, solution B, or a solution that simultaneously satisfies A and B. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.
[0022] This invention proposes a method for quantitative elemental detection of sodium pyroantimonate products, such as... Figure 1 As shown, the steps include: S1. Provide standard products, which include antimony, iron, sodium, lead and arsenic elements; S2. The standard samples were analyzed by X-ray fluorescence spectroscopy to obtain standard curves for antimony, iron, sodium, lead and argon. S3. The sodium pyroantimonate product was tested by X-ray fluorescence spectroscopy, and the contents of antimony, iron, sodium, lead and arsenic in the sodium pyroantimonate product were determined according to the standard curve.
[0023] The technical solution of this invention uses known standard substances and employs a weight ratio method to calculate the corresponding concentration or proportion. Then, it uses X-ray fluorescence spectroscopy to establish a standard curve. Based on the established standard curve, it uses X-ray fluorescence spectroscopy to detect sodium pyroantimonate products, thereby achieving simultaneous, rapid, and accurate quantitative detection of different elements in sodium pyroantimonate products. Compared with existing chemical analysis methods, the required time is significantly reduced.
[0024] In some implementations, the standards include antimony trioxide (Sb₂O₃), ferric oxide (Fe₂O₃), sodium carbonate (Na₂CO₃), lead oxide (PbO), and arsenic trioxide (As₂O₃).
[0025] Antimony trioxide, ferric oxide, sodium carbonate, lead oxide, and arsenic trioxide are all materials with high stability, high cost-effectiveness, and easy availability, making them low-cost standards for quantitative elemental detection.
[0026] In some embodiments, the standard, by mass percentage, includes 57.5%–61.2% antimony trioxide, 0.005%–0.12% ferric oxide, 20.2%–22.2% sodium carbonate, 0.02%–1.8% lead oxide, and 0.01%–1.5% arsenic trioxide. For example, the antimony trioxide content in the standard is 57.5%, 58%, 58.5%, 59%, 59.5%, 60%, 60.5%, 61%, or 61.2%, etc. The ferric oxide content is 0.005%, 0.01%, 0.015%, 0.02%, 0.025%, 0.05%, 0.1%, or 0.12%, etc. The sodium carbonate content is 20.2%, 20.5%, 20.7%, 21%, 21.5%, 22%, or 22.2%, etc. The lead oxide content is 0.02%, 0.05%, 0.1%, 0.5%, 1%, 1.5%, or 1.8%, etc. The arsenic trioxide content is 0.01%, 0.05%, 0.1%, 0.5%, 1%, or 1.5%, etc.
[0027] The raw materials used are within the above-mentioned mass percentage range and have contents of antimony, iron, sodium, lead, and arsenic in sodium pyroantimonate products. Therefore, a standard curve for detecting sodium pyroantimonate products can be obtained with a smaller amount of standard products.
[0028] In some implementations, the standard also includes boric acid (H3BO3). Adding boric acid to the standard primarily serves as a binder; moreover, boric acid is a colorless and transparent substance, ensuring that the various components in the standard are bound together as a whole without affecting the detection results of X-ray fluorescence spectroscopy.
[0029] In some embodiments, the standard comprises 17.23% to 17.98% boric acid by mass percentage. For example, the boric acid content in the standard is 17.23%, 17.35%, 17.54%, 17.76%, 17.8%, 17.82%, 17.83%, 17.85%, 17.86%, 17.87%, 17.88%, 17.9%, or 17.98%, etc.
[0030] Furthermore, in some embodiments, the standard product includes a first sub-standard product, a second sub-standard product, a third sub-standard product, a fourth sub-standard product, a fifth sub-standard product, a sixth sub-standard product, a seventh sub-standard product, an eighth sub-standard product, and a ninth sub-standard product.
[0031] Specifically, by mass percentage, the first sub-standard comprises 57.5% antimony trioxide, 0.005% ferric oxide, 21.9% sodium carbonate, 1.8% lead oxide, 1% arsenic trioxide, and 17.795% boric acid; The second sub-standard includes 57.8% antimony trioxide, 0.1% ferric oxide, 21.1% sodium carbonate, 1.6% lead oxide, 1.5% arsenic trioxide, and 17.9% boric acid; The third sub-standard includes 58% antimony trioxide, 0.06% ferric oxide, 22% sodium carbonate, 0.8% lead oxide, 1.28% arsenic trioxide, and 17.86% boric acid. The fourth sub-standard includes 58.9% antimony trioxide, 0.09% ferric oxide, 22.2% sodium carbonate, 0.1% lead oxide, 0.81% arsenic trioxide, and 17.9% boric acid; The fifth sub-standard includes 59.5% antimony trioxide, 0.12% ferric oxide, 21.5% sodium carbonate, 0.6% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid; The sixth sub-standard includes 60.7% antimony trioxide, 0.008% ferric oxide, 21.3% sodium carbonate, 0.012% lead oxide, 0.1% arsenic trioxide, and 17.88% boric acid; The seventh sub-standard includes 60.8% antimony trioxide, 0.04% ferric oxide, 20.7% sodium carbonate, 0.6% lead oxide, 0.04% arsenic trioxide, and 17.82% boric acid; The eighth sub-standard includes 61.2% antimony trioxide, 0.01% ferric oxide, 21% sodium carbonate, 0.02% lead oxide, 0.01% arsenic trioxide, and 17.76% boric acid; The ninth sub-standard includes 61.2% antimony trioxide, 0.02% ferric oxide, 20.2% sodium carbonate, 0.3% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid.
[0032] In some embodiments, in step S1, the standard is prepared by a powder compression method. Specifically, the method for preparing the standard includes the following steps: S11, Provide plastic rings; S12. Weigh a certain amount of standard sample in a plastic ring; S13. Place the plastic ring on a press for tableting.
[0033] The diameter of the plastic ring is 40 mm.
[0034] In some implementations, the particle size of the standard sample is less than 0.1 mm. If the particle size of the standard sample is large, it can be ground. The grinding method can be ball milling, etc., and is not limited here.
[0035] In some embodiments, the tableting pressure is 20-40 tons (t). The unit of pressure for tableting is tons of force (tonnf). For example, the tableting pressure may be 20 t, 25 t, 30 t, 35 t, or 40 t. The holding time for tableting is 10-30 seconds. For example, the holding time may be 10 seconds, 15 seconds, 20 seconds, 25 seconds, or 30 seconds.
[0036] The following specific examples will provide further details.
[0037] Example 1 (1) Select the standard samples shown in Table 1.
[0038] Table 1. Composition of Standard Products
[0039] (2) Weigh different amounts of standard raw materials (particle size less than 0.1 mm) according to Table 2 below to prepare the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth sub-standards. The total amount is 6.2 g. Place the weighed standard raw materials in a plastic ring with a diameter of 40 mm, and then use a tablet press to perform tableting, wherein the tableting pressure is 30 t and the holding time is 30 s.
[0040] Table 2 Components of Standards
[0041] (3) All prepared sub-standards were tested using an X-ray fluorescence spectrometer, and a standard curve was plotted, such as... Figure 2 As shown.
[0042] (4) Provide 6 sodium pyroantimonate products to be tested (samples 1-5). Use the X-ray fluorescence spectrometer in (3) to test the 6 sodium pyroantimonate products to be tested, and calculate the content of each element (antimony, iron, sodium, lead, arsenic) in the sodium pyroantimonate products to be tested according to the standard curve obtained in (3).
[0043] (5) The sodium pyroantimonate product to be tested shall be chemically analyzed and tested using the international testing method (YS / T22-2010).
[0044] (6) The element content detected by the element quantitative detection method of sodium pyroantimonate product provided in the embodiment of the present invention in (4) is compared with the element content detected by the international detection method in (5), as shown in Table 3.
[0045] Table 3 Comparison of element content in the samples to be tested
[0046] As can be seen from Table 3, the elemental quantitative detection method for sodium pyroantimonate products in this embodiment of the invention can accurately detect the content of antimony, iron, sodium, lead and arsenic in the six samples, and its detection accuracy is not lower than that of the detection method in YS / T22-2010.
[0047] In summary, the technical solution of this invention uses known standard substances and a weight ratio method to calculate the corresponding concentration or proportion. A standard curve is established using X-ray fluorescence spectroscopy analysis. Based on the established standard curve, the sodium pyroantimonate product is detected using X-ray fluorescence spectroscopy analysis. The entire detection process can be completed in just ten minutes, significantly shortening the detection time. Furthermore, X-ray fluorescence spectroscopy analysis is a physical detection method, requiring no additional testing reagents, making it environmentally friendly. The overall detection method is simple, reducing errors caused by human measurement, and enabling simultaneous, rapid, and accurate quantitative detection of different elements in sodium pyroantimonate products.
[0048] The above description is merely an exemplary embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention specification and drawings under the technical concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.
Claims
1. A method for quantitative elemental detection of sodium pyroantimonate products, characterized in that, include: Provide standard samples, which include antimony, iron, sodium, lead, and arsenic. The standard samples were analyzed by X-ray fluorescence spectroscopy to obtain standard curves for antimony, iron, sodium, lead, and arsenic. The sodium pyroantimonate product was tested by X-ray fluorescence spectroscopy, and the contents of antimony, iron, sodium, lead, and arsenic in the sodium pyroantimonate product were determined according to the standard curve.
2. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 1, characterized in that, The standard substances include antimony trioxide, ferric oxide, sodium carbonate, lead oxide, and arsenic trioxide.
3. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 2, characterized in that, The standard comprises, by mass percentage: 57.5%–61.2% antimony trioxide, 0.005%–0.12% ferric oxide, 20.2%–22.2% sodium carbonate, 0.02%–1.8% lead oxide, and 0.01%–1.5% arsenic trioxide.
4. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 2, characterized in that, The standard includes boric acid.
5. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 4, characterized in that, The standard comprises 17.23% to 17.98% boric acid by mass percentage.
6. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 5, characterized in that, The standard products include a first sub-standard product, a second sub-standard product, a third sub-standard product, a fourth sub-standard product, a fifth sub-standard product, a sixth sub-standard product, a seventh sub-standard product, an eighth sub-standard product, and a ninth sub-standard product; By mass percentage, the first sub-standard comprises 57.5% antimony trioxide, 0.005% ferric oxide, 21.9% sodium carbonate, 1.8% lead oxide, 1% arsenic trioxide, and 17.795% boric acid; The second sub-standard comprises 57.8% antimony trioxide, 0.1% ferric oxide, 21.1% sodium carbonate, 1.6% lead oxide, 1.5% arsenic trioxide, and 17.9% boric acid; The third sub-standard comprises 58% antimony trioxide, 0.06% ferric oxide, 22% sodium carbonate, 0.8% lead oxide, 1.28% arsenic trioxide, and 17.86% boric acid. The fourth sub-standard comprises 58.9% antimony trioxide, 0.09% ferric oxide, 22.2% sodium carbonate, 0.1% lead oxide, 0.81% arsenic trioxide, and 17.9% boric acid. The fifth sub-standard comprises 59.5% antimony trioxide, 0.12% ferric oxide, 21.5% sodium carbonate, 0.6% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid. The sixth sub-standard comprises 60.7% antimony trioxide, 0.008% ferric oxide, 21.3% sodium carbonate, 0.012% lead oxide, 0.1% arsenic trioxide, and 17.88% boric acid. The seventh sub-standard comprises 60.8% antimony trioxide, 0.04% ferric oxide, 20.7% sodium carbonate, 0.6% lead oxide, 0.04% arsenic trioxide, and 17.82% boric acid. The eighth sub-standard comprises 61.2% antimony trioxide, 0.01% ferric oxide, 21% sodium carbonate, 0.02% lead oxide, 0.01% arsenic trioxide, and 17.76% boric acid. The ninth sub-standard comprises 61.2% antimony trioxide, 0.02% ferric oxide, 20.2% sodium carbonate, 0.3% lead oxide, 0.4% arsenic trioxide, and 17.88% boric acid.
7. The method for quantitative elemental detection of sodium pyroantimonate products as described in any one of claims 1 to 6, characterized in that, The standard is prepared by powder compression.
8. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 7, characterized in that, The method for preparing the standard includes the steps of: providing a plastic ring, placing the standard in the plastic ring, and performing tableting.
9. The method for quantitative elemental detection of sodium pyroantimonate products as described in claim 8, characterized in that, The particle size of the standard is less than 0.1 mm.
10. The method for quantitative elemental detection of sodium pyroantimonate product as described in claim 8, characterized in that, The pressure of the tableting process is 20-40 t, and the holding time of the tableting process is 10-30 s.