CN116223486A - Analysis method for yttrium content in yttrium-containing glass microsphere material - Google Patents
Analysis method for yttrium content in yttrium-containing glass microsphere material Download PDFInfo
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- CN116223486A CN116223486A CN202310336107.2A CN202310336107A CN116223486A CN 116223486 A CN116223486 A CN 116223486A CN 202310336107 A CN202310336107 A CN 202310336107A CN 116223486 A CN116223486 A CN 116223486A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention relates to the technical field of glass material detection, in particular to an analysis method for yttrium content in yttrium-containing glass microsphere materials. The analysis method comprises the following steps: a) Carrying out microwave digestion on the cleaned and dried sample under the heating condition of a digestion system containing mixed acid; the mixed acid comprises hydrofluoric acid, nitric acid and hydrochloric acid with the volume ratio of (3-10), (0.7-1.3), (2.5-3.5); b) Adding perchloric acid to remove hydrofluoric acid under heating condition after the sample is fully digested; c) And after the sample is cooled, completely dissolving the sample, and detecting by adopting an ICP-OES system to determine the yttrium content.
Description
Technical Field
The invention relates to the technical field of glass material detection, in particular to an analysis method for yttrium content in yttrium-containing glass microsphere materials.
Background
Hepatocellular carcinoma is currently the second most common malignancy in the world leading to death, and traditional surgical treatment is an important means by which liver cancer patients may survive for a long period of time. However, most patients have advanced in the treatment, and often have severe complications such as cirrhosis, and the available liver sources for transplantation are very limited, and statistics data show that about 10% of liver cancer patients can get the opportunity of operation, and most patients can only use conventional in vitro radiotherapy and chemotherapy means to control tumors in the cancer treatment stage. The prior art of global advanced yttrium-90 radiation microsphere interventional therapy shows that the therapy has better performance and expression on the treatment of advanced liver cancer through a large number of animal experiments and clinical experiments, can effectively shrink and even necrotize tumors so as to prolong the survival time of patients, and has great potential in combination with other treatment schemes.
For glass microsphere materials containing about 10% of yttrium by mass, no relevant report has been found in the prior art such as traditional wet chemistry methods, X-ray fluorescence methods and the like in order to accurately measure the yttrium content in finished products. ICP-OES is a detection technology developed and mature in the last twenty years, and has the advantages of more detection elements, wide detection range, strong element distinguishing capability, high result accuracy and the like, but the glass microsphere sample needs to be digested into a solution for testing. Because the glass microspheres are usually produced by taking aluminum oxide and silicon oxide as auxiliary materials, the conventional alkali dissolution method and acid dissolution method can not thoroughly digest samples, and can lead to inaccurate test data of yttrium and poor parallelism and repeatability and reproducibility; on the other hand, if the salt content or acidity is too high, it may affect the measurement performance of the analytical instrument ICP-OES. Therefore, there is a need to study a feasible pretreatment method and to explore and optimize the measurement parameters of ICP-OES instruments so that the accuracy and precision of measuring high concentration yttrium solutions can meet the test requirements.
In view of this, the present invention has been made.
Disclosure of Invention
The invention relates to an analysis method of yttrium content in yttrium-containing glass microsphere materials, which comprises the following steps:
a) Carrying out microwave digestion on the cleaned and dried sample under the heating condition of a digestion system containing mixed acid; the mixed acid comprises hydrofluoric acid, nitric acid and hydrochloric acid with the volume ratio of (3-10), (0.7-1.3), (2.5-3.5);
b) Adding perchloric acid to remove hydrofluoric acid under heating condition after the sample is fully digested;
c) And after the sample is cooled, completely dissolving the sample, and detecting by adopting an ICP-OES system to determine the yttrium content.
By adopting the analysis method, the sample can be fully dissolved to obtain a clear solution to be tested, meanwhile, the possible damage of high salt and high acid to a testing instrument is avoided, an ideal testing result can be achieved, and the yttrium testing data has small deviation, good parallelism, good stability and good reproducibility.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a standard operating curve provided by one embodiment of the present invention;
f(x)=2563.1776x+2.5241; R 2 =0.9995; BEC=0.001ppm; LoD=0.0012ppm。
Detailed Description
Reference now will be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. Indeed, it will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the scope or spirit of the invention. For example, features illustrated or described as part of one embodiment can be used on another embodiment to yield still a further embodiment.
Unless otherwise defined, all terms (including technical and scientific terms) used to describe the invention have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. By way of further guidance, the following definitions are used to better understand the teachings of the present invention. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The term "and/or," "and/or," as used herein, includes any one of two or more of the listed items in relation to each other, as well as any and all combinations of the listed items in relation to each other, including any two of the listed items in relation to each other, any more of the listed items in relation to each other, or all combinations of the listed items in relation to each other. It should be noted that, when at least three items are connected by a combination of at least two conjunctions selected from "and/or", "or/and", "and/or", it should be understood that, in this application, the technical solutions certainly include technical solutions that all use "logical and" connection, and also certainly include technical solutions that all use "logical or" connection. For example, "a and/or B" includes three parallel schemes A, B and a+b. For another example, the technical schemes of "a, and/or B, and/or C, and/or D" include any one of A, B, C, D (i.e., the technical scheme of "logical or" connection), and also include any and all combinations of A, B, C, D, i.e., any two or three of A, B, C, D, and also include four combinations of A, B, C, D (i.e., the technical scheme of "logical and" connection).
The terms "comprising," "including," and "comprising," as used herein, are synonymous, inclusive or open-ended, and do not exclude additional, unrecited members, elements, or method steps.
The recitation of numerical ranges by endpoints of the present invention includes all numbers and fractions subsumed within that range, as well as the recited endpoint.
Concentration values are referred to in this invention, the meaning of which includes fluctuations within a certain range. For example, it may fluctuate within a corresponding accuracy range. For example, 2%, may allow fluctuations within + -0.1%. For values that are larger or do not require finer control, it is also permissible for the meaning to include larger fluctuations. For example, 100mM, fluctuations in the range of.+ -. 1%,.+ -. 2%,.+ -. 5%, etc. can be tolerated. Molecular weight is referred to, allowing its meaning to include fluctuations of + -10%.
In the present invention, the terms "plurality", and the like refer to, unless otherwise specified, 2 or more in number.
In the invention, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present invention, "preferred", "better", "preferred" are merely embodiments or examples which are better described, and it should be understood that they do not limit the scope of the present invention. In the present invention, "optional" means optional or not, that is, means any one selected from two parallel schemes of "with" or "without". If multiple "alternatives" occur in a technical solution, if no particular description exists and there is no contradiction or mutual constraint, then each "alternative" is independent.
In the present invention, the term "microsphere" refers to an object that is substantially spherical and has a diameter of less than 1 millimeter. The specific shape can be sphere, near sphere, cube, polyhedron or irregular shape. The particle size of the microspheres may further be 5 μm to 500 μm, for example 10 μm, 50 μm, 80 μm, 100 μm, 200 μm, 300 μm, 400 μm; more preferably 10 μm to 100 μm, still more preferably 20 μm to 50 μm. The microspheres may be solid, hollow, or solid comprising a plurality of hollow cells, preferably solid. The density of the microspheres may be, for example, 1.0g/cm 3 ~5.0g/cm 3 Preferably 1.0g/cm 3 ~3.0g/cm 3 More preferably 1.0g/cm 3 ~2.0g/cm 3 。
In the present invention, the term "yttrium-containing glass microsphere material" contains yttrium element, in particular 90 Y, which can be used for the treatment of cancer. Of course, the yttrium-containing glass microsphere material may also contain other radioactive elements, suitable radionuclidesSelected from the group consisting of 32 P、 198 Au、 188 Re、 166 Ho、 99m Tc、 109 Pd、 140 La、 153 Sm、 165 Dy and Dy 169 One or more of Er. The material is glass as the main component, but may also contain other known components such as ceramics, polymers and resins. The term "glass" refers to a hard, brittle, amorphous inorganic substance that is generally transparent; glass is generally prepared using sodium carbonate and fused silicate as described in Webster's New World Dictionary.Ed.Guralnik, DB 1984. Glass is relatively resistant to radiation damage, extremely insoluble and non-toxic. Glass is easily spheroidized uniformly in size and has minimal radionuclide impurities. Technological developments have led to the preparation of glass microspheres that are substantially free of leaching of radioactive materials.
In the present invention, the reagent is preferably pure or higher, and water of a second or higher grade specified in GB/T6682 is used.
The invention relates to an analysis method of yttrium content in yttrium-containing glass microsphere materials, which comprises the following steps:
a) Carrying out microwave digestion on the cleaned and dried sample under the heating condition of a digestion system containing mixed acid; the mixed acid comprises hydrofluoric acid, nitric acid and hydrochloric acid with the volume ratio of (3-10), (0.7-1.3), (2.5-3.5);
b) Adding perchloric acid to remove hydrofluoric acid under heating condition after the sample is fully digested;
c) And after the sample is cooled, completely dissolving the sample, and detecting by adopting an ICP-OES system to determine the yttrium content.
In some embodiments, the mixed acid comprises hydrofluoric acid, nitric acid and hydrochloric acid in a volume ratio of (4-9): (0.7-1.3): (2.5-3.5).
In some embodiments, the mixed acid comprises mainly hydrofluoric acid, nitric acid and hydrochloric acid, and the molar content of the hydrofluoric acid, the nitric acid and the hydrochloric acid accounts for at least 80%, or 85%, or 90%, or 95%, or 97%, or 98%, or 99%, or 99.5% or more of the total amount of the mixed acid.
In some embodiments, the mixed acid contains only inorganic acids.
In some embodiments, the mixed acid contains only a strong mineral acid.
In some embodiments, the mixed acid may or may not contain one or more of boric acid, sulfuric acid, carbonic acid, and phosphoric acid.
In some embodiments, the ratio of the sample to the hydrofluoric acid is 0.1g (1 ml to 3 ml). Most preferably 0.1 g/2 ml. The addition of excessive hydrofluoric acid increases the test cost, and increases the acid removing time in the step S4 so as to reduce the pretreatment efficiency; too little hydrofluoric acid addition may result in incomplete digestion of the sample.
In some embodiments, the particle size of the sample is < 80 μm.
If the diameter of the sample is larger than 80 mu m, the sample can be cleaned by pure water, dried in an oven at 105-110 ℃ and cooled, and then the sample is ground by an agate mortar until the sample can pass through a sieve with a pore diameter of 80 mu m, and the mass is not less than 10g (error reduction).
In addition, in step a), the drying is preferably carried out in an oven at 105℃to 110℃for at least 1 hour, and then cooled in a dryer.
In some embodiments, the temperature of heating in step a) is 150 ℃ ± 5 ℃, e.g., 147 ℃, 150 ℃, 153 ℃.
In some embodiments, the temperature of heating in step b) is 150 ℃ ± 10 ℃, e.g., 145 ℃, 147 ℃, 150 ℃, 153 ℃, 155 ℃.
In some embodiments, in step c), the sample is dissolved with a dilute nitric acid solution to avoid precipitation of insoluble aluminum hydroxide from aluminum in the sample.
The dilute nitric acid solution is preferably 0.5 v/v% -1.5 v/v% nitric acid aqueous solution, for example 0.7 v/v%, 1.0 v/v%, 1.3 v/v%.
In some embodiments, the sample is diluted and sized, preferably to 100ml per 0.1g to 0.2g final sized, after dissolution with dilute nitric acid solution, using an ICP-OES system for testing.
In some embodiments, in step c), the elemental quality is analyzed with the measured strength of yttriumThe relation between the quantitative concentration is established to draw a working curve, the mass concentration (C) of yttrium in the solution to be measured is obtained from the working curve by measuring the intensity of yttrium in the solution to be measured, and the yttrium content omega in the sample is determined by calculation of a formula 1) Y ：
ω Y (%)=(C×V×10 -6 ) M 100%; 1, a method for manufacturing the same
Wherein: c, the mass concentration of yttrium in the solution to be measured, mug/ml;
v-determining the volume of the solution to be measured, and ml;
m-sample is actually weighed, g.
In some embodiments, the analysis line is selected to be 360.07nm or 371.03nm.
Both analysis lines have less spectral interference and high sensitivity. Preferably 360.07nm, the analytical line sensitivity is relatively low.
In some embodiments, ICP-OES is in a bidirectional observation mode, a plasma vertical observation mode can be selected, analysis sensitivity is reduced, and the instrument still has better stability when analyzing elements to be detected at a high concentration level.
In some embodiments, the standard curve is drawn with 3-5 different concentrations of yttrium standard solution in addition to 0 point.
Wherein the multiples of adjacent yttrium standard solution concentrations are preferably equal, but may also be different; multiples such as 2, 3, 4, 5, 10. In some specific embodiments, the concentration comprises at least 10 μg/ml, 50 μg/ml, 100 μg/ml, 200 μg/ml, 400 μg/ml. It will be readily appreciated that to reduce systematic errors, the sample volumes for each concentration of standard solution used to plot the standard curve are preferably kept consistent.
In some embodiments, the method comprises performing at least two parallel assays on the sample to be tested, with a weighing accuracy of no less than 0.0001g.
In the single experiment process, the amount of a single sample is preferably 0.1 g-0.2 g.
Embodiments of the present invention will be described in detail below with reference to examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples, in which specific conditions are not noted, are preferably referred to in the guidelines given in the present invention, and may be according to the experimental manuals or conventional conditions in the art, and may be referred to other experimental methods known in the art, or according to the conditions suggested by the manufacturer.
In the specific examples described below, the measurement parameters relating to the raw material components, unless otherwise specified, may have fine deviations within the accuracy of weighing. Temperature and time parameters are involved, allowing acceptable deviations from instrument testing accuracy or operational accuracy.
Examples
An analytical method for detecting yttrium content in yttrium-containing glass microsphere materials by ICP-OES, comprising the following steps:
s1, preparation of a sample: cleaning the sample with pure water, drying in an oven at 105-110 ℃ for at least 1 hour, cooling in a dryer, and sealing for later use. The sample is not less than 10g.
S2, weighing: accurately weighing 0.2g of sample to 0.0001g, placing into a microwave digestion tank, and performing parallel measurement in 5 parts.
S3, digestion: sequentially adding a small amount of water (wetting), 4ml of hydrofluoric acid, 1ml of nitric acid and 3ml of hydrochloric acid into a microwave digestion tank filled with the sample, placing the microwave digestion tank into a microwave digestion instrument, and decomposing the sample at the temperature of 150+/-5 ℃.
S4 acid removal: after the sample is fully digested, the microwave digestion tank is taken out and transferred to a temperature-controllable electric heating plate, 3ml of perchloric acid is added into the tank, the temperature of a heating plate is regulated to about 150+/-10 ℃, and the solution is slowly heated and evaporated until the solution is nearly dry so as to expel hydrofluoric acid. After cooling at room temperature, 10ml of nitric acid (volume ratio: 1 nitric acid: 99 water) was added to the tank, and after the sample was completely dissolved, the digestion tank was taken out of the heating furnace and cooled at room temperature.
S5, constant volume: transferring the solution in the digestion tank into a 100ml plastic volumetric flask, diluting to a scale with pure water, and shaking uniformly to obtain the solution to be measured.
S6, preparing a standard curve series solution: a standard solution of unitary evidence with yttrium concentration of 1000. Mu.g/ml was used. Into 6 plastic volumetric flasks of 100ml, 0ml, 1ml, 5ml, 10ml, 20ml and 40ml of yttrium single element standard solution are added respectively, 10ml of nitric acid (volume ratio: 1 nitric acid: 99 water) is added respectively, diluted to scale with water and shaken uniformly, thereby preparing standard curve solutions containing yttrium with mass concentration of 0 mug/ml, 10 mug/ml, 50 mug/ml, 100 mug/ml, 200 mug/ml and 400 mug/ml.
S7, on-machine test: ICP-OES is provided with a hydrofluoric acid resistant sample injection system. Opening instrument software and setting instrument parameters: RF power: 1150W; carrier gas flow rate: 0.65L/min; pump speed 45 rpm; auxiliary air flow: 1.00L/min; the cooling air flow is 12.5L/min; vertical visual height 10.0mm; analytical line selection Y360.07nm; the mode of acquisition parameters selects 'high content vertical observation', and the plasma observation selects 'vertical'; the sampling time and the washing time were set to 30s. And sequentially measuring standard curve series solutions, and automatically drawing a working curve by using the measured yttrium strength as an ordinate and the mass concentration of an analysis element as an abscissa by an instrument. Checking the working curve (fig. 1), linear correlation coefficient R 2 =0.9995, satisfying the linearity requirement of not less than 0.999. The standard curve solution with the concentration of 400 mug/ml is continuously measured 10 times (the measured data are shown in table 1), the relative standard deviation rsd=0.64% is calculated, and the requirement that RSD is not more than 1% is met, which shows that the measurement stability is good. Measuring the solution to be measured, and automatically checking the mass concentration of yttrium in the solution to be measured from the working curve by an instrument; the measurements of the replicates were repeated and 5 replicates were measured as shown in table 2. Calculating according to the formula 1), and measuring that the average yttrium content in the sample is 9.95 percent and is consistent with the theoretical proportioning ratio of 10 percent; standard deviation s=0.025%, indicating good parallelism of the test data.
Table 1 working curve highest mass concentration stability data measured 10 consecutive times
Table 2 example analysis results
Comparative example
The sample adopts a hydrofluoric acid dissolution method, which comprises the following steps:
s1, weighing: accurately weighing 0.2g of sample to 0.0001g, placing into a polytetrafluoroethylene beaker, and carrying out 5 parts of parallel measurement.
S2, decomposition: to a beaker containing the sample, a small amount of water (wet), 8ml of hydrofluoric acid, and 1ml of perchloric acid were sequentially added, a teflon watch glass was covered, and the sample was decomposed at 150.+ -. 10 ℃ on a hot plate. After the reaction was observed to stop, the dish was opened, heating was continued, the solution was observed to evaporate until white smoke was evolved (care was taken during the process to prevent the solution from splashing), the beaker was removed and cooled at room temperature, 20ml of pure water was added to the beaker, the dish was covered, boiled at 150 ℃ ± 10 ℃ on a hot plate, and the beaker was removed and cooled at room temperature.
S3, constant volume: the solution in the beaker was transferred to a 100ml plastic volumetric flask, diluted to scale with pure water, and shaken well to give the solution to be measured. At this time, a small amount of white powdery deposit was observed at the bottom of the solution to be measured, indicating that the sample was not completely decomposed.
S4, on-machine test: the supernatant of the above solution was taken and measured under the same standard working curve as in the examples. The measurement of the parallel sample was repeated, the measurement data of the 5 parallel samples are shown in Table 3, and the yttrium content in the sample was calculated according to the formula 1). The average yttrium content in the measured sample is 7.29 percent by calculation, and the average yttrium content is greatly different from the theoretical proportion of 10 percent; the measurement standard deviation s=1.29% indicates poor parallelism of the test data.
Table 3 comparative example analysis results
Therefore, by adopting the analysis method provided by the invention, the sample can be completely dissolved to obtain a clear solution to be tested, meanwhile, the possible damage of high salt and high acid to a testing instrument is avoided, the best testing result can be achieved, and the yttrium testing data has small deviation, good parallelism, good stability and good reproducibility.
Incorporated herein by reference:
all patents and publications cited herein are incorporated herein by reference.
Equivalent embodiment:
those skilled in the art will recognize, or be able to ascertain using no more than routine experimentation, many equivalents to the specific embodiments of the invention described herein. The claims are intended to include such equivalent embodiments.
Claims (10)
1. The method for analyzing the yttrium content in the yttrium-containing glass microsphere material is characterized by comprising the following steps of:
a) Carrying out microwave digestion on the cleaned and dried sample under the heating condition of a digestion system containing mixed acid; the mixed acid comprises hydrofluoric acid, nitric acid and hydrochloric acid with the volume ratio of (3-10), (0.7-1.3), (2.5-3.5);
b) Adding perchloric acid to remove hydrofluoric acid under heating condition after the sample is fully digested;
c) And after the sample is cooled, completely dissolving the sample, and detecting by adopting an ICP-OES system to determine the yttrium content.
2. The method for analyzing the yttrium content of the yttrium-containing glass microsphere material according to claim 1, wherein the addition ratio of the sample to the hydrofluoric acid is 0.1g (1 ml to 3 ml).
3. The method for analyzing the yttrium content of an yttrium-containing glass microsphere material according to claim 1, wherein the particle size of the sample is < 80 μm.
4. The method for analyzing the yttrium content of an yttrium-containing glass microsphere material according to claim 1, wherein the heating temperature in the step a) is 150 ℃ ± 5 ℃.
5. The method for analyzing the yttrium content of an yttrium-containing glass microsphere material according to claim 1, wherein the heating temperature in the step b) is 150 ℃ ± 10 ℃.
6. The method according to claim 1, wherein in step c), the sample is dissolved in a dilute nitric acid solution to avoid precipitation of insoluble aluminum hydroxide from aluminum in the sample.
7. The method according to any one of claims 1 to 6, wherein in the step C), a working curve is drawn according to the relationship between the measured yttrium strength and the mass concentration of the analysis element, the yttrium mass concentration (C) in the solution to be measured is obtained from the working curve by measuring the yttrium strength in the solution to be measured, and the yttrium content (ω) in the sample is determined by calculation according to the formula 1 Y ）：
ω Y (%)=(C×V×10 -6 ) M 100%; 1, a method for manufacturing the same
Wherein: c, the mass concentration of yttrium in the solution to be measured, mug/ml;
v-determining the volume of the solution to be measured, and ml;
m-sample is actually weighed, g.
8. The method of claim 7, wherein the analysis line is 360.07nm or 371.03nm.
9. The method for analyzing yttrium content in yttrium-containing glass microsphere material according to claim 7, wherein the standard curve is drawn by using 3-5 yttrium standard solutions with different concentrations besides 0 point.
10. The method for analyzing the yttrium content in the yttrium-containing glass microsphere material according to any one of claims 1 to 6, 8 and 9, wherein the method is characterized in that at least two parallel measurement is carried out on a sample to be detected, and the weighing precision is not lower than 0.0001g.
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| CN104914090A (en) * | 2015-05-08 | 2015-09-16 | 广东省矿产应用研究所 | Detection method for continuously measuring Ga, In and Ge In lead-zinc smelting smoke dust through microwave digestion-ICP-OES |
| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN108458918A (en) * | 2018-06-25 | 2018-08-28 | 广西冶金研究院有限公司 | A kind of method that micro-wave digestion-ICP-OES measures copper, lead, zinc, cadmium element in ion type rareearth slag |
| CN109297801A (en) * | 2018-11-09 | 2019-02-01 | 山东省食品药品检验研究院 | The detection method of arsenic in food additives silica |
| CN111272737A (en) * | 2018-12-05 | 2020-06-12 | 核工业理化工程研究院 | Method for determining percentage content of multiple elements in high-silicon aluminum alloy through microwave digestion-ICP-OES and application of method |
| CN110749643A (en) * | 2019-11-25 | 2020-02-04 | 中国科学院长春应用化学研究所 | Method for measuring content of inorganic elements in Mongolian medicine mineral medicine magnet |
| CN113109323A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine sediments |
| CN114739982A (en) * | 2022-03-21 | 2022-07-12 | 甘肃光轩高端装备产业有限公司 | Method for detecting element content in glass |
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