All-element analysis method for unknown waste

Abstract

The invention relates to the technical field of elemental analysis, in particular to an all-elemental analysis method for unknown waste. The all-element analysis instrument provided by the invention comprises an inductively coupled plasma emission spectrometer (ICP-OES), an inductively coupled plasma mass spectrometer (ICP-MS), an X-ray fluorescence spectrometer (XRF), an energy dispersive X-ray spectrometer (EDS), an infrared carbon-sulfur analyzer, an oxygen-nitrogen-hydrogen analyzer, an elemental analyzer (EA), a chemical method, a spark direct-reading spectrometer and an ion chromatograph (IC). The all-element analysis can accurately determine the contents of components and elements in the product, and can provide high-quality and comprehensive data, thereby helping researchers to better understand the interaction and influence among the elements. All-element analysis of the unknown waste is of great significance to improvement of waste resource utilization efficiency, optimization of waste treatment process, promotion of green low-carbon technical progress and formulation of effective resource utilization measures.

Description

Technical Field

[0001] The present invention relates to the technical field of elemental analysis, and specifically relates to a method for comprehensive elemental analysis of unknown waste. Background Art

[0002] Waste may contain heavy metals (such as lead, mercury, cadmium, arsenic), toxic organic substances (such as polycyclic aromatic hydrocarbons, dioxins) or radioactive substances, which can seep into the soil, damage the soil structure and physical and chemical properties, and then affect the growth of crops. In the long run, these contaminated soils can not only fail to produce healthy crops, but also cause long-term harm to human health through the food chain. Secondly, the pollution of waste to water bodies cannot be ignored either. Waste may contain a large number of harmful substances, such as heavy metal ions, organic substances, acid-base substances, etc. They will pollute surface water and groundwater, disrupting the water ecological balance. In some areas, due to the random placement of waste, groundwater has been severely polluted, which not only affects people's normal life, but also causes damage to the ecosystem and biodiversity. At the same time, waste often contains a large amount of recyclable resources. Random discarding not only wastes resources but also increases the environmental burden.

[0003] In view of the above problems, the present invention provides a method for comprehensive elemental analysis of unknown waste. Conducting comprehensive elemental analysis of unknown waste is of great significance for environmental protection, safety management, resource recovery, compliance, etc. By comprehensively understanding the chemical composition and properties of waste, waste can be managed and processed more effectively, reducing its potential harm to the environment and human health. Summary of the Invention

[0004] In view of the deficiencies of the prior art, a method for comprehensive elemental analysis of unknown waste, through the analysis of all elements of waste, not only helps environmental protection and resource recovery, but also meets compliance requirements, supports scientific research, and optimizes industrial production.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for comprehensive elemental analysis of unknown waste, comprising the following steps:

[0007] S1, analyzing the content of metal elements by inductively coupled plasma optical emission spectrometer (ICP-OES): accurately weigh the sample in a container, perform pre-digestion treatment, after constant volume, filter through a membrane and test on the machine, and run the standard curve at the same time to accurately analyze the content of metal elements, with a detection limit of 5 ppm;

[0008] S2, analyzing the content of metal elements by inductively coupled plasma mass spectrometer (ICP-MS): accurately weigh the sample in a container, perform pre-digestion treatment, after constant volume, filter through a membrane and test on the machine, and run the standard curve at the same time to accurately analyze the content of metal elements, with a detection limit of 10 ppb;

[0009] S3. Analyze the element content of 4Be - 92U by energy dispersive X-ray spectrometer (EDS): Directly stick the solid sample onto the conductive adhesive, perform gold spraying treatment, test on the machine, process and analyze the collected data to obtain the relative content of each element in the sample. Detection limit: 0.1% - 0.5%;

[0010] S4. Analyze the content of acid radical ions by ion chromatograph: Prepare acid radical ions (such as fluoride ions, chloride ions, bromide ions, and iodide ions) with different concentrations, draw a standard curve, accurately weigh the sample, filter it through a membrane after pretreatment and then test on the machine to calculate the content of fluoride ions, chloride ions, bromide ions, iodide ions, etc.

[0011] As a preferred embodiment of the present invention, the following steps are further included:

[0012] S5. Analyze the elements of 11Na - 92U by X-ray fluorescence spectrometer (XRF): Grind and prepare the sample, put the prepared sample into the sample chamber, set relevant parameters, conduct tests, and analyze the element composition and relative content;

[0013] S6. Analyze the content of carbon, hydrogen, oxygen, nitrogen, and sulfur elements in organic materials and organic compounds by elemental analyzer (EA): First, set the experimental parameters, first test the blank sample and standard sample, and then measure the sample after calibration. Put the weighed sample into a special crucible, seal it and place it at the injector position, start the test program, select the corresponding analysis method (such as CHNS mode or O mode), set parameters (combustion temperature, gas flow rate, etc.), the sample decomposes in a high-temperature combustion furnace to generate gases (such as CO2, H2O, N2, SO2, etc.), and the gases are separated by a chromatographic column and quantitatively analyzed by a detector (such as thermal conductivity detector TCD). Detection limit: 100 ppm;

[0014] As a preferred embodiment of the present invention, the following steps are further included:

[0015] S7. Analyze the content of carbon and sulfur elements in inorganic metal materials by infrared carbon-sulfur analyzer: Put the weighed sample and flux into a ceramic crucible, place it in the combustion furnace for determination, and run the standard sample at the same time to calculate the results of carbon and sulfur. Measurement range: low carbon: 1 ppm - 0.2%, high carbon: 0.2% - 6%, low sulfur: 1 ppm - 0.3%;

[0016] S8. Analysis of the contents of oxygen, nitrogen, and hydrogen elements in inorganic metal materials by an oxygen, nitrogen, and hydrogen analyzer: First, burn the crucible empty several times, select a suitable standard sample for analysis. If the analysis results meet the requirements, then conduct sample analysis. Weigh the sample precisely and place it in a graphite crucible, then put it into a combustion furnace and heat it to melt at a high temperature in any one of the helium or argon gas flows. The instrument performs the fusion analysis of oxygen, nitrogen, and hydrogen according to the automatic analysis process to obtain the contents of oxygen, nitrogen, and hydrogen in the sample. The measurement ranges are as follows: low oxygen: 0.1 ppm to 0.5%, high oxygen: 0.5% to 20%, low nitrogen: 0.1 ppm to 0.5%, high nitrogen: 0.5% to 50%, hydrogen: 0.1 ppm to 2000 ppm;

[0017] S9. Analysis of the contents of main metal elements by chemical method: Conduct quantitative analysis on the required elements according to the national standard method based on the sample situation;

[0018] S10. Analysis of the contents of solid block metal elements by a spark direct-reading spectrometer: First, select a suitable standard sample for calibration according to the sample material. Place the sample on the excitation stage and ensure good contact between the sample and the electrode. Set various parameters of the instrument according to the sample type and the required analysis accuracy. Start the instrument and start exciting the sample. The instrument automatically records the spectral data for analysis to obtain the element contents;

[0019] As a preferred solution of the present invention, the container in steps S1 and S2 is any one of polytetrafluoroethylene (PTFE), perfluoroalkoxy (PFA), quartz, a microwave digestion tank, a high-pressure digestion tank (pressure bomb), and borosilicate glass.

[0020] As a preferred solution of the present invention, the pretreatment before digestion in steps S1 and S2 is any one of wet digestion (acid digestion), microwave digestion, dry ashing method, high-pressure digestion tank method, alkali fusion method, ultraviolet photolysis, and enzymatic digestion.

[0021] As a preferred solution of the present invention, the reagent used for the pretreatment before digestion in steps S1 and S2 is any one of distilled water, inorganic acid, alkaline reagent, and normal salt.

[0022] As a preferred solution of the present invention, the pretreatment in step S4 is any one of filtration, dilution, solid-phase extraction (SPE), digestion (decomposition), oxygen bomb combustion, distillation / volatilization, precipitation and complexation, and derivatization.

[0023] As a preferred solution of the present invention, the temperature of the combustion furnace in step S6 is 900 °C to 1200 °C. For some samples that are difficult to decompose (such as ceramics or polymer materials), a higher temperature (such as 1300 °C) may be used.

[0024] As a preferred solution of the present invention, the solvent assistant in step S7 is any one of tungsten (W), tin (Sn), iron (Fe), tungsten + tin, copper (Cu), or copper oxide (CuO).

[0025] As a preferred embodiment of the present invention, the combustion temperature in step S8 is 2500°C to 3000°C.

[0026] The beneficial effects of the present invention are as follows:

[0027] Unknown waste may contain harmful substances. Without a complete elemental analysis, it is impossible to accurately judge its impact on the environment. Through analysis, components that may pose a threat to the ecosystem can be identified, and corresponding measures can be taken to prevent pollution. Commonly used elemental analysis methods on the market include inductively coupled plasma optical emission spectrometer (ICP-OES), X-ray fluorescence spectrometer (XRF), elemental analyzer (EA), etc. These detection methods can only detect the elements responded by each device and cannot analyze all elements. The complete elemental analysis method provided by the present invention can comprehensively analyze the elemental composition of various wastes, and use a variety of analysis methods to conduct qualitative and quantitative research on metal and non-metal elements, etc. Through the complete elemental analysis of unknown waste, it is possible to understand which elements are contained in the waste and their contents, which is crucial for evaluating the potential hazards of waste, formulating appropriate treatment methods, and exploring resource utilization approaches. Brief Description of the Drawings

[0028] Figure 1 It is the XRF data graph of Embodiment 1 of the present invention;

[0029] Figures 2 - 3 It is the EDS spectrum of Embodiment 1 of the present invention;

[0030] Figures 4 - 9 It is the ICP-OES spectrum of Embodiment 1 of the present invention;

[0031] Figure 10 It is the ICP-MS spectrum of Embodiment 1 of the present invention;

[0032] Figures 11 - 12 It is the EA spectrum of Embodiment 1 of the present invention;

[0033] Figures 13 - 14 It is the IC spectrum of Embodiment 1 of the present invention;

[0034] Figures 15 - 16 It is the EDS spectrum of Embodiment 2 of the present invention;

[0035] Figures 17 - 22 It is the ICP-OES spectrum of Embodiment 2 of the present invention;

[0036] Figure 23 It is the ICP-MS spectrum of Embodiment 2 of the present invention;

[0037] Figure 24 It is the spectrum of the carbon and sulfur analyzer of Embodiment 2 of the present invention;

[0038] Figures 25 - 27 It is the spectrogram of the oxygen, nitrogen and hydrogen analyzer in Embodiment 2 of the present invention;

[0039] Figure 28 It is the IC spectrogram in Embodiment 2 of the present invention;

[0040] Figures 29 - 34 It is the ICP-OES spectrogram in Embodiment 3 of the present invention;

[0041] Figure 35 It is the ICP-MS spectrogram in Embodiment 3 of the present invention;

[0042] Figures 36 - 37 It is the EDS spectrogram in Embodiment 3 of the present invention;

[0043] Figure 38 It is the IC spectrogram in Embodiment 3 of the present invention; Detailed implementation manners

[0044] Next, in combination with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0045] A method for total element analysis of unknown waste, characterized by comprising the following steps:

[0046] S1. Analyzing the content of metal elements by inductively coupled plasma optical emission spectrometer (ICP-OES): Weigh the sample accurately in a container, perform pre-treatment for digestion, make the volume constant, filter through a membrane and then test on the machine. At the same time, run the standard curve to accurately analyze the content of metal elements, with a detection limit of 5 ppm;

[0047] S2. Analyzing the content of metal elements by inductively coupled plasma mass spectrometer (ICP-MS): Weigh the sample accurately in a container, perform pre-treatment for digestion, make the volume constant, filter through a membrane and then test on the machine. At the same time, run the standard curve to accurately analyze the content of metal elements, with a detection limit of 10 ppb;

[0048] S3. Analyzing the content of elements from 4Be to 92U by energy dispersive X-ray spectrometer (EDS): Stick the solid sample directly onto the conductive adhesive, perform gold spraying treatment, test on the machine, process and analyze the collected data to obtain the relative content of each element in the sample, with a detection limit of 0.1% - 0.5%;

[0049] S4. Analyzing the content of acid radical ions by ion chromatograph: Prepare acid radical ions (such as fluoride ions, chloride ions, bromide ions, and iodide ions) with different concentrations, draw a standard curve, accurately weigh the sample, filter it through a membrane after pretreatment, and then test it on the machine to calculate the content of fluoride ions, chloride ions, bromide ions, iodide ions, etc.

[0050] Further, it also includes the following steps:

[0051] S5. Analyzing elements from 11Na to 92U by X-ray fluorescence spectrometer (XRF): Grind and prepare the sample, put the prepared sample into the sample chamber, set relevant parameters, conduct the test, and analyze the element composition and relative content;

[0052] S6. Analyzing the content of carbon, hydrogen, oxygen, nitrogen, and sulfur elements in organic materials and organic compounds by elemental analyzer (EA): First, set the experimental parameters, conduct blank sample and standard sample tests first, and measure the sample after calibration. Put the weighed sample into a special crucible, seal it, and place it at the injector position. Start the test program, select the corresponding analysis method (such as CHNS mode or O mode), set parameters (combustion temperature, gas flow rate, etc.). The sample decomposes in a high-temperature combustion furnace to generate gases (such as CO2, H2O, N2, SO2, etc.). After the gases are separated by the chromatographic column, they are quantitatively analyzed by a detector (such as a thermal conductivity detector TCD). Detection limit: 100 ppm;

[0053] Further, it also includes the following steps:

[0054] S7. Analyzing the content of carbon and sulfur elements in inorganic metal materials by infrared carbon-sulfur analyzer: Put the weighed sample and flux into a ceramic crucible, place it in the combustion furnace for determination, and run the standard sample at the same time to calculate the results of carbon and sulfur. Measurement range: low carbon: 1 ppm to 0.2%, high carbon: 0.2% to 6%, low sulfur: 1 ppm to 0.3%;

[0055] S8. Analyzing the content of oxygen, nitrogen, and hydrogen elements in inorganic metal materials by oxygen-nitrogen-hydrogen analyzer: Burn the crucible empty several times first, select a suitable standard sample for analysis. If the analysis result meets the requirements, conduct the sample analysis. Put the accurately weighed sample into a graphite crucible, place it in the combustion furnace, and heat and melt it at high temperature in any one of helium or argon gas flows. The instrument conducts the melting analysis of oxygen, nitrogen, and hydrogen according to the automatic analysis process to obtain the content of oxygen, nitrogen, and hydrogen in the sample. Measurement range: low oxygen: 0.1 ppm to 0.5%, high oxygen: 0.5% to 20%, low nitrogen: 0.1 ppm to 0.5%, high nitrogen: 0.5% to 50%, hydrogen: 0.1 ppm to 2000 ppm;

[0056] S9. Analyzing the content of main metal elements by chemical method: Conduct quantitative analysis of the required elements according to the national standard method according to the sample situation;

[0057] S10. Analyze the content of solid bulk metal elements by spark direct-reading spectrometer: First, select a suitable standard sample for calibration according to the sample material. Place the sample on the excitation stage and ensure good contact between the sample and the electrode. Set various parameters of the instrument according to the sample type and the required analysis accuracy. Start the instrument to excite the sample, and the instrument automatically records the spectral data for analysis to obtain the element content;

[0058] Further, the containers in steps S1 and S2 are any one of polytetrafluoroethylene (PTFE), perfluoroalkoxy (PFA), quartz, microwave digestion tank, high-pressure digestion tank (pressure bomb), and borosilicate glass.

[0059] Further, the pretreatment before digestion in steps S1 and S2 is any one of wet digestion (acid digestion), microwave digestion, dry ashing method, high-pressure digestion tank method, alkali fusion method, ultraviolet photolysis, and enzymatic digestion.

[0060] Further, the reagents used for the pretreatment before digestion in steps S1 and S2 are any one of distilled water, inorganic acids, alkaline reagents, and normal salts.

[0061] Further, the pretreatment in step S4 is any one of filtration, dilution, solid-phase extraction (SPE), digestion (decomposition), oxygen bomb combustion, distillation / volatilization, precipitation and complexation, and derivatization.

[0062] Further, the temperature of the combustion furnace in step S6 is 900 °C to 1200 °C, and some samples that are difficult to decompose (such as ceramics or polymer materials) may use a higher temperature (such as 1300 °C).

[0063] Further, the auxiliary solvent in step S7 is any one of tungsten (W), tin (Sn), iron (Fe), tungsten + tin, copper (Cu), or copper oxide (CuO).

[0064] Further, the combustion temperature in step S8 is 2500 °C to 3000 °C.

[0065] Example 1:

[0066] A total element analysis scheme for chemical industrial solid waste is provided:

[0067] As Figure 1 shown, X-ray fluorescence spectrometer (XRF) analysis: Take a certain amount of dry sample for grinding and sample preparation. Put the prepared sample into the sample chamber, set the relevant parameters, start the test, and analyze that the sample contains elements such as Ca, Ti, Fe, Si, Mg, Ba, S, Sb, Al, Na, Mn, K, Zn, Br, Cl, Cr, P, and Ni;

[0068] As Figures 2 - 3As shown in the figure, Energy Dispersive X-ray Spectrometer (EDS) analysis: Take an appropriate amount of the sample and directly stick it onto the conductive adhesive. After sputtering with gold, place it in the sample chamber for testing. The analysis shows that the sample contains elements C, O, Na, Mg, Si, S, Cl, Ca, Ti, Fe, and Br;

[0069] As Figures 4 - 9 shown in the figure, Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) analysis of metal element content: Accurately weigh 0.1 g of the sample into a triangular flask, add 10 mL of nitric acid and 1 mL of perchloric acid, boil it at a high temperature on a hot plate. After complete digestion, transfer the digestion solution to a volumetric flask, rinse the flask wall with distilled water, and transfer the rinsing solution to the volumetric flask together. After volume-fixing to 50 mL, filter it through a 0.45 μm filter membrane and then conduct on-machine testing. At the same time, run the standard curve of metal elements. The analysis shows that the sample contains elements As, Al, B, Ba, Ca, Cr, Cd, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Si, Sn, Sr, Ti, Zn, and Zr;

[0070] As Figure 10 shown in the figure, Inductively Coupled Plasma Mass Spectrometer (ICP-MS) analysis of metal element content: Accurately weigh 0.1 g of the sample into a polytetrafluoroethylene digestion tank, add 5 mL of nitric acid and 2 mL of hydrogen peroxide. Place the digestion tank in a microwave digestion instrument for pretreatment. After complete digestion, transfer the digestion solution to a volumetric flask, rinse the flask wall with distilled water, and transfer it to the volumetric flask together. After volume-fixing to 50 mL, filter it through a 0.45 μm filter membrane and then conduct on-machine testing. At the same time, run the standard curve of metal elements. The analysis shows that the sample contains elements Li, Be, B, P, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ge, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Rh, Pd, Ag, Cd, In, Sn, Cs, La, Ce, Pr, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Re, Au, Tl, Pb, Bi, and Th;

[0071] As Figures 11 - 12 shown in the figure, Element Analyzer (EA) analysis: ① Carbon, hydrogen, nitrogen, and sulfur mode: Accurately weigh 5.42 mg of the sample, wrap it with a tin boat, place it on an automatic sample feeder, add it to a combustion tube at about 1000 °C, inject oxygen, and use oxidation catalysts such as copper oxide and the combustion aid of tin to promote the sample to burn fully and completely. The analysis shows that carbon, hydrogen, nitrogen, and sulfur elements are detected in the sample. ② Oxygen mode: Accurately weigh 5.51 mg of the sample and pyrolyze it in a high-temperature furnace. Carry the pyrolysis products by helium through an activated carbon packed bed coated with nickel or platinum, convert all oxygen into carbon monoxide, and detect the carbon monoxide gas with a thermal conductivity detector to obtain that the sample contains oxygen element;

[0072] AsFigures 13 - 14 As shown in the figure, Ion Chromatography (IC) analysis: Prepare fluoride, chloride, bromide, and iodide solutions with different concentrations, plot the standard curve. Weigh 0.1 g of the sample accurately into a combustion crucible, place the crucible on the support inside the combustion bomb, add white oil, connect the ignition wire. Fill the combustion tank with the absorption solution of sodium carbonate and sodium bicarbonate, place the combustion bomb, charge it with oxygen and ignite. Wait for about half an hour. After releasing the gas, pour the absorption solution into a volumetric flask, rinse the inner wall with distilled water, transfer the washing solution into the volumetric flask as well, add distilled water to make the volume up to 50 mL, filter through a 0.22 μm aqueous membrane, and perform on-machine testing. Analysis shows that the sample contains fluoride, bromide, and chloride ions.

[0073] Example 2:

[0074] A complete elemental analysis solution for metal waste is provided:

[0075] As Figures 15 - 16 shown in the figure, Energy Dispersive X-ray Spectroscopy (EDS) analysis: Take an appropriate amount of the sample and directly stick it onto the conductive adhesive, place it in the sample chamber for testing. Analysis shows that the sample contains Al, Ti, and V elements;

[0076] Spark direct-reading spectrometer analysis: Polish the metal and place it on the excitation stage, and ensure good contact between the sample and the electrode. Set the instrument parameters, start the instrument, start exciting the sample, and the instrument automatically records the spectral data for analysis to obtain the content of elements such as Ti, Al, V, Fe, Cr, etc. in the sample;

[0077] Chemical titration analysis: Dissolve the sample with sulfuric acid + ammonium sulfate, reduce Ti to Ti 4+ under CO protection with an aluminum sheet 3+ , use ammonium ferric sulfate standard solution to titrate Ti 3+ with potassium thiocyanate as the indicator, and calculate the titanium content. According to Part 8 of GB / T 4698.8 - 2017, determine the content of aluminum element by the method of alkali separation - EDTA complexometric titration.

[0078] As Figures 17 - 22 shown in the figure, Inductively Coupled Plasma Optical Emission Spectrometer (ICP - OES) analysis: Weigh 0.1 g of the sample accurately into a polytetrafluoroethylene plastic cup, add 20 mL of aqua regia, 10 mL of sulfuric acid, and 2 mL of hydrofluoric acid, boil at high temperature on a hot plate until completely digested, add saturated boric acid to neutralize the excess hydrofluoric acid. Transfer the digestion solution to a volumetric flask, rinse the bottle wall with distilled water, transfer the rinsing solution to the volumetric flask together, make the volume up to 50 mL, then filter through a 0.45 μm filter membrane and perform on - machine testing. At the same time, run the standard curve of metal elements. For metal elements with high content, dilute the sample by 10 times and then perform on - machine testing. Analysis shows that the sample contains Al, Ca, Cr, Fe, Mg, Mn, Na, Ni, Ti, V elements;

[0079] As shown Figure 23 in the figure, Inductively Coupled Plasma Mass Spectrometry (ICP-MS) analysis: Precisely weigh 0.1 g of the sample, add 2 - 3 drops of distilled water into a polytetrafluoroethylene plastic cup, add 2 mL of hydrofluoric acid, heat and boil for digestion on a hot plate. After complete digestion, transfer the digestion solution to a volumetric flask, rinse the bottle wall with distilled water, transfer it to the volumetric flask together, make up the volume to 100 mL, then filter through a 0.45 μm filter membrane and test on the machine. At the same time, run the standard curve of metal elements. For metal elements with high content, dilute the sample 100 times and then test on the machine. Analysis shows that the sample contains elements such as Na, Mg, Al, P, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Nb, Sn, Cs, Pr, Nd, Ta, W, Pt, Pb, and U;

[0080] As shown Figure 24 in the figure, Carbon and Sulfur Analyzer analysis: Precisely weigh 0.3 g of the sample into a porcelain crucible, add 1.5 g of tungsten granule as a fluxing agent, place it in the instrument for testing, and at the same time select a standard sample for test calibration. The equipment automatically calculates to obtain the carbon and sulfur content in the sample.

[0081] As shown Figures 25 - 27 in the figure, Oxygen, Nitrogen and Hydrogen Analyzer analysis: First, burn the crucible empty several times, select a suitable standard sample for analysis. Precisely weigh 0.2 g of the sample into a graphite crucible and place it in a high-temperature furnace. Melt it under the protection of inert gas helium. At high temperature, oxygen, nitrogen, and hydrogen elements in the sample are released in the form of CO, CO2, N2, and H2. Analysis shows that oxygen, nitrogen, and hydrogen elements are detected in the sample.

[0082] As shown Figure 28 in the figure, Ion Chromatograph (IC) analysis: Precisely weigh 5 g of the sample into a beaker, add 30 mL of distilled water and ultrasonically extract for 24 h. Transfer the extraction solution to a volumetric flask, make up the volume to 50 mL, filter through a 0.22 μm hydrophilic membrane, and test on the machine. Analysis shows that halogen ions are not detected in the sample.

[0083] Example 3:

[0084] A full-element analysis scheme for industrial wastewater is provided:

[0085] As shown Figures 29 - 34As shown, Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) analysis: Accurately weigh 5 mL of the sample into an Erlenmeyer flask, add 20 mL of nitric acid and 2 mL of perchloric acid, boil at high temperature on a hot plate until completely digested. Transfer the digested solution to a volumetric flask, rinse the flask wall with distilled water, transfer the rinsing solution to the volumetric flask as well, make up the volume to 50 mL, then filter through a 0.45 μm filter membrane and conduct on-machine testing. At the same time, run the standard curve of metal elements. It can be analyzed that the sample contains elements such as Ca, K, Mg, Na, Si, and S;

[0086] As Figure 35 shown, Inductively Coupled Plasma Mass Spectrometer (ICP-MS) analysis: Accurately weigh 1 mL of the sample into an Erlenmeyer flask, add 5 mL of nitric acid, heat and boil for digestion on a hot plate. After complete digestion, transfer the digested solution to a volumetric flask, rinse the flask wall with distilled water, transfer it to the volumetric flask together, make up the volume to 50 mL, then filter through a 0.45 μm filter membrane and conduct on-machine testing. At the same time, run the standard curve of metal elements. It can be analyzed that the sample contains elements such as Li, B, Na, Mg, Al, P, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Ge, As, Se, Rb, Sr, Y, Zr, Ag, Cd, Ba, La, Ce, Hf, W, Au, Tl, Pb, Bi, and Th;

[0087] As Figures 36 - 37 shown, Energy Dispersive X-ray Spectrometer (EDS) analysis: Take a certain amount of the sample and dry it in an oven at 105 °C. Take an appropriate amount of the dried powder and directly stick it onto the conductive adhesive, conduct gold spraying treatment, and place it in the sample chamber for testing. It can be analyzed that the sample contains elements such as C, N, O, Na, Mg, Al, Si, S, Cl, K, and Ca;

[0088] As Figure 38 shown, Ion Chromatograph (IC) analysis: Prepare acid radical ions with different concentrations, draw the standard curve. Accurately weigh 0.5 g of the sample into a volumetric flask, make up the volume to 50 mL with distilled water, ultrasonicate for 2 h. Then take 10 mL of the sample and slowly pass it through a sodium-type pretreatment small column, and then through a 0.22 μm aqueous membrane for on-machine testing. It can be analyzed that the sample contains fluoride ions, chloride ions, nitrate ions, and sulfate ions.

[0089] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for comprehensive elemental analysis of unknown waste, characterized in that, Including the following steps: S1. Analyzing the metal element content by inductively coupled plasma optical emission spectrometer (ICP-OES): Weigh the sample accurately in a container, conduct pre-treatment for digestion, make the volume constant, filter through a membrane and then test on the machine. At the same time, run the standard curve to accurately analyze the metal element content, with a detection limit of 5 ppm. S2. Analyzing the metal element content by inductively coupled plasma mass spectrometer (ICP-MS): Weigh the sample accurately in a container, conduct pre-treatment for digestion, make the volume constant, filter through a membrane and then test on the machine. At the same time, run the standard curve to accurately analyze the metal element content, with a detection limit of 10 ppb. S3. Analyzing the element content of 4Be - 92U by energy dispersive X-ray spectrometer (EDS): Directly stick the solid sample onto the conductive adhesive, conduct gold spraying treatment, test on the machine, process and analyze the collected data to obtain the relative content of each element in the sample, with a detection limit of 0.1% - 0.5%. S4. Analyzing the acid radical ion content by ion chromatograph: Prepare acid radical ions (such as fluoride ion, chloride ion, bromide ion and iodide ion, etc.) with different concentrations, draw the standard curve, weigh the sample accurately, conduct pre-treatment, filter through a membrane and then test on the machine to calculate the contents of fluoride ion, chloride ion, bromide ion and iodide ion, etc.

2. The method for full-element analysis of an unknown waste according to claim 1, wherein It also includes the following steps: S5. Analyzing the elements of 11Na - 92U by X-ray fluorescence spectrometer (XRF): Grind and prepare the sample, put the prepared sample into the sample chamber, set the relevant parameters, conduct the test and analyze the element composition and relative content. S6. Analyzing the contents of carbon, hydrogen, oxygen, nitrogen and sulfur elements in organic materials and organic compounds by elemental analyzer (EA): First, set the experimental parameters, conduct tests on blank samples and standard samples first, and then measure the samples after calibration. Put the weighed sample into a special crucible, seal it and place it at the injector position, start the test program, select the corresponding analysis method (such as CHNS mode or O mode), set the parameters (combustion temperature, gas flow rate, etc.), decompose the sample in a high-temperature combustion furnace to generate gases (such as CO2, H2O, N2, SO2, etc.), and after the gases are separated by the chromatographic column, conduct quantitative analysis by the detector (such as thermal conductivity detector TCD), with a detection limit of 100 ppm.

3. The all-element analysis method for an unknown waste as claimed in claim 1, wherein It also includes the following steps: S7. Analyzing the carbon and sulfur element contents in inorganic metal materials by infrared carbon and sulfur analyzer: Put the weighed sample and flux into a ceramic crucible, place it in the combustion furnace for determination, run the standard sample at the same time, calculate the results of carbon and sulfur, with a measurement range: low carbon: 1 ppm - 0.2%, high carbon: 0.2% - 6%, low sulfur: 1 ppm - 0.3%. S8. Analysis of the contents of oxygen, nitrogen and hydrogen elements in inorganic metal materials by an oxygen, nitrogen and hydrogen analyzer: First, the crucible is blank-fired several times, and a suitable standard sample is selected for analysis. If the analysis results meet the requirements, the sample analysis is carried out. The accurately weighed sample is placed in a graphite crucible and placed in a combustion furnace. It is melted by high-temperature heating in any one of helium or argon gas streams. The instrument performs the fusion analysis of oxygen, nitrogen and hydrogen according to the automatic analysis process to obtain the contents of oxygen, nitrogen and hydrogen in the sample. The measurement ranges are as follows: low oxygen: 0.1 ppm - 0.5%, high oxygen: 0.5% - 20%, low nitrogen: 0.1 ppm - 0.5%, high nitrogen: 0.5% - 50%, hydrogen: 0.1 ppm - 2000 ppm; S9. Analysis of the contents of main metal elements by chemical method: Quantitative analysis of the required elements is carried out according to the national standard method according to the sample situation; S10. Analysis of the contents of solid block metal elements by spark direct-reading spectrometer: First, a suitable standard sample is selected for calibration according to the sample material. The sample is placed on the excitation stage and it is ensured that the sample is in good contact with the electrode. According to the sample type and the required analysis accuracy, various parameters of the instrument are set. The instrument is started and the sample is excited. The instrument automatically records the spectral data for analysis to obtain the element contents.

4. The method for comprehensive elemental analysis of an unknown waste according to claim 1, characterized in that, The containers in steps S1 and S2 are any one of polytetrafluoroethylene (PTFE), perfluoroalkoxy (PFA), quartz, microwave digestion tank, high-pressure digestion tank (pressure bomb), and borosilicate glass.

5. The method for comprehensive elemental analysis of an unknown waste according to claim 1, characterized in that, The pretreatment before digestion in steps S1 and S2 is any one of wet digestion (acid digestion), microwave digestion, dry ashing method, high-pressure digestion tank method, alkali fusion method, ultraviolet photolysis, and enzymatic digestion.

6. The method for comprehensive elemental analysis of an unknown waste according to claim 1, characterized in that, The reagents used for the pretreatment before digestion in steps S1 and S2 are any one of distilled water, inorganic acids, alkaline reagents, and normal salts.

7. A method for the complete elemental analysis of an unknown waste, as claimed in claim 1, wherein The pretreatment in step S4 is any one of filtration, dilution, solid-phase extraction (SPE), digestion (decomposition), oxygen bomb combustion, distillation / volatilization, precipitation and complexation, and derivatization.

8. The method for comprehensive elemental analysis of an unknown waste according to claim 2, characterized in that, The temperature of the combustion furnace in step S6 is 900°C - 1200°C. For some samples that are difficult to decompose (such as ceramics or polymer materials), a higher temperature (such as 1300°C) may be used.

9. The method for comprehensive elemental analysis of an unknown waste according to claim 3, characterized in that, The flux in step S7 is any one of tungsten (W), tin (Sn), iron (Fe), tungsten + tin, copper (Cu), or copper oxide (CuO).

10. The method for comprehensive elemental analysis of an unknown waste according to claim 3, characterized in that, The combustion temperature in step S8 is 2500°C - 3000°C.

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