CN116879380A - Quantitative detection method for thallium content in converter graphite nodules - Google Patents
Quantitative detection method for thallium content in converter graphite nodules Download PDFInfo
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- 229910052716 thallium Inorganic materials 0.000 title claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 68
- 239000010439 graphite Substances 0.000 title claims abstract description 68
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 239000012086 standard solution Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
- 229910052738 indium Inorganic materials 0.000 claims description 17
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000011088 calibration curve Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000011550 stock solution Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 230000000391 smoking effect Effects 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 5
- 238000004445 quantitative analysis Methods 0.000 claims 14
- 238000004090 dissolution Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 150000003475 thallium Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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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
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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
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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Abstract
A quantitative detection method for thallium content in converter graphite nodules comprises the following steps: 1) Pretreatment of converter graphite nodules; 2) Preparing a standard solution series; 3) And detecting the thallium content in the converter graphite nodules. The invention discovers that the pretreatment method is suitable for converter graphite nodules, namely the method is simple, convenient, quick and strong in operability, and the method can completely dissolve the converter graphite nodules, thereby improving the stability of quantitative determination of thallium content in the converter graphite nodules; the method is suitable for quantitative detection of thallium content in the converter graphite nodules with thallium content not less than 0.0062 mug/L, and the thallium recovery rate is up to 99.1%; the analysis accuracy is high; the detection lower limit is as low as ppb level, and the sensitivity is high; has the advantages of simple operation, simple analysis condition and low labor intensity. Therefore, the invention has obvious economic benefit and has the advantages of simplicity, convenience and economy.
Description
Technical Field
The invention belongs to the technical field of trace detection, and particularly relates to a quantitative detection method for thallium content in converter graphite nodules.
Background
Thallium element is a highly toxic radioactive element, and can enter human body through food, water and breath, so that health is damaged, and when thallium content exceeds 12 mg/kg in human body, death can even be caused. Therefore, there are strict control standards for thallium element emissions. The converter graphite nodule is used as an important raw material in iron and steel smelting, and has the advantages of high carbon content, high temperature resistance, high conductivity, etc. and may be used widely in steel smelting, refractory material and conducting material. In order to control the thallium content from the source, the detection of the thallium content in the graphite nodules is of great importance.
At present, no patent is available about a method for detecting thallium element in graphite spheres and a method for dissolving thallium element, and the method for detecting thallium element comprises a graphite furnace atomic absorption spectrometry, an inductively coupled plasma emission spectrometry and a spectrophotometry, but the method has the defects of complex operation, long experimental period, high detection limit and the like, and cannot meet the detection requirement. In order to monitor and control thallium in the converter graphite nodules, a rapid, accurate, low detection limit quantitative detection method must be developed.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a quantitative detection method for thallium content in converter graphite nodules.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a quantitative detection method for thallium content in converter graphite nodules comprises the following steps:
1) Pretreatment of converter graphite nodules: placing the converter graphite nodules in a muffle furnace 750 o C～850 o C, pre-burning is carried out for 1 hour; taking out, cooling, transferring to polytetrafluoroethylene beaker, sequentially adding analytically pure substances with purity gradeAnd hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid 5-10 mL, 5-10 mL, 2-8 mL, 2-5 mL are dissolved at low temperature, the volume is concentrated after smoking, the slightly cooled product is taken down, and dilute nitric acid is added to dissolve salts; taking down, cooling to room temperature, and uniformly mixing after constant volume by deionized water;
2) Preparation of a standard solution series:
preparation of thallium standard solution series: removing dilute nitric acid to pave the bottom, removing Tl standard stock solutions with different contents of 1000 mug/mL according to the dilution ratio, fixing the volume by deionized water, and shaking uniformly to prepare the solution with concentration gradients of 0 mug/L, 0.1 mug/L, 0.3 mug/L, 0.5 mug/L, 0.7 mug/L, 1.0 mug/L, 5.0 mug/L and 10.0 mug/L;
preparing an indium internal standard solution: transferring 10 mug/mL of indium standard solution by a liquid transferring gun, fixing the volume by deionized water, and shaking uniformly to prepare 5 mug/L of indium internal standard solution;
(3) Detecting thallium content in the converter graphite nodules: and (3) taking the indium standard solution in the step (2) as an internal standard, taking 205Tl as a measurement isotope in an oxygen reaction mode, respectively measuring the series thallium standard solution in the step (2) and the converter graphite nodule solution in the step (1) by an inductively coupled plasma mass spectrometry, establishing a calibration curve equation, and then calculating the thallium content in the converter graphite nodule in the wastewater according to the standard curve equation.
Preferably, the particle size of the converter graphite nodules in step (1) is 0.125.ltoreq. 0.125 mm.
Preferably, the addition amount and concentration of the dilute nitric acid in the step (1) and the step (2) are 20-mL and 10-50%.
Preferably, the amount of 1000. Mu.g/mL Tl standard stock solution removed in step (2) is 0. Mu.L, 10. Mu.L, 30. Mu.L, 50. Mu.L, 70. Mu.L, 0.1. 0.1mL, 0.5. 0.5mL, 1. 1mL.
Preferably, the constant volume in step (2) is 100mL.
Preferably, the amount of the indium internal standard solution removed and the volume of the indium internal standard solution to be removed in the step (2) are respectively 0.5mL and 1000mL.
Preferably, the mass spectrometer operating parameters in step (3) are: the auxiliary air flow is 0.8-0.9L/min, the atomization air flow is 0.9-1.0L/min, the cooling air flow is 10-20L/min, the oxygen flow is 0.5-0.8L/min, and the power is 800-1000W.
Further, the specific steps of detecting thallium ion concentration in the converter graphite nodules by inductively coupled plasma mass spectrometry in the step (3) are as follows:
under the optimized experimental condition, respectively measuring the intensity values of the converter graphite nodule to-be-measured liquid and a series of thallium ion standard solutions by using an inductively coupled plasma mass spectrometry method, and using the mass concentration of Tl elementx(%) is the abscissa, the ratio of signal intensity of Tl element to internal standard element InI(cps) is ordinate, a calibration curve is established, and the regression equation of the calibration curve isI（cps）=ax(%) +b, the linear correlation coefficient is R. In the equation, a and b are constants; and substituting the signal intensity ratio of the liquid to be measured into a standard equation, and finally calculating the thallium content in the liquid to be measured.
The invention has the following advantages and beneficial effects:
(1) The invention discovers that the pretreatment method is suitable for converter graphite nodules, namely the method is simple, convenient, quick and strong in operability, and the method can completely dissolve the converter graphite nodules, thereby improving the stability of quantitative determination of thallium content in the converter graphite nodules; the method is suitable for quantitative detection of thallium content in the converter graphite nodules with thallium content not lower than 0.0062 mug/L, and the thallium recovery rate is as high as 99.1%.
(2) In the process of detecting the thallium content, the accuracy of quantitative detection of the thallium content In the converter graphite nodules is improved In the following way, namely under the optimal working condition, the influence of a matrix effect is eliminated by eliminating a carbon matrix through burning pretreatment and controlling the mass concentration of the matrix, the mass spectrum interference is eliminated by adopting an oxygen reaction mode and selecting 205Tl isotopes, and the analysis accuracy is improved through In internal standard correction.
(3) The thallium concentration in the solution to be detected of the graphite nodule in the transfer furnace is detected by adopting an inductively coupled plasma mass spectrometry, and compared with a graphite furnace atomic absorption spectrometry and an ICP-OES (inductively coupled plasma emission spectrometry), the solution to be detected has a lower detection lower limit, can be as low as ppb level, and has higher sensitivity; compared with spectrophotometry, the method has the advantages of simpler operation, simpler analysis conditions and lower labor intensity. Therefore, the invention has obvious economic benefit and has the advantages of simplicity, convenience and economy.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1: quantitative detection method for thallium content in converter graphite nodules
The method comprises the following steps:
(1) Pretreatment of converter graphite nodules: placing the converter graphite nodules in a muffle furnace at 750 o C, pre-burning for 1 hour, taking out, cooling, transferring to a polytetrafluoroethylene beaker, sequentially adding 5mL hydrochloric acid, dissolving for 10 minutes at low temperature, adding 5mL nitric acid, 2 mL hydrofluoric acid, dissolving for 10 minutes at low temperature, adding 2 mL perchloric acid, heating to dissolve, concentrating to 1mL after smoking, taking down slightly cool, adding 20mL of 10% dilute nitric acid dissolved salts, taking down, cooling to room temperature, fixing the volume to 100mL by deionized water, and uniformly mixing.
(2) Preparing a standard solution: preparation of thallium standard solution series: removing dilute nitric acid to pave the bottom, and respectively removing 0 muL, 10 muL, 30 muL, 50 muL, 70 muL, 0.1mL, 0.5mL and 1mL of 1000 mug/mL Tl standard stock solution according to the dilution ratio, and shaking uniformly after the constant volume of deionized water to prepare thallium standard solutions with different concentration gradients:
indium internal standard solution (5. Mu.g/L): a pipette was used to remove 0.5mL of a 10. Mu.g/mL indium standard solution, and deionized water was used to determine the volume to 1000mL, and then shaking was performed.
(3) Detecting thallium content in the converter graphite nodules: and under an oxygen reaction mode, using 205Tl as a measurement isotope, respectively measuring a series of thallium standard solutions and converter graphite nodule solutions by an inductively coupled plasma mass spectrometry method, establishing a calibration curve equation, and calculating the thallium content in the converter graphite nodule in the wastewater according to the standard curve equation. The measurement working parameters of the mass spectrometer are as follows: auxiliary air flow rate is 0.8L/min, atomization air flow rate is 0.9L/min, cooling air flow rate is 10L/min, oxygen flow rate is 0.5L/min, and power is 800W.
The thallium standard curve is thus plotted: and (3) taking the mass concentration x (%) of the Tl element as an abscissa and the signal intensity ratio I (cps) of the Tl element and the internal standard element In as an ordinate, and establishing a calibration curve, wherein the regression equation of the calibration curve is I (cps) = 90802x (%) +84 (R= 0.9992).
Substituting the signal intensity value of the liquid to be measured into a standard equation to calculate that the thallium content concentration in the liquid to be measured of the converter graphite nodule is 0.0188 mug/L, and the calculated recovery rate is 97.5%.
The recovery rate calculation formula is:
11 parallel experiments were carried out in the above-described manner to obtain a mean concentration of thallium content in the test solution of converter graphite nodules of 0.0188. Mu.g/L, a relative standard deviation RSD (n=11) of 1.6%, and a calculated recovery of 97.5%. The detection method provided by the invention has higher accuracy and precision.
Example 2: quantitative detection method for thallium content in converter graphite nodules
The method comprises the following steps:
(1) Pretreatment of converter graphite nodules: placing the converter graphite nodules in a muffle furnace at 750 o C, pre-burning for 1 hour, taking out, cooling, transferring to a polytetrafluoroethylene beaker, sequentially adding 5mL hydrochloric acid, dissolving for 10 minutes at low temperature, adding 5mL nitric acid, 2 mL hydrofluoric acid, dissolving for 10 minutes at low temperature, adding 2 mL perchloric acid, heating to dissolve, concentrating to 1mL after smoking, taking down slightly cool, adding 20mL of 50% dilute nitric acid dissolved salts, taking down, cooling to room temperature, fixing the volume to 100mL by deionized water, and uniformly mixing.
(2) Preparing a standard solution:
preparation of thallium standard solution series: removing dilute nitric acid to pave the bottom, and respectively removing 0 muL, 10 muL, 30 muL, 50 muL, 70 muL, 0.1mL, 0.5mL and 1mL of 1000 mug/mL Tl standard stock solution according to the dilution ratio, and shaking uniformly after the constant volume of deionized water to prepare thallium standard solutions with different concentration gradients;
indium internal standard solution (5. Mu.g/L): a pipette was used to remove 0.5mL of a 10. Mu.g/mL indium standard solution, and deionized water was used to determine the volume to 1000mL, and then shaking was performed.
(3) Detecting thallium content in the converter graphite nodules: and under an oxygen reaction mode, using 205Tl as a measurement isotope, respectively measuring a series of thallium standard solutions and converter graphite nodule solutions by an inductively coupled plasma mass spectrometry method, establishing a calibration curve equation, and calculating the thallium content in the converter graphite nodule in the wastewater according to the standard curve equation. The measurement working parameters of the mass spectrometer are as follows: auxiliary air flow rate is 0.9L/min, atomization air flow rate is 1.0L/min, cooling air flow rate is 20L/min, oxygen flow rate is 0.8L/min, and power is 1100W.
The thallium standard curve is thus plotted: and (3) taking the mass concentration x (%) of the Tl element as an abscissa and the signal intensity ratio I (cps) of the Tl element and the internal standard element In as an ordinate, and establishing a calibration curve, wherein the regression equation of the calibration curve is I (cps) = 11367x (%) +9 (R=0.9994).
Substituting the signal intensity value of the liquid to be measured into a standard equation to calculate that the thallium content concentration in the liquid to be measured of the converter graphite nodule is 0.0113 mug/L, and the calculated recovery rate is 96.9%.
Example 3: quantitative detection method for thallium content in converter graphite nodules
The method comprises the following steps:
(1) Pretreatment of converter graphite nodules: the converter graphite nodules were placed in a muffle furnace at 850 f o C, pre-burning for 1 hour, taking out, cooling, transferring to a polytetrafluoroethylene beaker, sequentially adding 10 mL hydrochloric acid, dissolving for 10 minutes at low temperature, adding 10 mL nitric acid, 8 mL hydrofluoric acid, dissolving for 10 minutes at low temperature, adding 5mL perchloric acid, heating to dissolve, concentrating to 1mL after smoking, taking down slightly cool, adding 20mL 50% dilute nitric acid dissolved salts, taking down, cooling to room temperature, fixing the volume to 100mL by deionized water, and uniformly mixing.
(2) Preparation of standard solution
Preparation of thallium standard solution series: removing dilute nitric acid to pave the bottom, and respectively removing 0 muL, 10 muL, 30 muL, 50 muL, 70 muL, 0.1mL, 0.5mL and 1mL of 1000 mug/mL Tl standard stock solution according to the dilution ratio, and shaking uniformly after the constant volume of deionized water to prepare thallium standard solutions with different concentration gradients;
indium internal standard solution (5. Mu.g/L): a pipette was used to remove 0.5mL of a 10. Mu.g/mL indium standard solution, and deionized water was used to determine the volume to 1000mL, and then shaking was performed.
(3) Detecting thallium content in the converter graphite nodules: and under an oxygen reaction mode, using 205Tl as a measurement isotope, respectively measuring a series of thallium standard solutions and converter graphite nodule solutions by an inductively coupled plasma mass spectrometry method, establishing a calibration curve equation, and calculating the thallium content in the converter graphite nodule in the wastewater according to the standard curve equation. The measurement working parameters of the mass spectrometer are as follows: auxiliary air flow rate is 0.9L/min, atomization air flow rate is 0.9L/min, cooling air flow rate is 15L/min, oxygen flow rate is 0.8L/min, and power is 1000W.
The thallium standard curve is thus plotted: and (3) taking the mass concentration x (%) of the Tl element as an abscissa and the signal intensity ratio I (cps) of the Tl element and the internal standard element In as an ordinate, and establishing a calibration curve, wherein the regression equation of the calibration curve is I (cps) = 67820x (%) +48 (R=0.9998).
Substituting the signal intensity value of the liquid to be measured into a standard equation to calculate that the thallium content concentration in the liquid to be measured of the converter graphite nodule is 0.0378 mug/L, and the calculated recovery rate is 99.1%.
The above examples only show a few embodiments of the present invention, which are described in detail and are not to be construed as limiting the scope of the invention, but all the technical solutions obtained by equivalent substitution or equivalent transformation shall fall within the scope of the invention.
Claims (8)
1. The quantitative detection method for the thallium content in the converter graphite nodule is characterized by comprising the following steps:
1) Pretreatment of converter graphite nodules: placing the converter graphite nodules in a muffle furnace 750 o C～850 o C, pre-burning for 1 hour; taking out, cooling, transferring to a polytetrafluoroethylene beaker, sequentially adding hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid with the purity grade of analytical purity or above 5-10 mL, 5-10 mL, 2-8 mL and 2-5 mL respectively for low-temperature dissolution, concentrating the volume after smoking, taking down slightly cooled, and adding dilute nitric acid to dissolve salts; taking down, cooling to room temperature, and uniformly mixing after constant volume by deionized water;
2) Preparation of a standard solution series:
preparation of thallium standard solution series: removing dilute nitric acid to pave the bottom, removing Tl standard stock solutions with different contents of 1000 mug/mL according to the dilution ratio, fixing the volume by deionized water, and shaking uniformly to prepare the solution with concentration gradients of 0 mug/L, 0.1 mug/L, 0.3 mug/L, 0.5 mug/L, 0.7 mug/L, 1.0 mug/L, 5.0 mug/L and 10.0 mug/L;
preparing an indium internal standard solution: transferring 10 mug/mL of indium standard solution by a liquid transferring gun, fixing the volume by deionized water, and shaking uniformly to prepare 5 mug/L of indium internal standard solution;
(3) Detecting thallium content in the converter graphite nodules: and (3) taking the indium standard solution in the step (2) as an internal standard, taking 205Tl as a measurement isotope in an oxygen reaction mode, respectively measuring the series thallium standard solution in the step (2) and the converter graphite nodule solution in the step (1) by an inductively coupled plasma mass spectrometry, establishing a calibration curve equation, and then calculating the thallium content in the converter graphite nodule in the wastewater according to the standard curve equation.
2. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the granularity of the converter graphite nodules in the step (1) is less than or equal to 0.125 and mm.
3. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the addition amount and concentration of the dilute nitric acid in the step (1) and the step (2) are 20mL and 10% -50%.
4. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the amount of 1000. Mu.g/mL Tl standard stock solution in step (2) was 0. Mu.L, 10. Mu.L, 30. Mu.L, 50. Mu.L, 70. Mu.L, 0.1mL, 0.5mL, 1mL.
5. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the constant volume in the step (2) is 100mL.
6. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the removal amount and the constant volume of the indium internal standard solution in the step (2) are respectively 0.5mL and 1000mL.
7. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: the mass spectrometer operating parameters described in step (3) are: the auxiliary air flow is 0.8-0.9L/min, the atomization air flow is 0.9-1.0L/min, the cooling air flow is 10-20L/min, the oxygen flow is 0.5-0.8L/min, and the power is 800-1000W.
8. The quantitative determination method for the thallium content in the converter graphite nodules of claim 1, wherein the quantitative determination method is characterized by comprising the following steps: in the step (3), the specific steps of detecting the thallium ion concentration in the converter graphite nodule by adopting the inductively coupled plasma mass spectrometry are as follows:
under the optimized experimental condition, respectively measuring the intensity values of the converter graphite nodule to-be-measured liquid and a series of thallium ion standard solutions by using an inductively coupled plasma mass spectrometry method, and using the mass concentration of Tl elementx(%) is the abscissa, the ratio of signal intensity of Tl element to internal standard element InI(cps) is ordinate, a calibration curve is established, and the regression equation of the calibration curve isI（cps）=ax(%) +b, the linear correlation coefficient is R; in the equation, a and b are constants; and substituting the signal intensity ratio of the liquid to be measured into a standard equation, and finally calculating the thallium content in the liquid to be measured.
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