Method for improving stability of electronic grade hydrofluoric acid metal detection

Abstract

The invention provides a method for improving the metal content detection stability of electronic grade hydrofluoric acid, the content of trace metals in the electronic grade hydrofluoric acid is detected by inductively coupled plasma mass spectrometry (ICP-MS), the trace metals comprise 30 elements of Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd and Ta, and the standard deviations of the 30 metal elements are all less than 0.33 ppt.

Description

Technical Field

[0001] This invention relates to the field of electronic-grade hydrofluoric acid metal detection, and more specifically to a method for improving the stability of electronic-grade hydrofluoric acid metal detection. Background Technology

[0002] Electronic-grade hydrofluoric acid, as one of the key basic chemical materials in the microelectronics industry, is widely used in large-scale integrated circuits, mainly for chip cleaning and etching. It can also be used as an analytical reagent and for preparing high-purity etching solutions. Its purity and cleanliness have a significant impact on the yield, electrical performance, and reliability of integrated circuits. With the rapid development of the semiconductor industry and continuous industrial upgrading, the demand for high-quality electronic-grade hydrofluoric acid is increasing year by year. Currently, the most advanced hydrofluoric acid production and testing technologies in the world can only achieve a limit of 1 ppt, but ensuring high stability in testing is also crucial to maintaining leading product quality. Summary of the Invention

[0003] This invention provides a method to improve the stability of trace metal content detection in electronic-grade hydrofluoric acid. It employs a unique sample processing technology to ensure that the standard deviation of the results of 10 consecutive tests of the same sample on the same day and 10 consecutive tests of the same sample over 10 days for the 30 main cations of electronic-grade hydrofluoric acid is <0.33ppt.

[0004] A method for improving the stability of metal content detection in electronic-grade hydrofluoric acid is disclosed, which employs inductively coupled plasma mass spectrometry (ICP-MS) to detect trace metal content in electronic-grade hydrofluoric acid. The trace metals include 30 elements: Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd, and Ta.

[0005] Furthermore, when using inductively coupled plasma mass spectrometry (ICP-MS) to detect trace metal content in electronic-grade hydrofluoric acid, the specific detection modes employed are as follows: Nogas mode is used to detect Be and B; O2 mode is used to detect Pd, In, Tl, and Pb; Cool mode is used to detect Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag; Ti mode is used to detect Ti, V, Zn, and As; and He mode is used to detect Zr, Nb, Mo, Cd, and Ta.

[0006] Furthermore, the detection includes the following steps: A. Sampling: A1. The sample bottle is filled 2-4 / 5 full with SG grade hydrofluoric acid; A2. With the bottle opening facing down, shake the bottle up and down; then rotate it 120°, 240° and 360° in sequence, shaking the bottle after each rotation; A3. With the bottle opening facing upwards, shake the bottle up and down; then rotate it 120°, 240° and 360° in sequence, shaking the bottle after each rotation; A4. With the bottle opening facing down, tilt the bottle and rotate it while pouring until the hydrofluoric acid is emptied. A5. Repeat steps A1 to A4 three times; B. ICP-MS injection: B1. Using the standard addition method, draw a standard curve; B2. The sample to be tested is injected, and the results of 30 elements, namely Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd, and Ta, are obtained through a standard curve.

[0007] Furthermore, the sample introduction system, nebulization system, platinum cone, and rectangular tube of the platinum center tube of the ICP-MS are all made of hydrofluoric acid resistant material.

[0008] Furthermore, the shaking time for each bottle is 20-40 seconds.

[0009] Furthermore, the SG grade hydrofluoric acid is a 10ppt grade hydrofluoric acid.

[0010] Furthermore, the standard curve described in step B1 uses the undiluted 49% HF sample as a substrate and employs the standard addition method to establish standard curves with spikes of 0 / 10 / 20 / 30 / 50 ppt. The specific establishment steps are as follows: 1) Spike 0ppt: Place a 100ml PFA bottle on a balance and tare it. In a clean bench, pour clean 49%HF sample into the bottle. The balance does not return to zero. Test on the instrument. 2) Add 10ppt: After the 0ppt test is completed, accurately weigh the remaining sample in the sample bottle, calculate the weight of the 1ppb standard solution to be added, add the standard solution to the remaining sample, and then test it on the instrument. 3) Following the method in step 2), perform the scalar point test with 20, 30, and 50 ppt in sequence, and obtain the standard curve based on the test results; the R value of the standard curve must be >0.995 to be used.

[0011] Furthermore, when using Nogas mode to detect elements Be and B, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1500W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: 2-6V, extraction lens 2: -150~-120V, Omega deflection voltage: -160~-70V, Omega lens voltage: 12-13V, octupole deflection voltage: -20~-5V, octupole RF: 120-180V, energy discrimination: 5-6V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using O2 mode to detect elements Pd, In, Tl, and Pb, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1550W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: 2-6V, extraction lens 2: -70~-120V, Omega deflection voltage: -160~-70V, Omega lens voltage: 12-15V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, oxygen flow rate: 20mL / min, octupole deflection voltage: -10~-5V, octupole RF: 120-180V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using Cool mode to detect elements Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 20mm, nebulizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.6-1.2L / min, extraction lens 1: -120~-90V, extraction lens 2: -40V~-5V, Omega deflection voltage: -70~-50V, Omega lens voltage: 2~8V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 0mL / min, octupole deflection voltage: -20~-8V, octupole RF: 120-150V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using Ti mode to detect elements Ti, V, Zn, and As, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 17mm, nebulizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: -100~ -70V, extraction lens 2: -10~ -20V, Omega deflection voltage: -190~ -100V, Omega lens voltage: 10~ 20V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 15mL / min, octupole deflection voltage: -10~ -2V, octupole RF: 100~ 180V, energy discrimination: -5~ 5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using He mode to detect elements Zr, Nb, Mo, Cd, and Ta, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1200W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: -160~-140V, extraction lens 2: -10~-20V, Omega deflection voltage: -190~-100V, Omega lens voltage: 10~20V, helium flow rate: 5mL / min, hydrogen flow rate: 1mL / min, octupole deflection voltage: -16V, octupole RF: 150~170V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm.

[0012] Furthermore, when using Nogas mode to detect elements Be and B, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1500W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.51L / min, extraction lens 1: 4V, extraction lens 2: -127V, Omega deflection voltage: -158V, Omega lens voltage: 12.9V, helium flow rate: 0, hydrogen flow rate: 0, ammonia-helium mixture flow rate: 0, oxygen flow rate: 0, octupole deflection voltage: -9V, octupole RF: 126V, energy discrimination: 5.1V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm; When using O2 mode to detect elements Pd, In, Tl, and Pb, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1550W, sampling depth: 8mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.55L / min, extraction lens 1: 3.9V, extraction lens 2: -80.5V, Omega deflection voltage: -148V, Omega lens voltage: 14V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 20mL / min, octupole deflection voltage: -3V, octupole RF: 140V, energy discrimination: -3.4V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm; When using Cool mode to detect elements Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 20mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.92L / min, extraction lens 1: -90V, extraction lens 2: -33.5V, Omega deflection voltage: -46V, Omega lens voltage: 2.7V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 0mL / min, octupole deflection voltage: -8V, octupole RF: 120V, energy discrimination: -5.1V, torch horizontal position: -0.9mm, torch vertical position: -0.5mm; When using Ti mode to detect elements Ti, V, Zn, and As, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 17mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.55L / min, extraction lens 1: -91V, extraction lens 2: -15V, Omega deflection voltage: -185V, Omega lens voltage: 14V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 15mL / min, octupole deflection voltage: -4.3V, octupole RF: 175V, energy discrimination: -6.3V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm; When using He mode to detect elements Zr, Nb, Mo, Cd, and Ta, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1200W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.48L / min, extraction lens 1: -154.1V, extraction lens 2: -19V, Omega deflection voltage: -161V, Omega lens voltage: 13.5V, helium flow rate: 5mL / min, hydrogen flow rate: 1mL / min, ammonia-helium mixture flow rate: 0, oxygen flow rate: 0, octupole deflection voltage: -16V, octupole RF: 170V, energy discrimination: -3V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm.

[0013] Furthermore, the sample vial is a PFA sample vial.

[0014] Compared with existing technologies, the advantages of this invention are as follows: the testing method provided by this invention can accurately and stably detect key metal elements in ppt-grade hydrofluoric acid, with the standard deviation of all 30 metal elements being <0.33 ppt. The more stable hydrofluoric acid testing technology provided by this invention is beneficial to ensuring the continuous improvement of the quality of ultra-high purity hydrofluoric acid. Attached Figure Description

[0015] Figure 1 The standard curves for the first 16 of the 30 key elements in this invention.

[0016] Figure 2 The standard curves for the last 14 of the 30 key elements in this invention. Detailed Implementation

[0017] The embodiments of the present invention will be described in detail below with reference to the examples. The following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention.

[0018] Example 1 A method for improving the stability of trace metal content detection in electronic-grade hydrofluoric acid, the specific detection method includes the following steps: A. Sampling: A1. The sample bottle is filled 2-4 / 5 full with SG grade hydrofluoric acid (10ppt grade hydrofluoric acid); A2. With the bottle opening facing down, shake the bottle up and down for 20-40 seconds; then rotate it 120°, 240° and 360° in sequence, shaking the bottle for 20-40 seconds after each rotation; A3. With the bottle opening facing upwards, shake the bottle up and down for 20-40 seconds; then rotate it 120°, 240° and 360° in sequence, shaking the bottle for 20-40 seconds after each rotation; A4. With the bottle opening facing down, tilt the bottle and rotate it while pouring until the hydrofluoric acid is emptied. A5. Repeat steps A1 to A4 three times; B. ICP-MS injection: B1. Using the undiluted 49% HF sample as the substrate, establish standard curves for spiked 0 / 10 / 20 / 30 / 50 ppt using the standard addition method. The specific steps are as follows: 1) Spike 0ppt: Place a 100ml PFA bottle on a balance and tare it. In a clean bench, pour clean 49% HF sample into the bottle. The balance will not return to zero. Test on the instrument. 2) Add 10ppt: After the 0ppt test is completed, accurately weigh the remaining sample in the sample bottle, calculate the weight of the 1ppb standard solution to be added, add the standard solution to the remaining sample, and then test it on the instrument. 3) Following the method in step 2), perform the spike point test with 20, 30, and 50 ppt in sequence, and obtain the standard curve based on the test results; the R value of the standard curve must be >0.995 to be usable; B2. The sample to be tested is injected, and the results of 30 elements, namely Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd, and Ta, are obtained through a standard curve.

[0019] The sample introduction system, nebulization system, platinum cone, and rectangular tube of the platinum center tube of the ICP-MS are all made of hydrofluoric acid resistant material.

[0020] The instrument parameter settings for the ICP-MS sample injection test are shown in Table 1 below: Table 1

[0021] Spike recovery test (20 ppt spiked, recovery rate calculated): Place a 100ml PFA bottle on a balance and tare it. In a clean bench, pour clean 49% HF sample into the bottle. Do not zero the balance. Test the sample. After the test, accurately weigh the remaining sample in the bottle and calculate the weight of 1ppb standard solution to be added. Add the standard solution to the remaining sample and test the sample. Calculate the spiked recovery rate, which should be between 75% and 125%. The recovery rates are shown in Table 2 below.

[0022] Table 2

[0023] The standard deviations were calculated for 10 consecutive injections of the same sample on the same day and for 10 consecutive injections of the same sample over 10 days. The results are shown in Tables 3 and 4.

[0024] Table 3. Ten consecutive tests conducted on the same sample bottle on the same day.

[0025] Table 4. Continuous testing of the same bottle sample over 10 days

[0026] The data above show that the method for detecting trace metal content in ppt-grade hydrofluoric acid provided by this invention has high stability. When the same sample is injected 10 times on the same day, and the same bottle of sample is injected for 10 consecutive days, the standard deviation of the detected content of 30 trace metal elements in ppt-grade hydrofluoric acid is <0.33ppt.

Claims

1. A method for improving the stability of metal content detection in electronic-grade hydrofluoric acid, characterized in that, The trace metal content in electronic-grade hydrofluoric acid was determined by inductively coupled plasma mass spectrometry (ICP-MS). The trace metals included 30 elements: Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd, and Ta.

2. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 1, characterized in that, When using inductively coupled plasma mass spectrometry (ICP-MS) to detect trace metal content in electronic-grade hydrofluoric acid, the specific detection modes employed are as follows: Nogas mode is used to detect Be and B; O2 mode is used to detect Pd, In, Tl, and Pb; Cool mode is used to detect Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag; Ti mode is used to detect Ti, V, Zn, and As; and He mode is used to detect Zr, Nb, Mo, Cd, and Ta.

3. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 1, characterized in that, Includes the following steps: A. Sampling: A1. The sample bottle is filled 2-4 / 5 full with SG grade hydrofluoric acid; A2. With the bottle opening facing down, shake the bottle up and down; then rotate it 120°, 240° and 360° in sequence, shaking the bottle after each rotation; A3. With the bottle opening facing upwards, shake the bottle up and down; then rotate it 120°, 240° and 360° in sequence, shaking the bottle after each rotation; A4. With the bottle opening facing down, tilt the bottle and rotate it while pouring until the hydrofluoric acid is emptied. A5. Repeat steps A1 to A4 three times; B. ICP-MS injection: B1. Using the standard addition method, draw a standard curve; B2. The sample to be tested is injected, and the results of 30 elements, namely Be, B, Pd, In, Tl, Pb, Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, Ag, Ti, V, Zn, As, Zr, Nb, Mo, Cd, and Ta, are obtained through a standard curve.

4. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, The sample introduction system, nebulization system, platinum cone, and rectangular tube of the platinum center tube of the ICP-MS are all made of hydrofluoric acid resistant material.

5. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, The shaking time for each bottle is 20-40 seconds.

6. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, The SG grade hydrofluoric acid is a 10ppt grade hydrofluoric acid.

7. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, The standard curve described in step B1 uses an undiluted 49% HF sample as the substrate and employs the standard addition method to establish standard curves with spikes of 0 / 10 / 20 / 30 / 50 ppt. The specific steps for establishing these curves are as follows: 1) Spike 0ppt: Place a 100ml PFA bottle on a balance and tare it. In a clean bench, pour clean 49%HF sample into the bottle. The balance does not return to zero. Test on the instrument. 2) Add 10ppt: After the 0ppt test is completed, accurately weigh the remaining sample in the sample bottle, calculate the weight of the 1ppb standard solution to be added, add the standard solution to the remaining sample, and then test it on the instrument. 3) Following the method in step 2), perform the scalar point test with 20, 30, and 50 ppt in sequence, and obtain the standard curve based on the test results; the R value of the standard curve must be >0.995 to be used.

8. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, When using Nogas mode to detect elements Be and B, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1500W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: 2-6V, extraction lens 2: -150~-120V, Omega deflection voltage: -160~-70V, Omega lens voltage: 12-13V, octupole deflection voltage: -20~-5V, octupole RF: 120-180V, energy discrimination: 5-6V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using O2 mode to detect elements Pd, In, Tl, and Pb, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1550W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: 2-6V, extraction lens 2: -70~-120V, Omega deflection voltage: -160~-70V, Omega lens voltage: 12-15V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, oxygen flow rate: 20mL / min, octupole deflection voltage: -10~-5V, octupole RF: 120-180V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using Cool mode to detect elements Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 20mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.6-1.2L / min, extraction lens 1: -120~-90V, extraction lens 2: -40V~-5V, Omega deflection voltage: -70~-50V, Omega lens voltage: 2~8V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 0mL / min, octupole deflection voltage: -20~-8V, octupole RF: 120-150V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using Ti mode to detect elements Ti, V, Zn, and As, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 17mm, nebulizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: -100~ -70V, extraction lens 2: -10~ -20V, Omega deflection voltage: -190~ -100V, Omega lens voltage: 10~ 20V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 15mL / min, octupole deflection voltage: -10~ -2V, octupole RF: 100~ 180V, energy discrimination: -5~ 5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm; When using He mode to detect elements Zr, Nb, Mo, Cd, and Ta, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1200W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.3-0.7L / min, extraction lens 1: -160~-140V, extraction lens 2: -10~-20V, Omega deflection voltage: -190~-100V, Omega lens voltage: 10~20V, helium flow rate: 5mL / min, hydrogen flow rate: 1mL / min, octupole deflection voltage: -16V, octupole RF: 150~170V, energy discrimination: -5~5V, torch horizontal position: -2.0mm-2.0mm, torch vertical position: -2.0mm-2.0mm.

9. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, When using Nogas mode to detect elements Be and B, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1500W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.51 L / min, extraction lens 1: 4 V, extraction lens 2: -127 V, Omega deflection voltage: -158 V, Omega lens voltage: 12.9 V, helium flow rate: 0, hydrogen flow rate: 0, ammonia-helium mixture flow rate: 0, oxygen flow rate: 0, octupole deflection voltage: -9 V, octupole RF: 126 V, energy discrimination: 5.1 V, torch horizontal position: -0.9 mm, torch vertical position: -0.2 mm; When using O2 mode to detect elements Pd, In, Tl, and Pb, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1550W, sampling depth: 8mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.55L / min, extraction lens 1: 3.9V, extraction lens 2: -80.5V, Omega deflection voltage: -148V, Omega lens voltage: 14V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 20mL / min, octupole deflection voltage: -3V, octupole RF: 140V, energy discrimination: -3.4V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm; When using Cool mode to detect elements Li, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Ga, Rb, and Ag, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 20mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.92L / min, extraction lens 1: -90V, extraction lens 2: -33.5V, Omega deflection voltage: -46V, Omega lens voltage: 2.7V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 0mL / min, octupole deflection voltage: -8V, octupole RF: 120V, energy discrimination: -5.1V, torch horizontal position: -0.9mm, torch vertical position: -0.5mm; When using Ti mode to detect elements Ti, V, Zn, and As, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 800W, sampling depth: 17mm, nebulizer gas flow rate: 0.8L / min, compensation gas flow rate: 0.55L / min, extraction lens 1: -91V, extraction lens 2: -15V, Omega deflection voltage: -185V, Omega lens voltage: 14V, helium flow rate: 1mL / min, hydrogen flow rate: 3mL / min, ammonia-helium mixed gas flow rate: 0, oxygen flow rate: 15mL / min, octupole deflection voltage: -4.3V, octupole RF: 175V, energy discrimination: -6.3V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm; When using He mode to detect elements Zr, Nb, Mo, Cd, and Ta, the instrument parameters for ICP-MS injection testing are set as follows: RF power: 1200W, sampling depth: 8mm, atomizing gas flow rate: 0.8L / min, compensation gas flow rate: 0.48L / min, extraction lens 1: -154.1V, extraction lens 2: -19V, Omega deflection voltage: -161V, Omega lens voltage: 13.5V, helium flow rate: 5mL / min, hydrogen flow rate: 1mL / min, ammonia-helium mixture flow rate: 0, oxygen flow rate: 0, octupole deflection voltage: -16V, octupole RF: 170V, energy discrimination: -3V, torch horizontal position: -0.9mm, torch vertical position: -0.2mm.

10. The method for improving the stability of metal content detection in electronic-grade hydrofluoric acid according to claim 3, characterized in that, The sample vial is a PFA sample vial.

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