Methods for in situ QMS calibration for partial pressure and composition analysis

Ellefson, R.E.

doi:10.1016/j.vacuum.2013.08.011

Cited by 18 publications

(15 citation statements)

References 15 publications

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“…In this study, we primarily used a yttriated-iridium filament because of its improved oxygen tolerance. 8,10 The dwell time on each mass-to-charge ratio was 50 ms.…”

Section: Instrument and Vacuum Line Descriptionmentioning

confidence: 99%

“…The switch was made from a tungsten filament to a yttriated-iridium filament due to tungsten's reactivity with oxygen 15,16 and the increased oxygen tolerance of yttriated-iridium filaments. 8,10,15 As mentioned previously, m/z 44 has a fragmentation interference with m/z 28 4 ; therefore, m/z 14 was used as a proxy for m/z 28 for both the glass capillary and the calibration volume techniques. The SEM sensitivity also changed over the course of this period which also makes only the precision comparable between the two methods.…”

Section: New Calibration Techniquementioning

confidence: 99%

“…[1][2][3][4][5][6][7][8][9] The methods from previous studies include thermal decrepitation of fluid inclusions as well as physical crushing to release fluid inclusion volatiles. In these methods, different calibration techniques are employed, such as glass capillaries sealed with high-vacuum epoxy glue, 3 glass capillaries sealed with thermal wire strippers, 4 capillary-introduced laminar gas stream, 2,8 and multi-position switching-style calibration valves. 2,5 There are significant issues with each of these calibration techniques that affect the precision and accuracy of the measurement.…”

Section: Introductionmentioning

confidence: 99%

“…Quadrupole mass spectrometry is an accepted approach for quantitative gas analysis of mineral fluid inclusions in geological samples using a residual gas analyzer with an electron ionization ion source 1–9 . The methods from previous studies include thermal decrepitation of fluid inclusions as well as physical crushing to release fluid inclusion volatiles.…”

Section: Introductionmentioning

confidence: 99%

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A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

Pettitt

Schaller

2020

Rapid Comm Mass Spectrometry

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Rationale Quantitative gas analysis by quadrupole mass spectrometry is used widely in the study of fluid inclusion volatiles, but the currently available instrument calibration techniques have a number of limitations. We describe a new method to overcome these by employing custom‐machined stainless‐steel calibration volumes that fit into modified bellows valves and can be filled on the high‐vacuum prep line of the instrument. This allows the calibration gas to be introduced in a pulse‐like fashion, replicating a burst of sample gas from a ruptured fluid inclusion. Methods The modified bellows valves equipped with calibration volumes are loaded onto the high‐vacuum inlet of a quadrupole mass spectrometer. Cobalt‐based alloy stem tips are then used to seal calibration gases (dry air, in this case) at known pressures into the calibration volumes for analysis. Results Two volumes of different dimensions were used to produce a relationship between moles introduced and integrated beam area for m/z 14, 32, 40, and 44. A linear fit along with a 95% confidence band for the relationship of moles introduced and integrated beam area was determined for the purpose of quantitative gas analysis in fluid inclusions containing atmospheric air. The calibration curves for each m/z have R‐squared (COD) values of 0.94 or better. For validation of this calibration technique, measurements were made using outside air as an unknown. Conclusions A new calibration technique has been developed for measuring femto‐ to pico‐mole quantities of atmospheric air that greatly reduces contamination and introduces calibration gas in a pulse similar to sample gas. This technique has reduced the error in quantifying these small aliquots of air to an uncertainty of ±1.5%.

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“…In this study, we primarily used a yttriated-iridium filament because of its improved oxygen tolerance. 8,10 The dwell time on each mass-to-charge ratio was 50 ms.…”

Section: Instrument and Vacuum Line Descriptionmentioning

confidence: 99%

Section: New Calibration Techniquementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

Pettitt

Schaller

2020

Rapid Comm Mass Spectrometry

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“…특히 플라즈마 를 이용하는 공정 챔버에서는 다양한 전자 충돌 화 학 반응으로 가스종이 생성된다. QMS (quadrupole mass spectrometer)로 이들 중성종의 분압 측정이 가능하다 1,2) . QMS의 구조는 중성 입자의 이온화를 담당하는 이온원과 이를 사중극 질량 필터에 조준 하여 입사시키기 위한 간단한 구조의 이온 렌즈, 그 리고 고주파와 직류 전압을 이용한 질량 필터와 최 종적으로 이온 전류를 측정하는 FC (Faraday cup) 와 EM (electron multiplier)이 있다 3) .…”

Section: 서 론unclassified

Analysis of contaminated QMS, cleaning and restoration of functions

Kim¹,

Joo²

2015

Journal of the Korean institute of surface engineering

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Quadrupole Mass Spectrometers (QMS) is a very useful tool in vacuum process diagnosis. Tungsten filament based ion sources are vulnerable to contamination from process gas monitoring. Common symptoms of quadrupole mass spectrometer malfunction is appearance of unwanted contaminant mass peaks or no detection of any ion peaks. We disassembled used quadrupole mass spectrometer and found out black insulating deposits on inside of ion source parts. Five steps of cleaning procedure were applied and almost full restoration of functions were confirmed in two types of closed ion source quadrupole mass spectrometer. By using a numerical modeling (CFD-ACE+) technique, the electric potential profile of ion source with/without insulating deposit was calculated and showed the possibility of quadrupole mass spectrometer malfunction by the deterioration of designed potential profile inside the ion source.

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Development of quantitative detection method for mass spectrometry coupled to an infrared laser spectroscope (Picarro) to monitor in nitrogen matrix a complex gas mixture of H₂, He, CO, N₂, Ne, O₂, Ar, CO₂, H₂S, CH₄, C₂H₄, C₂H₆, C₃H₆, C₃H₈, i‐C₄H₁₀, n‐C₄H₁₀, and C₅H₁₂

Keita¹,

Noirez

Berthe

et al. 2023

Rapid Comm Mass Spectrometry

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RationaleThe deep geological repository is considered the international reference for radioactive waste management. All gas exchanges must be understood in the context of the feasibility of such a repository. The technological challenge is to continuously monitor a wide range of gaseous molecules at low concentrations in confined spaces.MethodsA gas monitoring station, composed of two complementary analyzers, was developed: an electron impact quadrupole mass spectrometer (HPR‐20 R&D Hiden Analytical) and an infrared laser spectroscope (Picarro). The spectrometer was calibrated using simple mixtures (i.e., C2H6 in N2) and multiple mixtures (i.e., H2, He, CO2, CH4, and O2 in N2) at different concentrations to correct interferences. A matrix calculation is proposed to calculate the relative concentrations.ResultsThe method developed allows the measurement of gaseous species: light hydrocarbons, noble gases, sulfides, greenhouse gases, oxygen, hydrogen, and nitrogen in the same mixture. For each gas, the SDs and the limits of detection and quantification were calculated. The method was validated by comparing the concentrations of the measured gas species with the reference values of two standard gas cylinders.ConclusionsCalibration of a complex gas mixture remains a challenge because fragmentation of molecules, especially hydrocarbons, reduces the sensitivity of the method. The method developed is suitable for continuous gas monitoring in a confined environment and can be implemented to perform experiments in underground structures: galleries, microtunnels (cells), and boreholes.

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Methods for in situ QMS calibration for partial pressure and composition analysis

Cited by 18 publications

References 15 publications

A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

Analysis of contaminated QMS, cleaning and restoration of functions

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Methods for in situ QMS calibration for partial pressure and composition analysis

Cited by 18 publications

References 15 publications

A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

A new calibration technique for quantitative gas analyses of fluid inclusions using a quadrupole mass spectrometer

Analysis of contaminated QMS, cleaning and restoration of functions

Development of quantitative detection method for mass spectrometry coupled to an infrared laser spectroscope (Picarro) to monitor in nitrogen matrix a complex gas mixture of H2, He, CO, N2, Ne, O2, Ar, CO2, H2S, CH4, C2H4, C2H6, C3H6, C3H8, i‐C4H10, n‐C4H10, and C5H12

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