Over fifty years ago, two professors changed the landscape of mass spectrometry by developing innovative RF and DC power supplies. Their discoveries became the foundation of Extrel—the world’s leading manufacturer of state-of-the-art research and process mass spectrometers, residual gas analysers, and quadrupole mass spectrometry components.
Since 1964, Extrel’s instruments have been recognized for their exceptional performance, reliability and flexibility, and are complemented by the most comprehensive application, technical and on-site support in the industry. Providing solutions for the needs of today’s leading researchers from individual components to full all-in-one systems, Extrel works with their customers to deliver the best product for their needs.
Extrel’s focus on the serviceability of their instruments is second-to-none, delivering thorough and comprehensive technical support and service on a worldwide level through on-site and remote support. The company also provides in-depth training through their Support Schools, customer-site training, and webinar classes, allowing customers to build a training curriculum that is right for them. The company’s analytical and process instruments have been applied in both research and industry—used by Nobel laureates and thousands of others in a variety of applications worldwide. Extrel looks forward to the next 50 years of inspiring scientific progress in research environments.
MAX300-EGA Evolved Gas Analyzer from Extrel
The MAX300-EGA Evolved Gas Analyzer from Extrel is the latest evolved gas analyzer within the high-performance MAX300 family of Extrel. It has been developed for combining with instrumentation in materials science, pharmaceutical and organic chemistry laboratories and features the 19 mm quadrupole mass filter from Extrel. High resolution, sensitivity, and flexibility make the MAX300-EGA ideal for the characterization and quantitation of off-gas.
The gas analyzer is provided with a 2 m heated transfer line, an extensive compound library, and the ability to import a variety of external signals and is optimized for interfacing with thermal analyzers and microreactors. The chemically inert capillary maintains the sample hot and under vacuum all the way from the furnace to the ionizer to prevent condensation and chemical interaction during transit. The Questor 5 software comes standard with the ability to receive external signals, like the start-of-heating signal from a TGA. Trend and manipulate data within Questor 5 or simply export it for use on a different platform.
The MAX300-EGA features the speed, flexibility and precision of the Extrel MAX300 family, optimized for evolved gas analysis.
The key features of the gas analyzerare:
– Heated transfer line
o Length: 2 m
o 200°C standard
o 300 and 400°C options available
– Mass analyzer: 19 mm quadrupole filter
– Operating frequency: 1.2 MHZ
– Mass Rang: 2-200 amu Standard
o 250, 300, and 500 amu options available
– Detectable components: Any gas or vapor with a molecular weight or fragment ion within the mass range
– Dynamic Range: Can Measure components from 100 % to 10 ppb*
– Ionizer: Disposable EI source
o Plug and play for Ease of Maintenance
Filament: Two, one active and one spare with automatic switchover
MAX300-AIR Environmental Mass Spectrometer for Industrial Gas Analysis
The MAX300-AIR is an advanced industrial gas analyzer specifically developed for environmental monitoring and regulatory compliance. A single analyzer is capable of measuring unlimited compounds and it can be automated to track more than 160 sample points, spread across the production site.
The MAX300-AIR quadrupole mass spectrometer is fast and sensitive, making it possible to detect and measure a wide range of poisonous industrial contaminants. The system can measure total sulfur, toxic chemical release, TWA exposure values and BTU (energy content). It also allows explosive limit analysis.
The main features of the MAX300-AIR environmental mass spectrometer are as follows:
– ppt detection limits
– High precision for safety and regulatory reporting
– Quantitative analysis of separate contaminants
– Rapid analysis time
– Multiport sample systems for overall site monitoring
– Minimum maintenance and calibration required
– Number of sample streams: 16, 31, 40, 80, 120, 160
– Detectable compounds: Any vapor or gas sample
– Detection range: 100% – 10ppb standard, 10ppt w/ membrane inlet
– Analysis rate: 0.4 seconds per component
– Number of analysis routines: Unlimited
– Number of components: Unlimited
– Number of user configurable data tags: Unlimited
– Analysis precision: ±0.0025 absolute
– Stability: ±0.05 absolute over 30 days
– Filaments: Two – one active and one spare with automatic switchover
– Minimum maintenance with manual or fully automated calibration and validation
– 19mm high-transmission quadrupole filter
– Mass range options: 1-200, 300, 500 amu
The MAX300-AIR environmental mass spectrometer can be used in the following industrial sites:
– Pharmaceutical solvents
– Specialty chemicals
– Pesticides and herbicides
Extrel’s MAX300-BIO is an analytical platform designed to provide real-time process data on up to 80 reactors within the facility as well
as offer high sensitivity to measure trace contaminants in the end product.
Mass spectrometry is a powerful tool for bioreactor monitoring. Any alterations in the headspace composition in a fermenter or bioreactor provide critical information into cellular health and production efficiency. This enables the rapid and precise analysis of the gases flowing out of the reactor essential for real-time process control.
The MAX300-BIO is designed with the advanced quadrupole mass spectrometer technology to quantify bioreactor gases from multiple reactors within the facility and supplies reports to the control system in real-time.
The Questor5 software drives the MAX300-BIO to measure all sample points in a completely customizable sequence for site-specific, automated production control.
Based on the effluent composition, the MAX300-BIOcalculates the key indicators of organism health and process efficiency:
– Total gas flow
– Total mass balance
– Respiratory quotient (RQ)
– Carbon dioxide evolution rate (CER)
– Oxygen uptake rate (OUR)
– Liquid concentrations in the vessel
– Batch quality – Testing of minor ppm/ppb level components such as formaldehyde, methanol, acetic acid, etc.
The main features of the MAX300 are listed below:
– Detectable compounds: Any gas or vapor sample
– Detection range – 100% – 10ppm standard, 10ppb with the electron multiplier option
– Number of components – unlimited
– Number of analysis routines – unlimited
– Number of sample streams – 16, 31, 40, 80
– Analysis rate – <0.4 sec per component
– Number of user-configurable data tags – unlimited
– Analysis precision – <0.25% relative standard deviation
– Stability – <0.5% relative standard deviation over 30 days
– Mass range options – 1-250, 300, or 500amu
– Dual filament – one active/one spare with automatic switchover
– Manual or fully-automated calibration and validation
– Maintenance – typically two PMs per year
The following are the products produced by industrial bioreactors:
– Alcoholic beverages
– Bread products
– Waste treatment
– Pharmaceutical products – Enzymes, antibiotics, steriods and vitamins
MAX Systems: UHV-Compatible Flange-Mounted Quadrupole Mass Spectrometer from Extrel
MAX Systems, a range of UHV-compatible flange-mounted quadrupole mass spectrometers, are designed based on Extrel’s advanced mass spectrometer technology. Developed for a wide range of applications, the MAX Systems feature a detector, quadrupole mass filter and an ionizer mounted on a flange.
The electronics of the system include the Merlin Command System (CS) and the rack-mountable QCi quadrupole mass filter power supply. The system also features the 9.5mm and 19mm tri-filter mass filters and the Merlin mass spectrometer controller software.
The main features of the MAX Systems are as follows:
– UHV-compatible flange mounted with quadrupole mass filter, detector, and ionizer
– Electronics integrates Merlin Command System and quadrupole mass filter power supply
– RF power supplies
– 9.5mm and 19mm tri-filter mass filters
Merlin mass spectrometer controller software
The Extrel MAX-LT flange mounted quadrupole mass spectrometer systems offer high resolution and high sensitivity. The systems are mounted on a UHV compatible flange, and come with an ionizer, ion detector, quadrupole mass filter, controller, power supplies, and software.
The systems utilize Extrel’s high performance 9.5 mm rod Tri-Filter™ quadrupole mass filter and can be used as the foundation for a new MS system or incorporated to current systems for extended capabilities.
The main features of the MAX-LT flange mounted quadrupole mass spectrometers are as follows:
– 9.5 mm quadrupole with pre-and post-filter
– All components in vacuum probe UHV compatible
– High abundance sensitivity: 1 x 106
– High sensitivity: 1.0 mA/Torr
– Pulse counting mode for enhanced S/N and for multi-channel scalar data acquisition
– Ionizer with cross beam arrangement available for photo ionization experiments
– Merlin automation data system with rapid data acquisition speed of 12,500 data pts/s
– Flexibility with imbedded macros for data acquisition and system control
– Negative ions option provided for pulse counting data acquisition
The main applications of the MAX-LT flange mounted quadrupole mass spectrometers are listed below:
– Emissions monitoring
– CVD process monitoring
– Dynamic SIMS
– Plasma monitoring
– Laser ablation studies
– End point detection
– Residual gas analysis (RGA)
– Outgassing studies
– Flow tube detection
– Molecular beam studies
– Temperature programmed desorption (TPD)
– Combustion analysis
– Bakeout/vacuum pumpdown
Temperature Programmed Desorption (TPD)
When gases desorb from a surface, they are ionized, examined, and compared with the temperatures at which they were desorbed. Small molecules, such as CO and H2O, typically attract interest. The MAX-LT’s ionizer can be placed near the substrate to ionize even the low concentration desorbed compounds.
The system is able to manage a wide temperature range from many TPD sources with target temperatures ranging between 4 K and 1000 K. A shielded ion source helps to reduce neutrals in the chamber, minimizing the observed background during analysis.
The MAX-LT in a TPD application has excellent control of the ionizer to conduct “soft” ionization to maintain the molecular ion with fragmentation. The system maintains high sensitivity and outstanding confidence for the resulting data and mass spectrum.
Secondary Ion Mass Spectrometry (SIMS)
Secondary ion mass spectrometry (SIMS) studies are used to collect data about a surface being analyzed and can be categorized as dynamic or static. Dynamic SIMS is used for bulk analysis using an ion beam and quadrupole mass spectroscopy (QMS), such as the MAX-LTconfigured for SIMS applications.
The system has a conical aperture on the ionizer that can be placed near the substrate to gather and convey the secondary ions or ionize the desorbed neutral compounds in an effectively. The optional Extrel Energy Filter Ionizer allows researchers to distinguish between secondary ions and ionized neutrals in the chamber, guaranteeing that the resulting data is representative of the experiment.
The MAX-CS control system allows the researchers to have fine control of the ionizer to conduct “soft” ionization to preserve the molecular ion without fragmentation.
The optional Extrel Energy Filter Ionizer sets the LT-SIMS apart from the rest.
The Energy Filter Ionizer provides reduction in experimental noise and background in the mass spectrometer. It handles many sources of noise such as high energy ions (1 keV – 100 keV), which cannot be easily analyzed by a QMS, and has to be blocked from entering the analyzer.
The energy filter’s center stop keeps neutrals from entering the analyzer by impeding the line-of-sight. The cone aperture permits close placement to the target surface, which allows better sensitivity to the sputtered plume of ions. The on-axis energy filter performs a fine energy scan of <0.6 eV full width at half maximum (FWHM) resolution.
Every MAX-LT is equipped with the Merlin Automation Data System™ software as standard. Merlin Automation is one of the most powerful and flexible research software commercially available, allowing complete user control over their system.
Users can gather, examine and conduct library searches on all data. Merlin Automation offers researchers the power to observe the complete workflow. From analyte monitoring in the chromatogram window, Centroid spectra or live Profile, to spectral comparison in the Mass Map window, it offers researchers maximum flexibility for their application.
When researchers look for a software package that enables them to perform quantitative measurements, data trending and security tracking, they select to Extrel’s Questor5™ Software. It is Extrel’s true quantitative software platform, providing unrestricted flexibility in automation and analysis design, all packaged with a user-friendly interface.
Questor5, paired with the performance and stability of Extrel’s MAX probe products, enables effortless quantitative data trending, with each component quantified and reported within 400 msec. Several labs are concerned about security issues, such as user tracking for downtime or validation due to unidentified operator failure.
To discover if information has been breached, the data logger is an ideal choice as it will report every user and every event, providing total traceability. The system also includes 21 CFR 11 compliance, for the pharmaceutical sector.
MAX-LT Specifications and Features
The main specifications and features of the MAX-LT are as follows:
The new IQ-2000 from Extrel is a research-quality, high-performance mass spectrometry system in an educational package.
It features an innovative open-chamber design to highlight its high-tech components, and its small, transportable profile facilitates convenient mobility between classrooms.
The Extrel IQ-2000 features not only an analytical instrument aimed at educating future scientists, but also a fully interactive e-textbook. The text is the result of a collaboration among leading educators and researchers who are experts in mass spectrometry.
The text covers an introduction to mass spectrometry, quadrupole theory, and data analysis, while also including an in-depth look at MS systems, components, and applications.
The full textbook will be available with the instrument and is coming soon in the Apple®iBooks®store and Kindle™ bookstore.
Breath Analysis using a Benchtop Mass Spectrometer
Mass spectrometry is a gas analysis technique that is extensively used in several respiratory applications. The MAX300-LG is capable of determining all compounds present in a sample, needs minimal sample flow, and provides data updates in a rapid manner (Figure 1).
Researchers involved in biomedical or physiological studies of metabolism and respiration can employ breath analysisdata to study the underlying processes within complex biological systems (Figure 2).
Figure 2. Mass spectrometry for indirect calorimetry, a clinic patient inspiring 30% O2 at a normal breathing rate. The MAX300-LG measures all compounds in the sample with 400 full updates per breath. From this data, metabolic parameters, like the respiratory quotient (RQ) can be calculated without the need for additional equipment to measure flow. O2, and CO2 measurements are shown, RQ=1 ± 0.007 (equation 1).
The MAX300-LG provides high repeatability, which ensures that calculated metabolic parameters obtained from the gas analysis, such as the respiratory quotient (RQ), are precise (Table 1)
Table 1.Typical MAX300-LG breath analysis performance. The mass spectrometer analyzes all compounds in the sample with very high precision. In addition to the components listed here, the analyzer has the flexibility to measure trace volatiles such as formaldehyde, acetic acid, ammonia, and hydrocarbons for the purpose of diagnostic evaluation.
Equation 1. Nitrogen is not absorbed during respiration, so the ratio of the volumetric % of N2 in the inspired and expired sample is used to develop an RQ equation in which measured sample flow is not necessary. All O2, CO2, and N2 terms above are measurements of % volume.
The MAX300-LG’ssample inlet is custom designed for breath analysis application. Present configurations are used for sampling from sub-atmospheric pressures or high pressure (hyperbaric) conditions, like those detected at high altitudes. The inlet is modeled to automatically adjust and maintain the peak analytical performance (Figure 3) regardless of the sample pressure.
Laboratory gas analyzer, MAX300-LG features a rapid acquisition software and inlet configuration that are custom designed to produce the full breath-to-breath quantitative profile. The gas analyzer provides high precision measurements of all components present in the breath sample, with almost 50 updates for every single compound per second. The complete sample composition enables the scientist to determine metabolic parameters, such as the RQ, without integrating extra flow measurements.
Breath Analyzer Features
The breath analyzer features of the MAX300-LG include:
· Sample transit times as fast as 0.1 seconds
· Measurement rate: up to 5 ms per compound
· Quantitative analysis of O2, CO2, N2, H2O, and trace volatiles
Minimum sample flow < 0.04 atm cc/s
Industry, Laboratory, Government and University Research Centres
A Single Process Mass Spectrometer Solution for Quantitative Analysis in Refinery Flare Emissions Monitoring (40 CFR 60 Subpart Ja)
Chemical manufacturers and oil refineries are required to measure the component concentration of waste gas streams moving towards the flare according to new environmental regulations such as the EPA’s 40 CFR 60 subpart Ja. This EPA regulation mandates the analysis of Total Sulfur, hydrogen sulfide, and BTU content in the flare gas released from US refineries by November 2015.
Since flare streams consist of a range of components of varying concentrations, mass spectrometryis ideal for flare monitoring application, as it is capable of delivering real-time data on total sulfur, hydrogen sulfide, hydrocarbon content, and BTU of the sample.
Besides providing the Flare CEMS measurements mandated by Subpart Ja, mass spectrometrydelivers speciated hydrocarbon and sulfur data for root-cause analysis in the case of a reportable release.
This article discusses the use of an Extrel MAX300-IG process control mass spectrometer (Figure 1) to measure a range of simulated flare conditions. The MAX300-IG can perform quantitative analysis for a number of compounds at a concentration range of 100% down to 10ppb. The mass spectrometeruses a 19mm quadrupole mass filter for improved sample throughput, yielding long-term stability and high analysis repeatability.
Dynamic Range and Linearity of Hydrogen Sulfide
Different sulfur compounds down to ppm levels are typically present in flare gas waste streams, including hydrogen sulfide (H2S), carbonyl sulfide (COS), sulfur dioxide (SO2), and carbon disulfide (CS2). This experiment simulated a variety of potential plant conditions using blended gas bottles to demonstrate the accuracy and linearity of the MAX300-IGmeasurements for H2S (Figure 2) and Total Sulfur (Figure3).
The mass spectrometer employed a single point calibration which was recorded on the 1986ppm standard. It provided a speciated analysis for each sulfur component in the sample, and provides real-time calculation of total sulfur for reporting purposes. The dynamic range of the analyzer for all components is linear up to 100%.
The linearity of the MAX300-IG on the hydrogen sulfide in the sample ensures the accuracy of the single-point calibration across the entire dynamic range of the mass spectrometer. In addition, it facilitates an alternative validation procedure for hydrogen sulfide measurement by means of a low-level sulfur standard rather than expensive, unsafe, high-percent hydrogen sulfide blends.
Real-time Measurement of Total Sulfur and High Heating Value
As per 40 CFR 60 subpart Ja, total sulfur values need to be recorded and reported to the EPA in the event of discharge exceeding a stipulated limit, and the root-cause analysis of such discharge events needs to be performed. This can be done with the full, speciated analysis of each hydrocarbon and sulfur component, as a spike of a specific chemical is useful to determine the source of the emission and to facilitate reporting.
The MAX300-IG can also quantify the presence of non-sulfur components in a flare stream. It’s highly accurate measurements of non-sulfur components help reporting BTU values with precision and reproducibility (Table 1). The instrument performs the real-time calculation and reporting of the BTU values to the plant control system, and records the speciated concentrations of each hydrocarbon. Monitoring each component across the full dynamic range (up to 100%) in the event of a release is crucial aspect for root-cause analysis.
Table 1. Speciated hydrocarbon measurements and calculated stream high heating value (HHV).
Instrument Range and Linearity Independent of Component
The MAX300-IG was integrated to a sample system consisting of a blend of hydrogen and carbon dioxide to demonstrate its entire dynamic range, and its linearity of response to different compounds. Here, H2S and CO2 were measured from 0-100% by altering the sample composition subsequent to a a single-point calibration (Figure 4).
In this flare gas application, the same equipment was used by the MAX300-IGfor the analysis of each component as it has only one sample path. Moreover, the physics of ion trajectories forms the basis of the separation principle in the case of a mass spectrometer. Hence, the accuracy and linearity of the mass spectrometeris independent of compound identity; this validates the instrument across the entire range by means of any high concentration standard, irrespective of chemical composition.
Dangerous high-concentration sulfur standards are normally used to validate compliance with regulations such as subpart Ja. However, validations can be done at the high range using safe-to-handle gases such as argon, nitrogen and carbon dioxide, thanks to the separation principle of the mass spectrometer. This allows the flare CEMS system to be installed and operated safely and cost effectively.
Sulfur Analysis Response Time and Hysteresis
The timely response of the instrument to stream changes is crucial in dynamic sample analysis. Hysteresis and clearing are the major problems while handling compounds such as H2S due to their reactivity with steel surfaces. The MAX300 is designed for the analysis of flares containing sulfur, and uses sulfur specific components for the sample path’s wetted surfaces. Figure 5 shows the fast response of the analyzer to a change from a 100% H2S sample to a 100% CO2 sample (<10 seconds).
Since subpart Ja has mandated total sulfur measurement within the 0-300ppm analysis range, even slight hysteresis in the instrument can affect the measurement accuracy significantly. Here, the nitrogen gas was used to dilute a sulfur blend to record the decreasing sulfur concentrations at different levels from 0 to 300ppm. Then, increasing sulfur concentrations were recorded by reducing the nitrogen flow. The results shown in Figure 6 illustrate the lack of hysteresis, and the true linearity of the MAX300measurements of both H2S and Total Sulfur.
The MAX300-IG can measure hydrogen sulfide, BTU content and Total Sulfur in flare gas simultaneously, offering the dynamic response, dynamic range, and speed of analysis demanded by regulations such as subpart Ja.
In addition, the mass spectrometeris capable of monitoring more than one flare without compromising the 15-minute reporting cycle. It can measure percent to ppb level changes, and is highly sensitive to varying sample compositions. Further, speciation of all compounds delivers essential data for root-cause analysis and the linearity of the MAX300-IG allows for two alternative validation strategies to reduce the risk by avoiding the use of unsafe and expensive high- concentration H2S standards.
Applications that Require High Resolving Power at Low Masses
High-resolving power at low masses is required in several critical applications in the industrial and academic sectors. These include the determination of hydrogen isotopes in the presence of helium such as 4He /D2as well as CO in the presence of nitrogen (N2). Only 0.0033 amu is the mass difference between D2 and 4He.
Quadrupole Mass Spectrometers
Many quadrupole mass spectrometer instruments that are commercially available in the market are not capable of resolving such closely isolated masses. Extrel has over five decades of expertise in quadrupole development and sophisticated manufacturing methods, and they are capable of showing routine, high resolution, high stability performance with the advanced MAX-50 quadrupole mass spectrometer, a 19 mm tri-filter mass filter equipped with 2.9 MHz RF electronics (Figure 1).
The MAX-50 can independently deal with a wide range of UHV applications like geochronology, TPD, and high resolution SIMS. When integrated with Extrel’s application matched VeraSpec HRQ gas analysis systems, the measurement field is expanded to cover a broad range of gas analysis applications up to atmospheric pressure. The high-resolution MAX-50 is part of the MAX-QMS Series of quadrupole instruments.
Figure 2 shows spectra that were determined using the traditional MAX-50production instruments containing 2.9 MHz electronics, 19 mm tri-filter mass filter, negative/positive ion pulse counting multiplier with conversion dynode, and axial electron impact ionizer with dual thoriated iridium filaments.
High Resolution Power at Low Masses
Analysis of Carbon, Nitrogen, Oxygen, Argon, and Sulfur isotopes are areas of interest in geochemistry. Figure 2 depicts the usual resolution performance determined at m/z=40 and shows the top end resolution. Systems developed by Extrel have a resolution of at least 3000 FWHM at 40 m/z. With careful tuning, users are able to push these limits.
The resolution performance for low masses is shown in Figure 3. The measurements were carried out in a UHV chamber, where a mixture of 10 ppm deuterium and 10 ppm UHP helium diluted in UHP argon was spiked to a pressure of 5 x 106 Torr and shows excellent properties like baseline separation and peak shape.
In high-resolution experiments, peak stability is debatably as significant as anything else. When analytes are separated, just a few thousandths of an amu apart, it is necessary to get an accurate reading of the mass position. N2(MW=28.019) and CO (MW=28.008) are one of the toughest pairs of compounds to examine at the same time. However, Extrel’s MAX-50 quadrupole instrument can separate and differentiate both peaks to over a 30% valley (Figure 4).
High-resolution QMS quadrupole systems from Extrel are also utilized in isotopic analysis. In addition to splitting D2and He, hydrogen isotopes arealso studied at nuclear research facilities. Figure 5 shows peaks of diatomic hydrogen and 4He, 3He, and D2.
Extrel provides exceptional capabilities for high-resolution, low mass analysis, abundance-sensitivity characteristics, and unique resolution and transmission, which are not seen in any other commercially available quadrupole mass spectrometers. Extrel’s MAX-50 instrument can be utilized as a probe based MS system, a turnkey standalone VeraSpec HRQ system, or can be integrated into any current VeraSpec system.
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