Danet Vrazel - KIN-TEK Analytical, Inc.

Low concentration calibration for high vapor pressure gases

January 7, 2025 by Danet Vrazel

Calibration challenges solved with Permeation Tube Technology

Challenge: The challenge is that permanent gases or air pollutants that cannot be liquefied, such as O2, NO, CO, N2, CH4, NO, etc. must be used in the gas form for calibration and are unstable in static mixtures at trace concentrations (ppm and lower). Using a permeation tube emitting at a very low flow rate for dilution to ppm and lower concentrations requires precision flow, pressure, and temperature control devices. Dynamically generating the gas mixture as it is needed eliminates issues created from storing the mixture.

Solution: Trace Source™ 57H Gas Fed permeation tubes used within a system that combines the FlexStream™ Base and PM/GF Modules provide the controls needed for creating trace concentrations of high vapor pressure (permanent) gases such as O2, NO, CO, N2, CH4, etc. that cannot be liquefied. The mechanism and controls needed to deliver accurate gas standards at trace concentrations is a combination of the tube construction and the equipment controls required to hold the tube at equilibrium conditions. The FlexStream™ System provides automated mechanical controls to hold the permeation tube at equilibrium for dynamically delivering a precise gas standard with each use.

Read more “Low Concentration Calibration for High Vapor Pressure Gases”

Trace Gas as Biomarkers

August 12, 2024 by Danet Vrazel

Why Trace Gas Concentrations are important for Disease Diagnosis…

Challenge: A breath analysis medical technology that is a quick and non-invasive test for detecting diseases is currently being developed using trace gas concentrations as biomarkers. Fluctuations in gas concentrations of various metabolic gases can determine if a person is healthy, at risk, or sick. For example, measuring Hydrocarbons, aromatic compounds, Nitriles, and Ketones in human breath can diagnose lung cancer but precise quantities of test gases are required to aid in biomarker research.

Referencing the linked papers below, trace concentrations of Heptane and Isopentane vapor were generated to test measurement values for establishing biomarkers related to lung cancer. Both papers determine if a breath analyzing technique is effective in analyzing different concentration ranges needed for effective and accurate diagnosis.

Other research includes the analysis of trace Ammonia for Chronic Kidney Disease (CKD), Ethane and Acetone for Diabetes, and Carbonyl Sulfide for Liver Disease. Simulating trace gases expelled from patients fordetermining disease requires accurate and precise gas standards targeting ppm, ppb, and pptr concentrations that are not easily provided using a static cylinder blend.

Target ppm and lower gas concentrations…

Solution: KIN-TEK offers the modular and automated FlexStream™ system that can target ppm and lower gas concentrations of over 550 different gas standards. The FlexStream™ system can create ppm down to pptr concentrations with a Base Module and Secondary Dilution Module. Each permeation tube in this system has a dilution range of 1:10,000. This allows a researcher to create a wide range of compounds and concentrations for gas standards.

With accuracy and reliability being key factors, the FlexStream™ system with Trace Source™ permeation tubes offers always fresh NIST traceable concentrations. With the complimentary FlexLink™ software that comes with the FlexStream™, data can be logged over time and saved to the computer for reference.

Published Papers Using KIN-TEK Products:

ZEUS (ZIF-based electrochemical ultrasensitive screening) device for isopentane analytics with focus on lung cancer diagnosis

R.E.A.C.T-Rapid Electro-Analytical graphitic Carbon nitride-based screening Tool for lung cancer – Case study using heptane

Calibrate Your Way

July 25, 2024 by Danet Vrazel

CALIBRATE YOUR WAY! Dependable Gas Calibration for your Analyzers, Detectors, and Sensors

KIN-TEK Industrial Gas Standard Generators with Trace Source™permeation tubes are used in industrial environments to deliver calibration gas standards directly to your process GC, GC-MS, or any type of gas analyzer.

Provide multi-point calibration for accurate gas analysis.

Span Pac^TM I for industrial, process GC applications in Nema 4 Hazardous Atmospheres.
FlexStream^TM for Laboratory, QA/QC.
Create custom gas mixtures for process or analytical environments.
Over 550+ Gas Compounds available to provide complex gas mixtures.

CALIBRATE YOUR WAY – Permeation Systems for Process GC Calibration or Laboratory GC, GC/MS Calibration!

KIN-TEK Analytical, Inc. provides trace gas calibration solutions for industrial or laboratory environments. Trace gas calibration in ppm to ppb ranges requires accurate and reliable standards that are dynamically generated using permeation tubes. KIN-TEK offers permeation systems built for industrial areas or for QA/QC labs.

The Span Pac™ Industrial (SP61-I) Permeation System dynamically creates NIST traceable gas standards for on-line calibration of process gas analyzers typically located in a plant analyzer house. Span Pac™ I Units are designed for N.E.C. Class 1, Group C or D, Div II hazardous atmospheres and can be adapted to Div 1 service to work side-by-side with your process analyzers. These units are wall mountable with Z-purge or X-purge options and provide the perfect solution for injecting the calibration gas directly into an automated sampling system.

For calibrating laboratory gas analyzers, the FlexStream™ Base automated permeation system works as a stand-alone instrument or controls an array of modules to fit unique calibration applications. For example, gas mixtures that require secondary dilution or the addition of variable humidity are easily created by selecting the appropriate modules in a series. Users benefit from operating the FlexStream™ with a local touchscreen interface or via a user supplied PC running FlexLink™ Software supplied with the instrument. FlexLink™ Software is easy to use, provides visual graphics, and logs data – saving users time and effort. Other systems without automation such as the 491Flex™ product series or the simplified EcoFlex are also available.

KIN-TEK offers over 550 chemical gas standards using permeation tube technology for delivering accurate NIST Traceable calibration gases. Certified Trace Source™ disposable or refillable type tubes come with a NIST Traceable Certificate of Calibration and are manufactured for use within a Span Pac Industrial or FlexStream™ Permeation system. Trace calibration gases from high ppm to ppb concentrations, complex gas mixtures, and multi-point calibration curves are created easily using specified permeation tubes.

Whether you need trace sulfurs, VOCs, BTEX or other standard gases for calibration, contact KIN-TEK Analytical for solutions to Calibrate Your Way!

KIN-TEK Articles

May 30, 2024 by Danet Vrazel

KIN-TEK Company Articles

“Identifying the Right Permeation Tube for Your Application” by Danet M. Vrazel 2024/12
Permeation tubes have been used for many years in various applications for creating trace concentration gas standards for calibrating gas analytical devices such as a gas chromatograph. Permeation tubes create NIST traceable gas standards because they are held at a stable temperature and are certified via gravimetric weight loss method where both the temperature and weight loss are measured by fundamental traceable standards (4). Creating NIST traceable gas standards for calibration is not the only use for these highly underrated small devices, it just may be the most likely use for them. Permeation tubes can be used for more than routine calibration of gas analytical devices and understanding how they work, and …. Click for more…

“Low Concentration Calibration for High Vapor Pressure Gases” by Danet M. Vrazel 2024/08
Calibration challenges solved with permeation tube technology. Creating trace calibration gas standards for high vapor pressure atmospheric gases such as O2, NO, CO, N2, CH4, and others has driven the requirement for using permeation tubes to achieve repeatable NIST Traceable gas sources. Since 1966, permeation tubes have been a proven method of calibration for trace concentration gases after O’Keefe, and Ortman published early findings relating permeation tubes as a primary standard used for trace gas analysis (7). Since then, environmental, air monitoring, petrochemical, and other applications have improved detection capabilities that require lower concentration gas standards beyond what is typically feasible… Click for more…

“Ambient Air Monitoring” by Danet M. Vrazel 2023/02
Dynamically Blending % Level Gases for Calibration. A broad concentration range gas mixture or precise mixture of specific gases can be required for testing, exposure, or calibration for a variety of applications. An ambient air monitoring station is such an application that requires calibration with accurate and traceable gas mixtures. Outside ambient air monitoring stations monitor and measure gases such as N2, O2, NO2, CO, CO2, VOCs, SO2, H2S or others. The gases detected, the gas concentration, and the monitoring or detection device drive the requirement of the application… Click for more…

“Adding Humidity to Trace Concentration Gas Standards” by J J McKinley
A key, but often overlooked, factor in the behavior of gas sampling & measuring systems is the effect of relative humidity (RH) on performance of the system. RH can have a significant effect on the sensitivity and stability of a sensor system. Even for sensors that are not sensitive to RH, the RH level may affect the efficiency of sample delivery to the sensor. Systems sampling ambient air should be calibrated with standards that simulate ambient air. This paper discusses the various techniques for adding humidity to trace concentration gas standards without compromising the accuracy of the standard… Click for more…

“Test Gas Mixtures – The Bridge from Sensing to Quantification” by J J McKinley, T. Shirley 2012/04
Poster Presentation, Trace Explosives Detection Workshop, Boston, MA, April 2012. Test gas mixtures are the key tools required to take a sensing technique from the laboratory curiosity stage to the reliable measurement technique stage. Yet relatively little attention is given to the definition, production and delivery of effective test mixtures. Factors addressed in this presentation are test mixture requirements, techniques for creating known trace concentration mixtures of reactive vapors, atmosphere simulation, interferent identification, and test mixture delivery… Click for more…

“Getting a handle on HAP’s” by J J McKinley
The Clean Air Act depends on our ability to measure hazardous air pollutants – but this is no simple task, as Jim McKinley explains. It is widely accepted that “what you cannot measure, you cannot control.” For controlling the more that 170 compounds plus 17 compound categories identified in the 1990 Clean Air Act as hazardous air pollutants (HAPs), there are two challenges. The first is to develop reliable methods for sampling and detecting the various HAPs in industrial atmospheres… Click for more…

“Permeation Tubes: A Pragmatist’s Approach to Creating Almost Nothing” by Jim McKinley 2007
Permeation tubes offer the “path of least resistance” to traceability. The production of trace concentration calibration gas mixtures is a challenging process that faces increasing requirements, especially for the calibration of newer, sophisticated analytical instruments. The permeation tube is a molecular-based flow control device that is ideally suited for that purpose. While lower and lower concentrations of an increasing number of complex compounds are required, confinement as stable, static mixtures remains a problem for trace concentration mixtures. Click for more…

“Permeation Tubes: A Simple Path to Very Complex Gas Mixtures” by Jim McKinley 2008/Jan/Feb
As applications requiring gas mixtures become more sophisticated, the mixtures required become progressively more complex. Permeation tubes can supply miniscule flows of a wide range of analyte vapors while compensating for background contamination in the matrix. Acomplex gas mixture may contain a few or many com- ponents; however, there is typically another factor that makes the mixture difficult to prepare and impractical (and often impossible) to store. For example, the require- ment that a mixture be delivered at a specific relative humidity (RH) moves any mixture into the “complex” cat- egory. The RH value is a function of both temperature and pressure, so storage of the humidified mixture is out of the question…Click for more…

“Establishing Temperature Change Characteristics Associated with Equilibrium Times
of Permeation Tubes” by Danet M. Vrazel
Teflon® permeation tubes are a proven method for making trace concentration gas mixtures when used in their equilibrium state. Permeation rates are established by a gravimetric weight loss method after equilibration at a stable temperature. Frequently, permeation tubes are subjected to drastic temperature changes when stored at low temperatures or used over a range of temperatures. Such changes can cause transient characteristics that result in substantial deviation from expected permeation rate data. Performing calibrations during non-equilibrated transient phases affect analyses and wastes time… Click for more…

“Calibration for Trace Sulfur in Olefins” 2003 September
Maintaining reliable standards for tree sulfur compounds in an olefin matrix is a common problem in industrial quality assurance. Using permeations uses to dynamically blend the required mixtures offers a simple solution. Measurement of trace sulfur compounds is required throughout industry. In the manufacture of polyethylene and polypropylene, for example, even low ppm concentrations of some sulfur compounds will poison the catalyst, affecting yield and product quality. Because some compounds are more troublesome than others, speciation is required. Click for more…

“The Preparation of Calibration Standards for Volatile Organic Compounds – A Question of Traceability”
by J. McKinley and R.E. Majors
The analysis of trace volatile organic compounds (VOC’s) has been of considerable interest for decades, particularly for monitoring air emissions, ambient air, and indoor air contamination int he workplace. The combustion of new gas chromatography (GC) column technology with improvements in GC Instrumentation, especially in detector sensitivity and selectivity improvements. has led to routine measurement and detection of sub-parts-per-billion concentrations. Researchers have directed much effort toward decreasing detection limits and achieving repeatability. Click for more…

“Permeation tube sources for internal standards in process samples” by J.J. McKinley, Dale C. Merriman
In-process analytical instrumentation is becoming increasingly important for process control and product quality measurement in a production environment in many industries, including the following: petroleum, petrochemical, chemical, pharmaceutical, food and biotechnology. The journal provides a multidisciplinary forum for scientists and engineers involved in research, plant design, process quality control and environmental monitoring. Chemists, chemical/mechanical/electrical and instrument engineers, computer scientists, quality assurance engineers, instrument manufacturers and consultants form the primary audience… Click for more…

“Using Permeation Tubes to Prepare Trace Moisture Standards in Reactive Gases” by Jim McKinley
The measurement of trace concentrations of water vapor in reactive gases has become very important in the semiconductor manufacturing industry. Techniques for measuring low ppm and ppm moisture in NH3, Hal, and other reactive gases have been developed, but producing standards for a system calibration and data validation remains a problem. Click for more…

“Using Permeation Tubes to Create Trace concentration Moisture Standards” by J.J. McKinley
Moisture standards have traditionally been prepared by techniques which saturate the gas at known conditions. Preparing standards at trace concentrations (low ppm, ppm) requires saturation at cryogenic temperatures. Standard techniques require large cumbersome apparatus, and are generally not well suited for field use. Additionally the method cannot be used with condensable gases frequently of industrial interest. Click for more…

“Testing at the limits” by Jim McKinley
Calibrating and validating ppm and ppm on-line analysers. On-line analytical measurements have become commonplace in the petrochemical and other processing industries. Opertors rely heavily on this up-to-the-minute analytical data for guidance in making the day-to-day operating decisions. Often, analyses are actually in closed loop control of some portions of the process. Click for more…

Article A Continuous On-line Generator for Trace VOC Standards in Water Thumbnail

“A Continuous On-Line Generator for Trace VOC Standards in Water” by J.J. McKinley, M.Quazi, C.A. Thomas
Analyzers for monitoring water quality in process or waste water streams require calibration with liquid standards. Traditional techniques for preparing these standards are cumbersome and often inadequate in their functions. These problems are rectified with the use of permeation tubes to continuously add trace VOCs to a clean water stream to generate the standards on line… Click for more…

“Adding Relative Humidity to Trace Concentration Gas Standards in a Permeation System” by Danet M. Vrazel
Gas sensor sensitivity levels have increased in equipment where atmospheric conditions, such as relative humidity, directly affect test results. Calibrating for changes in relative humidity in trace level gas concentrations has generated the need for effectively adding relative humidity to the output gas of a permeation system. Click for more…

ESG

May 13, 2024 by Danet Vrazel

Calibrate for Trace Moisture in Electronic Specialty Gases

Challenge: Semiconductor chips are used in a variety of electronics such as smartphones, military equipment, vehicles, and healthcare equipment. The production of semiconductor chips requires the use of high purity Electronic Specialty Gases (ESG) that should be free of trace contaminants such as moisture. The ubiquitous nature of trace moisture makes it challenging to calibrate and test for contaminant levels in ESG. To mitigate risk of damage to semiconductor chips, the manufacturing process must analyze ESG for ppm to pptr of moisture concentration. The KIN-TEK Analytical customized Span Pac^TM 61-H₂O WeldedX (SP61-H₂O-WX) moisture permeation system calibrates for trace moisture content in various ESG.

As semiconductor chips are extremely sensitive, any ESG used in the production process is required to be as pure as possible (typically higher than 99.998% purity) or risk damaging the chips. ESGs are used for etching and deposition processes to create the layers and tracks on the semiconductor chips. A few examples of an ESG are Hydrogen (for Purging), Ammonia (for Deposition), and Chlorine (for Etching). Depending on the application, analysis of impurities such as moisture may be from ppmv down to pptr concentrations. Calibration must be done with a moisture standard that is isolated from atmospheric moisture but adds a known measured amount of water vapor to the test gas.

How to Calibrate for trace moisture content…

Solution: KIN-TEK Analytical, Inc. offers a customized orbitally welded moisture generator (SP61-H₂O-WX) that switches between carrier gases easily. Using the standard addition technique, trace moisture calibrations are done by spiking the carrier gas with an accurate moisture concentration to yield a known standard beyond baseline values.

Integrated third party software available on a user supplied PC provides an extra feature of real time graphical interface and data logging of mass flow over time.
Changing carrier gases is done by choosing the predetermined ESG from a drop-down menu and physically connecting that gas at 60 psig.
NIST Traceable standards for mulitpoint calibration and validation is done easily with the SP61-H₂O-WX or SP61-H₂O-WSDX (with secondary dilution capability).

Dynamic Gas Mixing for High ppm and % Concentrations

April 5, 2024 by Danet Vrazel

Flexible automated solutions for dynamically blending gases to achieve high ppm to % concentration gas mixtures.

Challenge: KIN-TEK Analytical, Inc. (KIN-TEK) provides trace gas calibration solutions to the gas analyzer, sensor, and detector industry using permeation tubes and gas standard generators. Permeation tubes are a proven, accurate, and traceable solution for creating trace concentration ranges (ppm to pptr) since the pure permeating gas can be accurately diluted to create lower concentrations. However, generating percent (%) concentration targets are beyond the reach of typical permeation devices and it would take multiple devices and equipment to achieve 5% or higher concentrations. How to Calibrate in % Level Concentrations…

Solution: To bridge the gap between permeation tube concentration capabilities and percentage level concentrations, KIN-TEK’s FlexMixer™ Multi-Gas Blending System provides a flexible automated solution for dynamically blending gases to achieve high ppm to % concentration gas mixtures.

The FlexMixer™ Multi-Gas Blending System dynamically blend source gases creating an easily controlled, accurate, and traceable gas mixture that can be automated for multi-point flow generation and delivered in real time.

Automated Gas Blending of Balance Gas and up to 3 Component Gases.
100+ preloaded gas configurations available; 20 user defined gas blends.
Profile and Manual control modes.
Create, control, and measure custom gas blends.
Perform multi-point calibration of analyzers, sensors, detectors.
Dilute existing cylinder sources.
User friendly software for a simplified solution with integrated safety shut off.
Portability between labs or facilities with small footprint.

Read more about using the FlexMixer^TM in Ambient Air Monitoring to dynamically blend % level gases for Calibration.

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