Traceable Certified Calibration Gas for Emission Analyzer...

Traceable Certified Calibration Gas for Emission Analyzer Systems.

Traceable Certified Calibration Gas for Emission Analyzer Systems.

Ashish SrivastavaCHEMTRON SCIENCE LABORATORIES PVT LTD

EL-47 ELECTRONICS ZONE MAHAPE NAVI MUMBAI, INDIA

Monday, September 24, 2018 SOx-NOx Confrence - Chemtron Science Labs (C) 1

India’s Largest Certified Emission Calibration Gas ProducerIndia’s Largest Certified Emission Calibration Gas Producer

Outline -Outline -• Introduction to Calibration Gas Standards.• Selection of Calibration Gas.• How is it made.• Gas Certification Guide.• Product mix for CEMS and AQMS.• Speciality Cylinder Regulators for Emission Gas Blends.• OEMs and Customers


India’s Largest Certified Calibration Gas ProducerIndia’s Largest Certified Calibration Gas Producer

Introduction to Calibration Gas Standards -Introduction to Calibration Gas Standards -– A Calibration gas standard establishes a reference point for

the verification of an analysis.– It is synthetically blended using high purity gases to form a

homogenous gas mixture.– The Preparation of Gas mixtures is done as per ISO 6142 – The Analysis is done in accordance of ISO 6143.– The Certificate of Analysis is in accordance of ISO 6141.



Introduction to Calibration Gas Standards -Introduction to Calibration Gas Standards -– Various methods are used to prepare Calibration gas standards

which are;• Gravimetric Method as per ISO 6142 (most widely used)• Static Volumetric Mixtures as per ISO 6144• Dynamic Volumetric Method as per ISO 6145

– The most accurate with minimum uncertainties is gravimetric method, in which blends are prepared by weighing individual gases in a precision comparator weight balance sequentially.



Selection of Calibration Gas-Selection of Calibration Gas-– Compatibility:

• There is a limitation of components in blends, due to its physical and chemical properties.

• Acidic Gases cannot be blended with Basic Gases. The resultant blend can never be stable as they constantly react with each other. E.g. Ammonia and SO2 Blend

• Flammable mixtures. E.g. Oxygen and Hydrocarbon’s.• Reactivity with Cylinder MOC. E.g. less than 10 PPM of NO,CO and

SO2 in Carbon Steel Cylinders.



Selection of Calibration Gas-Selection of Calibration Gas-– Cylinder Capacity/MOC of Cylinder:

• Cylinder capacity ideally decides useable gas content.• Usable gas to be decided on:

– Quantity of gas required during one calibration.– No. of calibration to be done in a year.– To take in to account purge and at least 10% residue for refilling.

– MOC is typically decided by Gas manufacturer depending on gas blend and concentration.



Selection of Calibration Gas-Selection of Calibration Gas-– Delivery Time. Plan in advance !!

• Gas Blends manufacturing is highly specialized process.• All Blends are “Made To Order” and is never a stock item.• All raw material gases in the blends have to be analysed before

blending. • The Gas Blends, post manufacturing has to go through Stability

Study which unfortunately cannot be sped up.• Transportation, not all freight forwarders handle DG cargo, which

gas cylinders come under (HAZ 2.1) hence can only be transported through surface transport in India.



Selection of Calibration Gas-Selection of Calibration Gas-– Cylinder Handling and Precautions:

• Cylinders should be used with Speciality Gas regulators only.• These regulators have SS316L wetted parts with Teflon®

Diaphragms, Safety Relief valves (to protect Gas Analysers) and are specially treated for use in reactive gas blends.

• While refilling, ideally the same composition should be refilled.• Genuine CCOE Certified Cylinders should be used as per law. • Cylinder should be stored and used in accordance to Gas Cylinder

Rules 2016 – Dept of Explosives.Monday, September 24, 2018 SOx-NOx Confrence - Chemtron Science Labs (C) 8


How is it Made -How is it Made -– Check for Compatibility

• As mentioned before, the blend components should be stable.– Calculation of Total Mole of Blend and its component Mole Fractions

• The method of calculating the mass of each component in the blend is done using its concentration or mole fraction in accordance to ISO 6142.

– Cylinder Conditioning and Passivation• Speciality Gas Cylinders are special cylinders. They are specifically treated for low surface energy

to avoid adsorption. The biggest culprit is moisture which interferes with components that effects stability.

• The cylinder undergoes through passivation to stabilize it for the target mixture.• ONLY after the conditioning time, the gas blending is carried out.

– Testing for purity of all components of Gas Blend.• Each component is tested for its purity. The calculation of individual mass and its uncertainty

calculation is a function of purity of stock solutions used in manufacturing.



How is it Made -How is it Made -– The Filling process (Gravimetric filling ISO 6142)

• The Blends for Emission analysers is filled majorly by gravimetric filling.• Various stock solutions or gas blends is used in order to achieve the final gas blend.

– Preparation Tolerance.• There is always some tolerance while making gas blends due to various limitations.• PT typically is 30% for < 10 PPM and about 1% for > 5% Blends.

– Quality Control and Final Gas analysis (ISO 6143)• All emission Gas Blends are compared analytically with NIST/VSL Primary SRMs.• The traceability of analysis is referenced to these SRMs with Certification

accuracy/Uncertainty @ 1%.– Final Pressure Test, Painting As per Gas Code.

• Cylinders are painted as per Gas code, Pressure tested and Sealed with Blinds.



Gas Certification - Guide Gas Certification - Guide



ISO StandardsISO StandardsType of BlendsType of Blends Relative UncertaintyRelative Uncertainty

ISO 17034(Traceable to SI units)

ISO 17034(Traceable to SI units)

Primary SRMs(For Metrological Institutions,

Gas manufacturers)

Primary SRMs(For Metrological Institutions,

Gas manufacturers)

Less than 0.5%

Less than 0.5%

ISO 17025(Certified Using SRM like (NIST,VSL etc)

ISO 17025(Certified Using SRM like (NIST,VSL etc)

Traceable to SRMs (For Critical/Precision

Applications)

Traceable to SRMs (For Critical/Precision

Applications)

Less than 1%

Less than 1%

ISO 9001/Internal SOPs(Gravimetric High Precession Internal Standards)

ISO 9001/Internal SOPs(Gravimetric High Precession Internal Standards)

Working Standards (End users like Power

Plants and OEMS)

Working Standards (End users like Power

Plants and OEMS)

Less than 2%

Less than 2%

Certificate of Analysis and Traceability- NO, SO2 and COCertificate of Analysis and Traceability- NO, SO2 and CO



Certificate of Analysis and Traceability- Blends of CO,NO and SO2Certificate of Analysis and Traceability- Blends of CO,NO and SO2



Speciality GasRegulators for

Gas Blends


Gas Blends




Carrier gases, Zero Gas


Carrier gases, Zero Gas

Some of Our OEM Customers-Some of Our OEM Customers-



Some of Our End Customers-Some of Our End Customers-





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