epa metrology laboratory instrument calibration services

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Scott A. Moore, Engineering Technician

EPA Metrology LaboratoryInstrument Calibration Services

Office of Research and Development (ORD)National Risk and Management Research Laboratory (NRMRL)Air and Energy Management Division (AEMD)

Date: March 26, 2018

Office of Research and Development (ORD) • The Office of Research and Development (ORD) is the scientific research arm of EPA, whose leading-edge research helps provide the solid underpinning of science and technology for the Agency.

• https://www.epa.gov

• https://www.epa.gov/aboutepa/epa-organization-chart

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National Risk Management Research Laboratory (NRMRL)

• As EPA’s premiere laboratory for risk management research, NRMRL advances scientific and engineering solutions to manage current and future environmental risks.

• https://www.epa.gov/aboutepa/organization-chart-office-research-and-development-ord

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Air and Energy Management Division (AEMD)

• AEMD is responsible for research, development, and evaluation of air pollution control technologies and methods to characterize and mitigate emissions of air pollutants.

• https://www.epa.gov/aboutepa/organization-chart-office-research-and-development-ord

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AEMD Metrology Laboratory provides National Institute of Standards and Technology (NIST) Traceability for:

• Mass (Balances and Weight Sets)

• Flow Devises (MFC, Roots Meters, Laminar Flow, Wind Tunnel)

• Temperature• Legally defensible data.

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• Pipettes• pH, RH• Voltage• Ozone, Nox, Sox and PM 2.5

• Pressure

https://www.nist.gov/

Bureau International des Poids et Measures (BIPM) - Evaluation of Measurement Data - Guide to the Expression of Uncertainty in Measurement (JCGM 100:2008) - GUM• International Bureau of Weights and Measures• https://www.bipm.org/en/about-us/• Free to download.• https://www.bipm.org/en/publications/guides/gum.html

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International Organization of Standardization(ISO) 17025 Accreditation - National Voluntary Laboratory Accreditation Program (NVLAP)

• Third party verification.• Reviews all laboratory records, operating procedures.• Competency testing and review of reports.• https://www.nist.gov/nvlap

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Weight28%

Temperature19%Flow

15%

Pressure13%

RH/T6%

Volume6%

Relative Humidity3%

Absorbance/Transmittance2%

Gas Analysis3%

pH2%

Time1%

Fluorescence1%

Ozone Analysis1%

Electronic0%

Metrology Lab Utilization 9/21/17 to 3/22/2018

Weight

Temperature

Flow

Pressure

RH/T

Volume

Relative Humidity

Absorbance/Transmittance

Gas Analysis

pH

Time

Fluorescence

Ozone Analysis

Electronic

Pipette Calibrations•The standard method for calibrating a pipette is gravimetric.

•Most are calibrated on site. Some are shipped to the vender.

• Calibration includes 3 points before and after cleaning.

•Small volumes may be susceptible to evaporation errors on low humidity conditions.

•Vendor failure rate is <0.2%.

•3,000 pipettes per year.

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Alternate Technology for Pipette Calibrations •Pipette Calibration System (PCS)

•Uses a spectrometer to measure color change in calibration dyes.

•Low volumes (<0.5 ml) are more accurate than gravimetric.

•Dyes are less vulnerable to evaporation errors.

•520 nm range (blue)

•730 nm range (red)

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Artel Pipette Calibration System (PCS)

EPA does not endorse this or any other pipette calibration system.4/16/201810 U.S. Environmental Protection Agency

Advantages of the PCS•Alternate technology (not gravimetric).•Automatic reports.•Barcode system tracks each individual pipette.•Users have to go through a “Qualification” procedure.•System ready for ISO 17025 Accreditation (Manual and procedures already written by manufacture.) •Portable – easy to transport, recalibration not required.•At 0.50 ml and lower the PCS is more accurate than gravimetric.

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QUESTIONS

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This Photo by Unknown Author is licensed under CC BY-SA

15 MINUTE BREAKRESUME AT 2:45

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This Photo by Unknown Author is licensed under CC BY

Temperature Standards used in EPA’s Metrology Laboratory•Primary standard in our lab is the Triple Point Cell.

•Once a condition is created where water exists in a state of vapor, liquid and a solid, the reference temperature will be 0.01º C ± 0.0001º C.

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Triple Point Cell

4/16/201815 U.S. Environmental Protection AgencyEPA does not endorse this or any othercalibration system.

Dry Well Calibration Systems

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EPA does not endorse this or any other calibration system.

HART 9122A +50ºC to +700ºC ±0.5ºC

Dry Well Calibration Systems

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EPA does not endorse this or any other calibration system.

HART 9150 +150ºC to +1200ºC ±0.15ºC (S-Type TC)

Dry Well Calibration Systems

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EPA does not endorse this or any other calibration system.

FLUKE 9170 -45ºC to +140ºC ±0.1ºC (PRT)

Dry Well Calibration Systems

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EPA does not endorse this or any other calibration system.

FLUKE 9173 +50ºC to +700ºC ±0.15ºC (S-Type TC)

PRT, S-Type TC, HART BLACK STACK

PRT -196º C to +250 ±0.025º C HARTS-Type TC 0º C to 250º C ±0.15 BLACK STACK

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EPA does not endorse these or any other calibration system.

Various Types of Temperature Measuring Devises:

•PRT – Platinum Resistance Thermometer

PRT-A, Model: T100-250, Uncertainty: ±0.010º C

PRT-B, Model: 935-14-61, Uncertainty: ±0.004º C

•RTD – Resistance Thermometer Detectors

•Thermocouple – Dissimilar Metals - Types J, K, E, T, N, B, R, and S

•Thermistor – Thermal Resistor

•Thermometers – Liquid in glass4/16/201821 U.S. Environmental Protection Agency

EPA does not endorse these or any other calibration system.

Thermometer Calibration•Calibrate against a NIST Standard Thermometer. Dry Well will need to have direct contact to the sensor area. Due to the thermometer bulb shape, direct contact will not occur.

•Run the risk of breaking a glass thermometer in a Dry Well.

•Water bath is best option.

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Thermometer Calibration Frequency• Frequency of calibration will vary from vendor to vendor and conditions that it is used in.

• Historical data could have a significant impact on frequency.

• Risk of losing critical data should also be considered.

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Thermometer Calibration Frequency•How does the operating temperature affect the liquid inside the Thermometer?

•The NIST Standard should have a better accuracy than the thermometer being used in the actual process.

•Daily calibration checks could prevent data loss.

•NIST thermometer will require calibration at a prescribed interval.

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Thermometer Calibration Case Study• The analytical method for fecal Coliform bacteria in wastewater (SM 9222 D-2006) requires that the water bath be maintained at 44.5 ± 0. 2º C.

•If the temperature goes above or below the 0.2º C is there an increase of false/positive results?

•What can be done to prevent data loss?

•What is the range of the thermometer?4/16/201825 U.S. Environmental Protection Agency

Coliform bacteria

Thermometer Calibration Case Study•To ensure that ± 0.2º C tolerance can met, we require that the NIST traceable thermometer used to check the water bath thermometer have a stated accuracy of ± 0.1º C.

•What are the marking intervals on each Thermometer?

•What is your correction factor?

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Thermometer Calibration Case Study•What is the manufacturer’s stated accuracy of the process thermometer?

•Does the thermometer stay in the bath all the time?

•At 44.5º C, is the thermometer left in the bath 24 hours, 7 days a week?

•Will prolonged exposure at 44.5º C, have an effect on the thermometer’s internal liquid?

•How is the water bath temperature controlled?

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Conclusions• More frequent calibration checks.

• Eliminate correction factor on process thermometer.

• Consider using electronic thermometer.

• Consider using a Data Acquisition System.

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Acknowledgements•Mike Tufts, Jacobs Technology.

•Joshua Varga, Jacobs Technology.

•Todd Crawford, State of North Carolina.

•John Walker, U.S. EPA.

•Lara Phelps , U.S. EPA.

•NIST and BIPM.

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QUESTIONS

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This Photo by Unknown Author is licensed under CC BY-NC-ND