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THORNTON

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Mettler-Toledo
Conductivity Calibration Training
Victor M. Braga
Mettler-Toledo Thornton, Inc.
Bedford, MA 01730 USA
www.thorntoninc.com

Topics

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

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Definition of Calibration

A comparison between an item of measuring equipment or test


equipment, with a standard or a similar item of higher accuracy, for the
purpose of detection, correlation, and the documentation of, the
accuracy of the instrument or item of equipment being compared or
tested.

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National Standards

Leading Pure Water


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ASTM
American Society for
Testing and Materials

NIST
National Institute of Standards
and Technology

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What Is ASTM

American Society for Testing and


Materials

Organized in 1898, it is one of the largest voluntary standards


development organizations in the world

Not-for-profit organization that provides a forum for the development


and publication of voluntary consensus standards

It publishes more than 10,000 standards each year in the 73 volumes


of the Annual Book of ASTM Standards

What Is NIST

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National Institute of Standards and Technology


The National Institute of Standards and Technology is an agency of the U.S.
Department of Commerces Technology Administration

Established in 1901 to strengthen the U.S. economy and improve the quality
of life by working with industry to develop and apply technology,
measurements, and standards.

Operates primarily in two locations Gaithersburg, MD and Boulder, CO

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Calibration Traceability

Meters and calibrators (decade boxes)


-

Traceable to National Institutes of Standards (NIST)

Sensors
-

Cell Constant Traceable to American Society for Testing and Materials (ASTM)
and Ultrapure Water at 15, 25 and 40 C
Temperature - Traceable to National Institutes of Standards (NIST)

Instrument Calibration

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

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Why Calibrate Separately?

Instrument calibration assures calibration of all


measuring ranges

Auto Range
Range Manually Selected

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Instrument Calibration

Calibrated/verified with decade boxes


Calibrated/verified with manufacturers
calibrators

Calibration/verification may be performed at the


meter or at the end of the cable

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Traceability

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NIST
Cal Labs
Multi-Meters
Manufacturers
Calibrators (Decade Box)
Process Instrument

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Conductivity Sensor Calibration

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

12

Cell Constants

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Cell Constant = Multiplier

1cm
0.1cm

1cm

0.1 constant

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ASTM D1125
Primary Standard
and Pure Water
at 15, 25, 40C

Cell Constant Traceability

Standards Lab
Cell Constant

14

Production Cell
Constant

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Standard D1125

Standard Test Methods for Electrical Conductivity and Resistivity of


Water

Four Conductivity Solutions: A, B, C, D


Solution
A
B
C
D

Conductivity @ 25 C
111,342* S/cm (8.98 -cm)
12,856* S/cm (77.78 -cm)
1,408.8* S/cm (709.82 -cm)
146.93* S/cm (6,805.96 -cm)
*Plus conductivity of water used

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Fundamental Standard

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Ultrapure Water as a Fundamental


Standard

Effects of Temp. on Ultrapure Water Resistivity


Resistivity

100

18.18 M-cm
0.055 S/cm

31.87 M-cm
0.031 S/cm

80

8.85 M-cm
0.113 S/cm

60
40
20
0
0

10

20

30

40

50

60

70

Temperature (Deg C)

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80

90

100

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Ultrapure Water Sensor Verification/


Calibration/Certification System

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Traceability

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NIST
ASTM
(Ultrapure Water)

Manufacture's
Standard
Product

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Calibration Options

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

19

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Cell Calibration Methods

Methods used to verify/calibrate cells


-

Verify/calibrate in solution with stated conductivity


Solution may be purchased
Solution may be prepared to specific conductivity
Verify/calibrate vs. another calibrated cell
Return cell to factory for calibration

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Calibrating with Standard Solutions

I bought a standard conductivity solution... but whenever I use it to verify


the cell constant, they never agree. I always have to re-calibrate.

Nearly 20%
difference!!!

Standard
Solution

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Calibrating with Standard Solutions

Reasons for the difference between the Standard and what the meter
displays

The stated conductivity of the Standard is incorrect


You get what you pay for
SRM3198 Each time the bottle is opened, a portion of the solution will
evaporate, which will change the conductivity. Solution should be opened for
the minimum time required to dispense solution -- NIST
Contamination of the solution by dirty equipment
Conductivity of the solution was too low and was contaminated by CO2

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Calibrating with Standard Solutions

Reasons for the difference between the Standard


and what the meter displays

The meter is not calibrated


Calibrated wrong range circuits

1. Calibrate/verify all range circuits


2. Calibrate/verify the appropriate range circuit

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Calibrating with Standard Solutions

Reasons for the difference between the Standard and what the meter
displays

Not accounting for the temperature dependence of the solution


You are not at the standard temperature
You are not compensating when you should be

Out of the dynamic range of the meter and sensor

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Field Calibration

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

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Verify/Calibrate

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Verify/Calibrate Vs. Another Calibrated Cell


The water system must have a sample
port

Joints must be air tight


Must have adequate flow through the
chamber

Be aware of air ingress


-

CO2 will diffuse through most


polymers
Polypropylene will pick up 4 ppb per
meter of length
Nylon will pick up 0.04 ppb per meter

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Portable Cond./Res
Calibration Kit

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Calibration Sequence

Calibrate 200CR Temperature Circuit


Calibrate 200CR Resistance Circuit
Calibrate UUT Temperature Sensor
Calibrate UUT cell Constant

Portable Cond./Res
Calibration Kit

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Data Collections

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Record AS FOUND Sensor Calibration Factors


-

Sensor RES Multiplier


Sensor RES Adder (always = 0)
Sensor TEMP Multiplier
Sensor TEMP Adder

Verify 200CR Calibration


Record AS FOUND Readings
Calibrate 200CR (if required)
Calibrate Sensors Temperature (if required)
Calibrate Sensors Cell Constant (if required)

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Verify/Calibrate

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Verify/calibrate Vs. Another Calibrated Cell

Standard and UUT sensors


are exposed to the same
conditions

A STD Re 1.
000 M-cM
B STD Tp
26.3 C
C UUT Re 1.
000 M-cM
D UUT Tp
26.3 C

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Calibration Steps

1. Calibrate the Meter


a.
b.

Calibrate all resistivity circuits


Calibrate all temperature circuits

2. Calibrate the Sensors Temperature


3. Calibrate the Sensors Cell Constant
a.

Calibrate Uncompensated/Compensate

30

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Compensation Algorithm

Temperature
Compensation
Algorithm
Uncompensated
Resistance

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Compensated
Compensated
Readings
Readings

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Uncompensated Mode

Calibrating in the Uncompensated Mode


Standard sensor must be at the same temperature as UUT
-

Minimize tubing length


Increase flow rate
Assure stable temperature environment

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Return Cell to Manufacturer

Return Cell to Manufacturer for Calibration


-

Traceable ASTM calibration


Multi-point verification available
Certificate of calibration provided

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Specialized Calibration

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Instrument Traceability
Sensor Traceability
Instrument Calibration
Sensor Calibration
Calibration options
Field Calibration
Specialized Calibrations
Field Calibration Demo

34

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Standard Sensor Calibration

Standard calibration provides vital


information about the sensors
performance

35

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Elevated Temp. Calibration

Calibrating at or near operating temperature provides:


-

Greater temperature accuracy


More accurate compensated readings

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ASTM Verified Calibration

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One Point ASTM Verified Calibration


Sensor is calibrated at 0.055 S/cm and verified in ASTM
Solution D (147 S/cm)

S/cm

1,000

100

10

0.01 S/cm

USP waters

Solution C
Solution D

37

25C
UPW

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ASTM Verified Calibration


One Point ASTM Verified Calibration

Provides detailed report


with distribution data

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System Calibration

Calibrates sensor, meter and patch cord as a single item:


-

Reduces individual inaccuracies


Optimizes system accuracy

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Thank You
Victor M. Braga
Mettler-Toledo Thornton, Inc.

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