Introduction To Calibrations

PT.
ECOGREEN OLEOCHEMICALS
CALIBRATION
INTRODUCTION TO CALIBRATION
PT. ECOGREEN OLEOCHEMICALS
CALIBRATION ACCURACY VS PRECISION

IQ/OQ EQUIPMENT – NEW
Installation Qualification (IQ) – provides documented

evidence to confirm that the equipment and its component had been
supplied as order and properly installed in laboratory environment.
For examples:
• Manual / operating instruction ?
CALIBRATION
• Power supply – voltage 110/220 V and frequency 50/60

hertz ?
• Test reference, CRM/SRM?

• Spare parts or accessories required ? – tubing, electrical
cable, tools, PC software etc
IQ/OQ EQUIPMENT – NEW
Operational Qualification (OQ) - establish documented

evidence that the operation is effective and reproducible.
For example
• Power on – initializing system?
• Test Program - min /max range setting?
CALIBRATION
• Run CRM / SRM- check repeatability / recovery ?

Bad experiences
• High Temp Oil bath burnt/ short circuit because of plugged into
220V power supply instead of 110V, required transformer.
• pH meter –Oakton received with out electrode
PURPOSE OF CALIBRATION
There are three main reasons for having instruments
calibrated:
To ensure readings from an instrument are

consistent with other measurements.
CALIBRATION
To determine the accuracy of the instrument

readings.
To establish the reliability of the instrument i.e. that it

can be trusted.
CALIBRATION
ENVIRONMENTAL
CONTROL
When weighing is performed, verify the following

conditions:
 Humidity, 40% - 60%, stable ± 10%/ 4 h

CALIBRATION
 Temperature, 20 - 23 deg C, stable ± 1 deg C / 1h

 Air currents / drafts are minimized
Anti vibration for balances

INTERVAL OF CALIBRATION OR VERIFICATION
 In order to continuously perform correct measurements,

utilized measuring and test equipment must be monitored
and calibrated on a regular basis. The corresponding time
period is known as the calibration interval . In the
laboratory as below
CALIBRATION
Measuring Equipment Verification Calibration Interval Calibratio

Interval n type
pH meter As required Daily In-house

Balances As required Every 6 month In-house
Balances N/A Every 5 years External
Gas Chromatography Weekly Weekly In-house
SVM 3000 Viscosity / density meter As required Every 2 years External
Thermometer N/A Every 5 year External

MEASUREMENT STANDARD AND INTERMEDIATE
CHECK
Refer to WI-QA-024 (ISO 17025) as below:
 This is intended to maintain confidence in the calibration status of
reference, primary, working standard and reference materials.
 Allreference standards and materials being use in the laboratory shall

be carried out verification at least once in two years. For examples
 Reference Standards
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 Troemner’s Standard Weight for balances

 Standard thermometer
 Reference Materials
 Fatty acid standards
 Fatty alcohol standards
 Hydrocarbon standards
 Verified results shall meet the tolerance.
CALIBRATION TRACEABILTY
ADJUSTMENT OR RE-ADJUSTMENT
 Adjustment - defined as the '... operation of bringing a

measuring instrument into a state of performance suitable for its
use (VIM)
 Equipment often has the capability for adjustment. This
requirement ensures that you make the necessary adjustments to
keep the equipment operating correctly.
CALIBRATION
Examples
 Respond Factor - In general , is defined as the ratio
between the concentration of a compound being analyzed
and the response of the detector to that compound.
Response Factor (F) = True value / reading value

Corrected result = F x Read value
ADJUSTMENT OR RE-ADJUSTMENT
 Correction Factor -
In thermometer / volumetric calibration as below:
 Thermometer correction :
Corrected temperature = read temperature ± correction
factor , which correction factor obtained from calibration
against standard thermometer
CALIBRATION
 Regression Linear – relationship between two variables by fitting

a linear equation to observed data
Corrected result (Y) = aX + b, where X is the explanatory

variable and Y is the dependent variable. The slope of the line is
a, and b is the intercept (the value of y when x = 0).
a and b obtained from measurement of standards.
CALIBRATION - TOLERANCE AND STATUS
Tolerance is defined as the maximum allowable deviation

between a standard of known accuracy and your instrument.
 Equipment inaccuracies that exceed the specified tolerance can
usually be adjusted
 For example –
CALIBRATION
A standard weight is known to be 5.000g

 Measurement  5.05 g, depending on accuracy required, this may
pass or fail
 If a required tolerance of ± 0.02 g means the scale failed

calibration.
 If the tolerance of ± 0.10 g means the scale has passed
 Tolerance is set by:
 Manufacturer
 User – fit for requirements, but not allowed tighter than
manufacturer’s tolerance.
CALIBRATION
 Tolerance is set by:
.
CALIBRATION
 Equipment Tolerance
Equipment Standards % RSD Max Deviation

. (Absolute)
GC 50-100 % of Ci 1.0 0.5 %
20.0 - 49.9 2.0 0.4 %

CALIBRATION
4.0 – 19.9 5.0 0.3 %
1.0 – 3.9 15.0 0.2 %
< 1.0 30.0 0.05 %

pH meter Buffer 4.00; - 0.1 unit
Buffer 7.00 - 0.1 unit
Buffer 10.00 - 0.1 unit
Analytical Balance 100 g & 50 g - 0.5 mg
Top Loading Balance 100 g & 50 g - 0.10 g

SAFEGUARD FROM ADJUSTMENTS
 The intent is to ensure that QA personnelcannot

inadvertently make an adjustment that impacts the
measurement (invalid results)
Typically, QA personnel adjustments are on the front

panel and calibration adjustments are inside. For GC to
CALIBRATION
create password to lock EPC and temperature setting.

 The standard approach is have a seal that must be

broken to get at the calibration adjustments.
They are often adhesive paper circles placed so they

must be broken if the equipment is opened.
DAMAGE AND DETERIORATION PROTECTION
Measuring equipment shall be protected from

damage and deterioration during handling,
maintenance, and storage-
Be sure the equipment isn’t damaged by use, handling,

maintenance, or storage.
CALIBRATION
 For example, if you drop a piece of equipment and create

latent damage, you won’t be able to detect it by looking. You
should have it recalibrated.
Similarly, equipment that could be damage by temperature

extremes or excessive moisture should be stored (especially
long term storage) inside a heated facility.
RECORDS
 ISO 9001 – Clause 7.6 …. Record of the results of calibration and verification shall be
maintained (see 4.2.4)
The records must include:
 Equipment identification
 Calibration dates
 Name of the person performing calibration
CALIBRATION
 Next calibration date or Due date

 Status of Calibration
 The records often take two forms:
 Equipment’s calibration Report

 Calibration Tag
RECORDS
 Equipment’s calibration Report

CALIBRATION
CALIBRATION

Calibration Sticker
RECORDS
COMPUTER SOFTWARE ABILITY
ISO 9001 Clause 7.6 -When used in the monitoring and measurement of
specified requirements, the ability of computer software to satisfy the intended
application shall be confirmed. This shall be undertaken prior to initial use and
reconfirmed as necessary.
For example , GC, Bomb Calorimeter, Multi EA, SVM 3000,TOC analyzer, etc
Software used in monitoring and measuring needs to be
confirmed. Think of this as verification and validation (see IQ/OQ
report)
CALIBRATION
 The confirmation happens before the software is used initially

and whenever it is necessary to reconfirm.
 Two things could trigger reconfirmation

 The same software has new intended application, e.g., a new
model of an existing product
 Revised software used in the current intended application,
TOC analyzer.
In addition, a nonconformity may point to the need to
reconfirm software.
CASE – FOUND EQUIPMENT NOT CONFORMANCE
Out of calibration equipment ??
Assess and record the validity of the previous measuring

results when the equipment is found not to conform to
requirements.
Take appropriate action on the equipment and any product

CALIBRATION
affected as below which depend on how critical the

measurement is.
• Re-test the product since last calibration

• Rework the product if required
• Recall the product
EQUIPMENT MAINTENANCE
 Maintenance divided into two categories:
 Preventive maintenance – an activity performed regularly (scheduled)
to keep equipment in an existing state, prevent deterioration or
failure.
 Corrective Maintenance – an activity performed after failure has

occurred and intended to restore an item to a STATE in which it can
perform its required function.
CALIBRATION
Equipment 1W 3M 6M 1Y
GC Septum, liner, Column Column, Gas purifier

split vent trap
pH meter Electrolyte Electrolyte Electrode Electrode
Dosimat - - Piston Piston
Spectro - - cell cell

CALIBRATION PROCEDURES
 Calibration procedures are described in following work instruction:
WI No. Descriptions
EOB-WI-QA-003 KF Volumetric – Titer
EOB-WI-QA-005 LICO Colorimeter – APHA Color verification
EOB-WI-QA-013 HFP Analyzer – Flash Point Verification
EOB-WI-QA-031 Gas Analyzer Calibration - Factor
CALIBRATION
EOB-WI-QA-036 pH Meter Calibration

EOB-WI-QA-038 Conductivity Calibration
EOB-WI-QA-039 HACH DR/890 Colorimeter – Turbidity Verification
EOB-WI-QA-098 Gas Chromatography Calibration

EOB-WI-QA-103 Analytical Balance Calibration
EOB-WI-QA-104 SVM 3000- Viscosity / Density Calibration
CALIBRATION

Introduction To Calibrations

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PT.

CALIBRATION ACCURACY VS PRECISION

Installation Qualification (IQ) – provides documented

• Power supply – voltage 110/220 V and frequency 50/60

• Test reference, CRM/SRM?

Operational Qualification (OQ) - establish documented

• Run CRM / SRM- check repeatability / recovery ?

To ensure readings from an instrument are

To determine the accuracy of the instrument

To establish the reliability of the instrument i.e. that it

When weighing is performed, verify the following

 Humidity, 40% - 60%, stable ± 10%/ 4 h

 Temperature, 20 - 23 deg C, stable ± 1 deg C / 1h

 Air currents / drafts are minimized

Anti vibration for balances

 In order to continuously perform correct measurements,

Measuring Equipment Verification Calibration Interval Calibratio

pH meter As required Daily In-house

Thermometer N/A Every 5 year External

 Allreference standards and materials being use in the laboratory shall

 Troemner’s Standard Weight for balances

 Adjustment - defined as the '... operation of bringing a

and the response of the detector to that compound.

Response Factor (F) = True value / reading value

 Regression Linear – relationship between two variables by fitting

a linear equation to observed data

Corrected result (Y) = aX + b, where X is the explanatory

Tolerance is defined as the maximum allowable deviation

A standard weight is known to be 5.000g

 If a required tolerance of ± 0.02 g means the scale failed

Equipment Standards % RSD Max Deviation

20.0 - 49.9 2.0 0.4 %

4.0 – 19.9 5.0 0.3 %

1.0 – 3.9 15.0 0.2 %

< 1.0 30.0 0.05 %

pH meter Buffer 4.00; - 0.1 unit

Buffer 7.00 - 0.1 unit

Buffer 10.00 - 0.1 unit

Analytical Balance 100 g & 50 g - 0.5 mg

Top Loading Balance 100 g & 50 g - 0.10 g

 The intent is to ensure that QA personnelcannot

Typically, QA personnel adjustments are on the front

create password to lock EPC and temperature setting.

 The standard approach is have a seal that must be

They are often adhesive paper circles placed so they

Measuring equipment shall be protected from

Be sure the equipment isn’t damaged by use, handling,

 For example, if you drop a piece of equipment and create

should have it recalibrated.

Similarly, equipment that could be damage by temperature

The records must include:

 Next calibration date or Due date

 The records often take two forms:

 Equipment’s calibration Report

 Equipment’s calibration Report

 The confirmation happens before the software is used initially

 Two things could trigger reconfirmation

Out of calibration equipment ??

Assess and record the validity of the previous measuring

Take appropriate action on the equipment and any product

affected as below which depend on how critical the

• Re-test the product since last calibration

 Corrective Maintenance – an activity performed after failure has