“The Need, Use and Implementation of Traceability and

Uncertainty Measurements in an Analytical Testing Laboratory.”

 The Need for Good Quality Measurements

Measurement today is more valuable than ever.

We depend on measurement for almost everything -

from time keeping to weather forecasts, from car

speedometers to heavy-duty manufacturing, industrial
research and medical science.
 Good Quality Measurements
 With the advent and systematic implementation of ISO 17025, & ISO 15189 in the analytical and medical
testing community, the need for well-defined robust procedures for the documentation of measurements
is crucial.

 The treatment of both traceability and the assessment of uncertainty have become critical in the
generation of legally defensible analytical data.

 It is essential in the accreditation of testing laboratories that these two elements be seriously addressed
due to their direct and profound impact on the quality of the data produced.
What is the temperature of this room?
 How close can you guess?

 What are you calibrated against?

 Are there interfering factors?

 How critical is the result?

Therefore, a clear understanding of traceability and
uncertainty is paramount for the personnel involved in
making decisions based on measurement results.
Value of World Trade exceeded 17 Trillion, (2005)

A large proportion of this trade is dependent upon

chemical analyses.
(Reliability, Comparability, & Confidence)
 Petrochemicals
 Food
 Pharmaceutical Products
 Medicines
 Ores
 Plastics
 Countless other examples
 Accurate measurement enables us to:

 Maintain quality control during production processes

 Comply with and enforce laws and regulations

 Undertake research and development

 Calibrate instruments and achieve traceability to a national measurement standard

 Develop, maintain and compare national and international measurement standards
 Since measurement plays such a fundamental part in our lives, it is important that the accuracy
of the measurement is fit for purpose, i.e. it fully meets the requirements of the application.

 One way of ensuring that your measurements are accurate is by tracing them back to national
standards. This method of guaranteeing a measurement's accuracy through an unbroken chain
of reference is called traceability.
 "Traceability is the property of the result of a measurement or the value of a standard whereby it can be related to stated references, usually national or
international standards, through an unbroken chain of comparisons, all having stated uncertainties”, VIM

Traceability
Coke recall highlights need for complete traceability
23-Mar-2004
 Coca-Cola recalled its bottled water brand Dasani after finding samples that contained higher than permitted levels of the chemical
bromate.
 The recall of over half a million bottles in the UK took less than 24 hours, and although deeply embarrassing for the soft drinks giant, the recall could have
been much more damaging had the company not put in place adequate traceability measures.
 In a statement, Coca-Cola said that the recent contamination of Dasani water had been initially caused by its regular practice of adding calcium to
the product, calcium which in this case "did not meet our quality standards". As a result, bromate went on to be formed during the manufacturing
processes.
 The UK limit for bromate in bottled and tap water is 10 parts per billion, while the Dasani samples had tested between 10 and 22 parts per billion

 It is clear that Coca-Cola has taken the issue of traceability to heart.

 The company was forced to issue a recall after wood preserve seeped into a vending machine several years prior
 This cost was over $100 million, because no system was in place then that could trace the product back quick enough.
 Hierarchy of Traceability

ty 0.002% National calibration facility

Calibration laboratory
ain

0.01%
ert
nc

0.07% Company master item

u
ing
as

1% Production equipment
re
Inc

5% Final product

Traceability
 Every measurement is inexact and therefore requires a statement of
uncertainty to quantify that inexactness. The uncertainty of a measurement
is the doubt that exists about the result of any measurement.

 “Parameter, associated with the result of a measurement, that characterizes the

dispersion of the values that could reasonably be attributed to the measurand.”, GUM

Uncertainty
 Measurement Uncertainty & Bias
 Bias
 systematic effects; inaccuracy
 Measurement uncertainty (MU)
 random effects; imprecision
MU

-2sd +2sd

Result Bias of procedure

 Estimation of Bias
 Method and Laboratory bias can be estimated from:

 the analysis of certified reference materials

 the participation in proficiency tests
 from recovery experiments

 Sources of bias should always be eliminated if possible

Result Bias of procedure

 Estimation of Uncertainty
Three Step Process (ISO Approach)

 1) Identify all individual components of Uncertainty, (µ)

 Uncertainty in the level of extraction
 Uncertainty in the preparation of solutions
 Uncertainty in the purity of raw material
 Etc.
 Estimation of Uncertainty
 2) Quantify the contribution of each component
 Evaluate both random and systematic effects
 Type A (Evaluated from the statistical distribution of the results of series of measurements and characterised by standard deviations )
 Derived from repeated measurements
 Quality control material
 Duplicate analysis of samples
 Type B (Characterised by standard deviations, evaluated from assumed probability distributions based upon )
 Estimations derived from previous measurement data
 Experience (Professional opinion)
 Manufacturer’s data
 Uncertainties assigned to reference material
 General knowledge
 Estimation of Uncertainty
 3) Combine all the uncertainty components
 “Combined Standard Uncertainty”

 Square root of the sum of the squares

Combined µ = √ ∑ (x-xbar..)2
 Confidence Level
 To generate the confidence interval the combined standard
uncertainty is multiplied with a coverage factor, which gives
the expanded uncertainty.

95% Confidence = CF of 2
Expanded µ = 2 √ ∑ (x-xbar..)2
Confidence level Coverage factor
p k
90% 1.65
95% 1.96
99% 2.58
 So what does this mean
…..in the real world?
 Accreditation requirements
 ISO 17025
 Traceability 5.6.2.1.1
 Operated so as to ensure that calibrations and measurements
made by the laboratory are traceable to the International
System of Units (SI) through an unbroken chain of calibrations
or comparisons…
 Uncertainty 5.4.6.2
 Testing laboratories shall have and shall apply procedures for
estimating uncertainty of measurement.
 So what does this mean
…..in the real world?
Four Primary Questions:
What is needed?
What is practical?, e.g. Good Science
What is fit for use?, e.g. specific application
What can you sell?
 Develop an Uncertainty Budget
 Information needed to prove that a measurement is traceable in the technical sense:
 A list of the significant uncertainty contributors for the measurement.
 A list of the equipment (serial no. etc.) used in the measurement that adds significantly to the uncertainty.
 For each piece of equipment a reference to its traceability (Calibration scope, calibration source, calibration
date and calibration id, e.g. certificate number).
 For each calibration source, evidence of its credibility, e.g. accreditation.

 The requirement of credibility of the calibration source is what ensures that this
information is available at each link in the chain.
 Develop an Uncertainty Budget
 Define elements to answer your four questions
 What do you need to implement to achieve your goal
 Formal (policies, procedures, SOP, QAP)
 Informal (general requirements, brainstorming)

 How are you going to demonstrate objective evidence

 Final reports
 Control charts
Steps for Analytical
Laboratories
 Identify major uncertainty components
(EURACHEM/CITAC Guide)
 Clearly define the basis for the estimate of Uncertainty, when
required to report
 Contract review
 If possible, determine with client end use of data
Steps for Analytical
Laboratories
 Attempt to design robust QC process
 Ensure representative variation of inputs
 Fewer points require more emphasis on design
 May need to record additional data related to precision as objective evidence
 Establish control charts
Steps for Analytical
Laboratories
 Laboratory shall have procedures for monitoring validity of tests, including:
 regular use of CRMs
 participation in interlaboratory comparison or proficiency testing programs
 Record data so trends are detectable
 Laboratories in most cases already have sufficient data for estimating uncertainty
Steps for Analytical
Laboratories
 Make use of PT study data
 Compare internal precision data to spread of results of participants
 If study based on reference value, compare lab result/uncertainty
with reference
 Conclusion
 Traceability and uncertainty are fundamental properties of all measurements. It is only recently that
they have been given a high profile as part of quality assurance and accreditation in Analytical
Testing Laboratories, especially with the emphasis and implementation of ISO/IEC Guide 17025.

 Traceability and the determination of uncertainty are essential in order to establish comparability,
fitness for purpose and legal defensibility. The measurement community has always recognized
their importance but with more stringent regulations and a better educated client base, new focus
needs to be applied to these issues.
Thank you / Questions

Lance Boynton
Quality Director
Absolute Standards,Inc.
(800) 368-1131
www.AbsoluteStandards.com