SOP for Measurement of Uncertainty (MOU]

1.0 Objective:

This SOP describes detailed procedure for estimating Measurement of Uncertainty (MOU] associated
with any measurement activity.

2.0 Scope:

Applicable for use in testing and calibration laboratories.

3.0 Responsibility:

All Associates are responsible for estimating uncertainty.

QA Officer/QA Manager: Review the records and governing the document.

4.0 Procedure:

4.1 Information

ISO/IEC 17025 guidelines, Quality Manual, And NABL 141 requirements.

4.2 Frequency

Once for all data analyzed and as and when new method/process/equipment arrives.

4.3 Step by Step Instructions

Measurement of Uncertainty (MOU):

MOU is defined as “A parameter associated with the result of a measurement that characterizes the
dispersion of the values that could reasonably be attributed to the measurand”
Process of MOU calculations involves following four steps;

Step 1: Specify Measurand

Clearly mention what is being measured and also its relationship with input quantities on which it
depends.

Step 2: Identify source of uncertainty

List all possible sources of uncertainty including sources from chemical assumptions. (Sources of
uncertainty may arise from various sources, e.g. Sampling, Matrix effect, Interferences, Environmental
conditions, uncertainty due to mass and glass wares, reference values being used, approximation and
assumptions, random variations, repeatability and reproducibility of method used,
equipment/instruments used, and operator specific.)

Step 3: Quantify uncertainty components

Measure uncertainty component associated with each potential identified source. Check whether
available data accounts sufficiently for all sources of uncertainty.

Step 4: Calculate Standard uncertainty

Each component of uncertainty that contributes to measurement of uncertainty is expressed by an

estimated standard deviation termed as standard uncertainty U 1 and is equal to the positive square root
of variance U12.

Step 4: Calculate Combined uncertainty

Express the individual uncertainties calculated in step 3 as standard deviation and combined them as per
rule. Uc is calculated square root of the sum of the squares based on the law of propagation of
uncertainty.

Uc = √ U12+ U12+ U12+ U12+………….+ Un2

Step 5: Calculate Expanded uncertainty

Expanded uncertainty Ue is determined by multiplying Uc with coverage factor “k” such that the
estimated true value of a measurement result Y may lie within “y - U c “ and “y + Uc “ values, where “y” is
the measured value of the parameter Y = y ± U.

The coverage factor k is generally taken as 2, which is equivalent to a confidence level of 95%.

Methods for estimating Numerical Values of Uncertainty:

There are two methods to estimate numerical values of uncertainty;

Method 1: Type A Evaluation and

Method 2: Type B Evaluation.

Type A Evaluation of standard uncertainty:

ü Type A evaluation of standard uncertainty is the method of evaluating the uncertainty by statistical
analysis of a series of observation.

ü Here, standard uncertainty is the experimental standard deviation of the mean that follows from
averaging or an appropriate regression analysis.

ü Estimation is based on analysis of a series of observations by a valid statistical method.

ü Type A evaluation of standard uncertainty applies to situation where several independent

observations have been made under the same condition of measurement. If there is sufficient resolution
in the measurement process, there will be an observable scatter or spread in the values obtained.

ü Type A evaluation of standard uncertainty (U i) generally arise out of random effects and follows a
“Gaussian curve” or a normal probability distribution and the same is calculated using following formula;
Ui = SD/N or RSD = SD/ Mean of observations; N is no of observations recorded to get mean and SD.

SD – Standard Deviation;

SD Calculation: It is the amount of variation from the average of a set of a data. It is calculated using
following formulae;

SD (n) = √ ∑ (X – X) 2 / n-1

Where;

X = Individual Measurement

X = Average Measurement (Mean)

n = Number of measurements

Type B Evaluation of Standard Uncertainty:

ü This is another method of evaluation of uncertainty by means other than the statistical analysis of a
series of observations. The standard uncertainty is “ u (Xi) “ is evaluated by scientific judgment based on
all available information on the possible variability of Xi (measurand).

ü Values belonging to this category may be derived from;

· Previous measurement data

· Experience with behavior and properties of relevant materials and instruments

· Manufacturers specification

· Data provided in calibration and other certificates

· Uncertainties assigned to reference data taken from handbooks.

ü Type B evaluation of standard uncertainty can be as reliable as Type A evaluation of standard
uncertainty, especially in a measurement situation where a Type A evaluation is based only on a small
number of statistical independent observations.

ü During testing or calibration the maximum error at any point is considered as the accuracy class of the
equipment. If A is the accuracy of the measuring equipment, then for rectangular probability distribution
standard uncertainty (Ui) is calculated using the formula;

(Ui) = √ A2/k

Where;

K=2 at 95% confidence level (CL) and k = 3, at 99% CL.

ü The contribution to the standard uncertainties due to different factors are tabulated in the following
format; n 1-1

Source of Type Ui Value Divisor Degree of Standard

uncertainty freedom Uncertainty

Chemist A U1 SD1 1 n 1-1 SD1/N or

SD1/M

Sampling A U2 SD2 1 n 2-1 SD1/N or

SD1/M

Envt. A U3 SD3 1 n 3-1 SD1/N or

Conditions SD1/M

Reference B U4 X4 √3 or √6 X4/√3or √6
Material

Instrument B U5(1) X5(1) √3 or ∞ X5/√3or √6

Accuracy

Calibration B U5(2) X5(2) √3 or ∞ X5/√3or √6

Uncertainty
Note1: n1 , n2, n3….. are number of observations while testing variation in work piece and variation due
to instrument respectively.

Note 2:When calculating expanded uncertainty using uncertainty values from external calibration
certificates, the divisor for U5(2) divisor is 2.

When to use Normal distribution:

Sometimes quoted uncertainty is an input or output quantity stated along with level of confidence. In
such cases, value of coverage factor needs to be defined, so that the quoted uncertainty may be divided
by this coverage factor to obtain the value of standard uncertainty. When distribution type is not known,
it may be assumed to be normal values of the coverage factor. Various levels of confidence for a normal
distribution are as follows;

Confidence 68.27% 90% 95% 95.45% 99% 99.73%

Level (CL)

Coverage 1.000 1.645 1.960 2.000 2.576 3.000

factor (k)

When to use Rectangular distribution:

In some cases where it is possible to estimate only upper and lower limits of an input quantity and there
is no specific knowledge about the concentration of values within interval, one can assume that it has
equal probability to lie anywhere within interval ( rectangular distribution). In such cases, quoted
uncertainty may be divided by coverage factor √3 to obtain the value of standard uncertainty.

TABLE

Assumed Expression used to Comments or examples

probability obtain the standard

distribution uncertainty
 A digital
thermometer has a least significant digit of
0.1°C. The numeric rounding caused by finite
resolution will have semi-range limits of 0.05°C.
Thus the corresponding standard uncertainty
Rectangular U (Xi) = ai/√3 will be

U (Xi) = ai/√3 = 0.05/ 1.732 = 0.029°C.

A tensile testing machine is used in a testing

laboratory where the air temperature can vary
randomly but does not depart from the
nominal value by more than 3°C. The machine
has a large thermal mass and is therefore most

likely to be at the mean air temperature, with

Triangular U (Xi) = ai/√6 no probability of being outside the 3°C limits. It
is reasonable to assume a triangular
distribution, therefore the standard uncertainty
for

U (Xi) = ai/√6 = 3/ 2.449 = 1.2°C.

Normal A statistical evaluation of repeatability gives the

result in terms of one standard deviation;
(from U (X1) = S (q¯) therefore no further processing is required.
repeatability

evaluation)

A calibration certificate normally quotes an

expanded uncertainty U at a specified, high
Normal coverage probability. A coverage factor, k, will
(from a U (Xi) = U/k have been used to obtain this expanded
uncertainty from the combination of standard
calibration
uncertainties. It is therefore necessary to divide
certificate) the expanded uncertainty by the same
coverage factor to obtain the standard
uncertainty.
 Some manufacturers’ specifications are quoted
at a given coverage probability (sometimes
Normal U(Xi) = referred to as confidence level), e.g. 95% or
(from a Tolerance limit/k 99%. In such cases, a normal distribution

manufacturer’s can be assumed and the tolerance limit is

divided by the coverage factor k for the stated
specification coverage probability. For a coverage probability
of 95%, k = 2 and for a coverage

probability of 99%, k = 2.58.

If a coverage probability is not stated then a

rectangular distribution should be assumed.

Steps to summarize an estimate of Uncertainty associated with measurand:

Step 1 Specification of Measurand Write down clear statement about what

is to be measured including relationship
between measurand and parameters on
which it depends.

Step 2 Identification of uncertainty List out all the possible sources of

sources uncertainty associated with the input
quantities that contribute to the value of
the measurand.

Step 3 Quantify components of Estimate the size of uncertainty

uncertainty associated with each potential source of
uncertainty defined.

Step 4 Calculate Total uncertainty Combine the quantified uncertainty

component expressed as standard
deviations. As per appropriate rule to
give a combined standard uncertainty, U c.

Evaluation of Combined Uncertainty:

Rule 1- When all the calculated uncertainties are of same units:

After measuring the individual uncertainty due to type A and type B, the combined uncertainty (U c) is
calculated as follows;

Uc = √ (U12 + U12 + U12+……)

Where;

U1, U2, U3 etc are uncertainties calculated with same units.

Rule 2- When all the calculated uncertainties are of different units:

Uncertainty

Combined Uncertainty = Result Declared ×

Expected value or mean value

Uc = √ (R1×U1/V1) + (R1×U1/V1)+……

Where; U1, U2, U3 etc are uncertainties calculated R1, R2 etc are the result declared V1, V2 etc are the
expected value or mean value.

Combined Uncertainty of Precision:

Up = √ U12 + U12 + U12

As per rule 1.

Total Combined Uncertainty:

After measuring the individual uncertainty due to Type A and Type B, the combined uncertainty (U c ) is
calculated as;

Uc = √ Up2 + U42 + U5(1)2 + U5(2)2

Expanded Uncertainty:

The product of combined uncertainty and coverage factor (k) gives the expanded uncertainty. The
expanded uncertainty (Ue) calculated as;

Ue = Uc × 2

K is the coverage factor for different effective degree of freedom at 95% CL.

Final Result = Mean Value ± Ue

5. References

1. Clause 5.4.6 of ISO/IEC 17025:2005 guidelines,

2. Purchase specifications
3. NABL 141

4. Eurachem/CITAC guide for “Quantifying uncertainty in Analytical Measurement”

6.0 Documentation:

All the data of uncertainty parameters will be recorded and it will be filed in the respective files.

7.0 History of Revision:

Revision No. Effective Date Revision details Reason for revision