3/8/2010

Statistical Applications in
L b
Laboratories
i &
Uncertainty Estimation
Dr. Ashraf
s a S S. Youssef
ousse
Senior Member, ASQ
Quality Assurance Manager

Course Introduction

„ Welcome to training by
NRC!
„ Instructors introduction.
„ Participants
introduction: Please
p
complete “Participant
p
Profile” in your manual.

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Learning Objectives
„ Gain integrated perspective of statistical applications
in laboratories.
„ Understand the Sampling
p g & Normal distribution.
„ Learn Hypothesis test.
„ Learn Uncertainty Estimation technique.

Ashraf Youssef

Our Objective
You Enjoy While You Learn

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Training Approach

„ Focus on Basics
„ Interactive
„ Case Studies
„ Games
„ Exercises
„ Fun !!!!!!!!!!!!!!!!!!

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Agenda

1. Basic Statistical 2. Significant figures

Concepts rules
u es
„ Accuracy & Precision 3. Probability
„ Descriptive Statistics. Distributions
„ Inferential Statistics 4. Control charts
„ Method of Least Square 5. Sampling Plans

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Statistical Overview

Population
A llarge N
No. off N
Mean = µ
Standard Deviation = σ

Sample
A small No. of n
Sample Mean = X
Sample Standard
Deviation = s

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Accuracy & Precision

____________ ____________ ____________ ____________

____________ ____________ ____________ ____________

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Descriptive Statistics
„ Centrality Measures
¾ Mode
¾ Median
¾ Mean
„ Dispersion Measures
¾ Range
¾ Variance
¾ Standard Deviation
¾ Coefficient of Variation

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Exercise: Centrality Measures

„ Calculate the sample

mode, median and the
mean of the following
data set.
‰ Set A: 20, 20, 18, 17,
15,
5, 17,, 14,, 17,, 12,, 10
0
‰ Set B: 10, 20, 12, 13, 13,
16, 17, 12, 13, 17, 22

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Exercise: Dispersion Measures

„ Calculate the sample

range, variance,
standard deviation and
coefficient of variation.
‰ Set A: 20, 20, 18, 17,
15,
5, 17,, 14,, 17,, 12,, 10
0
‰ Set B: 10, 20, 12, 13, 13,
16, 17, 12, 13, 17, 22

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Exercise: Descriptive Measures

Sample Percents
„ The following Isooctane
measurements were 1 3.83
obtained for the 2 3.94
analysis of isooctane 3 3.88

in gasoline. 4 3.97
5 3.90
6 3.94

• Calculate X , S, and the C.V

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Estimate of Standard Deviation from

a Pair of Results (X1 and X2)
„ In case of a single
g duplicate
p p
pair of
measurements, the equation for the standard
deviation can be significantly reduced as follows

D X − X2
S= = 1
n 2

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Estimate of Standard Deviation from

Duplicate Measurements
„ For a set of measurements consisting g of p
pairs of
duplicate results, the standard deviation can be
estimated as follows:

S=
∑D 2

2k
ƒ Where K = the number of sets of
duplicates
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Combining (Pooling) Estimates of

Standard Deviations
„ It is p
possible to p
pool ((combine)) several estimates
of standard deviation using the following
equation:

Sp =
∑ν S i i
2

∑ν i

ƒ Where vi = the number of sets of

duplicates
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Exercise: Duplicates & Pooling

Sample Percents Percents
„ The following pairs of Isooctane Isooctane
duplicate results were
1 3.81 3.83
obtained for the
2 3.88 3.94
analysis of isooctane
3 3.85 3.88
in gasoline. 4 3.97 3.89

• Calculate S, and Sp

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Hypothesis Testing
„ Common questions that can be answered using
the null hypothesis approach:

¾ Is the mean of the data set significantly different from

the true value?
¾ Are the means of two different sets significantly
different?
¾ Are the precisions of two different data sets
significantly different?

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Test 1: Comparing the Mean With

the True Value
„ The largest difference that could be expected
as a result of indeterminate error is given by:
s
± t( )
n
− s
H o : ( X − μ ) p± t ( )
n
− s
H1 : ( X − μ ) f ± t ( )
n

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Test 2: Comparing Two Means

„ There are two occasions when we wish to

determine if two independently obtained results
are essentially the same.
− − n1 + n 2
H o : ( X 1 − X 2 ) p ± ts p
n1 n 2

− − n1 + n 2
H 1 : ( X 1 − X 2 ) f ± ts p
n1 n 2

Where Sp is the pooled standard deviation of the two samples.

( n1 − 1) S 1 + (n2 − 1) S 2
2 2

Sp =
n1 + n2 − 2

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Exercise: Comparing Two

Means
„ Compare the two
means, of the following
data set.
‰ Set A: 20, 20, 18, 17,
15, 17, 14, 17, 12, 10
‰ Set B: 10,
10 20
20, 12
12, 13
13, 13
13,
16, 17, 12, 13, 17, 22

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Test 3: Comparing Two

Precisions
„ To determine if the standard deviation from
one data set is significantly different from the
standard deviation of another data set
H o : Fc p Ft
H 1 : Fc f Ft
2

Fc =
Var1
= S 1
2
Var 2 S 2

•The larger variance is always numerator.

•Ft is the expected tolerance base on Normal distribution.

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Exercise: Comparing Two

Precisions
„ A ship of copper ore was purchased by a
local metal refiner. The analysis certificate
made out while the ship was being loaded,
show that %Cu =14.66 with a standard
deviation of 0.07% for 5 measurements.
When the ore arrived at the refinery, it was
analyzed and the following results were
obtained: %Cu = 14.58,
14 58 14.61,
14 61 14.69,
14 69
14.69, and 14.64. Should the refiner accept
the ore?

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Regression Analysis
„ Regression Analysis is a technique used for
obtaining the “best” line from a set of data, and
for specifying the uncertainties of that line.

„ The simplest regression analysis for a straight

line is called the least squares method of.

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Method of Least Square

a
X

Where: a is the intercept (Value of y when X=0)

b is the slope of the line

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Exercise: Regression Analysis

„ The following calibration data, assuming
p exists and the
a linear relationship
concentration is the independent
variable, using least square method,
calculate the slope and intercept of the
best-fit line.
Concentration (ppm) Signal
1.00 0.116
2.50 0.281
5.00 0.567
7.50 0.880
10.00 1.074

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Sample Collection
ƒ Most common source of analysis error.
ƒ Sample should be representative.
representative
ƒ Use sampling plans that are based on
appropriate statistical methods, whenever
reasonable.

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Sample Collection
ƒ The laboratory personnel and sample
collectors cooperate
p in establishing
g
Sampling Protocol.
ƒ The samples preparation and storage must
be made away from analysis area to avoid
contamination.

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Sampling Protocol
ƒ Should include the following:
¾ Sample size.
¾ Container type.
¾ Labeling.
¾ Preservation of sample.
¾ How to transport sample to lab.

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Significant Figures Rules

ƒ Rule1: Include all digits that are
known with certainty plus the first
uncertain digit. These digits are
called significant figures.

ƒ Rule 2: The last digit in a number is

assumed to be uncertain by +/-+/ 1
unless otherwise specified.

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Exercise: Significant Figures

Measure Measure
1 1
Uncertainty Uncertainty
2 2
Sig. Fig. Sig. Fig.

3 3

Which measurement is more precise?

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More Significant Figures Rules

ƒ Rule 3: Zeros that lie to the left of
the first nonzero digit are not
counted as significant figures
figures.
ƒ Rule 4: In a measured quantity, a
zero that lies to the right of the
decimal point, and which also lies to
the right of the first non-zero digit,
counts as a significant figure
figure.
Significant figure is the number
0.0054070
are _________

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Rounding Rules
ƒ Rule1: If the digit to be discarded is
5 or greater, increase the retained
preceding digit by 1.1 If it is less than
5, do not change the preceding digit.
Round one digit 1.047 =

ƒ Rule 2: When more than one digit is

to be dropped, Rule 1 is applied only
one time
i to the
h fifirst di
digiti ffollowing
ll i
the last retained digit.
Round two digits 1.047 =

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Addition & Subtraction

ƒ Rule1: The absolute uncertainty in a
sum or difference cannot be smaller
than the largest absolute uncertainty
in any of the terms in the calculation.
In other words, retain as many digits
to the right of the decimal as is found
in the number with the fewest digits
to the right of the decimal.
12.2 + 0.365 + 1.03 =

8.35 - 0.365 =

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Addition & Subtraction

ƒ Rule 2: When the numbers to be added
or subtracted have exponents, they must
b made
be d tto h
have th
the same exponentt
before addition or subtraction is carried
out

(5.6 x 10-2) + (3.2 x 10-1) =

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Multiplication & Division

ƒ Rule 1: Keep as many significant
figures in the final answer as is
found in the value with the least
number of significant figures.
6.2 x 7.00 = 3.142 / 8.05 =

ƒ Rule 2: Keep as many significant

figures in the final answer as is
f
foundd in
i th
the measured d value
l whenh
using an exact number.
5.0367 kg = _________________ gm

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Mixed Operation
ƒ General rule: The rules for problems
combining g addition/subtraction and
multiplication/division are applied
individually to each operation as it is
performed.

144.3 + (2.54 x 8.3) =

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Data Presentation:
ASTM Recommendations
ƒ Presents as a minimum, the average, g the
standard deviation, and the number of
observations.
ƒ If the number of observations is large,
present data in a grouped frequency.
ƒ P
Present t as much
h evidence
id as possible
ibl
that the data were obtained under
controlled conditions.
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Exercise: Measurement
Operation Results
((4.16x10-3) + ((1.724x10-1)

1.074 X 0.993

(40.1 X 0.1633)/204.228

((21.6 X 0.317)/4.1) + 16.037

(62 31 + 62
(62.31 62.47)/2
47)/2

9.1647 Round off to three significant digits

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Measurement: Objectives

„ To assess limits of error in measurements.

„ To reduce analytical errors to acceptable
levels.
„ To reduce amount of work needed to obtain
reliable results.
„ To provide basis for inter-comparison
inter comparison of
data.

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Measurement: Basic
Requirements
„ Understand the nature of errors.
„ Understand the measurement system
used.
„ Develop techniques and plans to
minimize errors.
„ Implement quality control measures.
measures
„ Establish quality assessment and quality
assurance measures.

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Measurements:
Quality Parameters
A laboratory is expected to be able to
specify the quality of its data in quantitative
terms. This requires
¾ Qualitative identification of the
measurements.
¾ Limits of certainty – needed to judge
confidence associated with the numerical
value.
l
¾ Quantitative accuracy.
¾ Probability distribution of data.

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Type of Measurement Errors

ƒ Systematic (or Determinate) Errors

¾ May cause the results to be high or low
low.
¾ Can be constant or variable.
¾ Can be determined and eliminated.
ƒ Random (or Indeterminate) Errors
¾ Occur in a symmetrical fashion around the real
value.
a ue
¾ Cannot be determined, controlled or eliminated.

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Methods Used to Detect

Systematic Errors
ƒ Use of standard samples of known
characteristics and performance.
ƒ Independent analysis (use different method
or send your sample to other labs).
ƒ Compare
p with different sample
p size.

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Measurement Accuracy &

Precision (Reproducibility)
ƒ The accuracy can be measured as:
¾ Absolute error for a single measurement,
Eabs = |xi – μ|
¾ Absolute error for a mean,
Eabs = |x – μ|
¾ Relative error = 100 * (Eabs/ μ)
ƒ The precision can be measured as:
ƒ Absolute deviation for a single measurement
d=|xi – x|
ƒ Relative deviation, drel = 100 * (d / x)

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Measures of Precision
(more than one measurement)
ƒ Range.
g
ƒ Relative range.
ƒ Average deviation of a sample.
ƒ Standard deviation of a sample.
ƒ Relative
e at e sta
standard
da d de
deviation
at o (C
(CV).
)

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How To Decrease Calibration

Uncertainty?
ƒ Increase the number of calibration
points
i t narrows th the b
band,
d as ddoes
increasing the number of
independent measurements of
each calibration standard.
ƒ Whenever p possible,, using
g the line
in its region of smallest uncertainty.
ƒ Avoiding extrapolation.

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Probability Distributions

ƒ Uniform
U if Di
Distribution
t ib ti SS=a/sqrt(3)
/ t(3)
ƒ Triangle Distribution S=a/sqrt(6)
ƒ Normal Distribution
ƒ T-Distribution
ƒ U-Distribution S=a/sqrt(2)

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Statistical Quality Control

„ Quality Engineering
„ Variability
„ Statistical Methods
„ Variable and Attributes
„ Specifications
„ Upper and Lower Specifications limits .

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Quality Characteristics

„ Physical
„ Sensory
„ Time Orientation

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Statistical Methods for Quality

Improvement
„ Acceptance Sampling
„ Statistical Process Control Charts (SPC)
„ Design of Experiments
„ Process Capability studies

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Statistical Quality Control

„ Statistical : With the help of numbers of data

„ Quality : We study the characteristics

process
„ Control : In order to make it behave the way
we want it to behave

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Cont.:
Statistical Quality Control
Can be applied to:
„ Engineering Problems

„ Inspection Problems

„ Operating Problems

„ Management Problems

„ Accounting and Clerical Problems

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Process:

„ Is any set of conditions, or set of causes,

which work together to produce a given
results.

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Control Charts Types

„ Variables Control Chart

„ Attributes Control Charts

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Type of Variations in Production

„ Within-Piece Variation
„ Piece-To-Piece Variation
„ Time-To-Time Variation

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Sources of Variation

„ Equipment
„ Material
„ Environment
„ Operator
„ Inspection Activity

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Causes of Variation

„ Chance Causes
These causes are difficult to detect.
„ Assignable Causes
They are large and readily identified

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The Control Chart Method

„ A graphical record of the quality of a

particular characteristics
„ It shows if the process is in a stable state with
chance causes of variation or not.

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Variables Control Charts

„ X-bar and R Charts

„ X-bar and S Charts
„ MA Control Charts

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Objectives of Variable Control

Charts
„ Quality Improvement
„ Determine the Process Capability
„ Setting Effective Specification Limits
„ Deciding to release the product to the next
phase or not

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Control Chart Building Technique

„ Select the Quality Characteristics

„ Choose the Rational Subgroup
„ Collect the Data
„ Determine the Trial Central Line and the
Control Limits
„ Establish the revised Central Line and the
C t l Li
Control Limits
it
„ Achieve the Objectives

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Selection of Quality Characteristics

„ Must be measurable and expressed in numbers

„ Seven basic units were used
a) Lengths e) Substance
b) Mass f) Time
c) Current g) Length intensity d)
Temperature
„ Variables can be treated as Attribute
„ One Characteristic only is selected

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Choosing the Rational Subgroup

„ The Inspection Cost

„ Test (Inspection) Type
„ Pre-Control Rule
„ Keep The results in tighter and sensitive
Control Limits
Usually sample of 5 is taken

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Establish X-bar and R Charts

X Chart R Chart

UCL X = X + Aσ 0 UCL R = D2 σ 0

LCL R = D1σ 0
LCL X = X − Aσ 0

R
Where σ0 =
d2

A, D1, D2 and
A d d2
are factors computed
related to the sample
size, and listed at
Appendix A
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Establish X- bar and S Charts

s
∑n
X Chart
S =

UCL = X + Aσ 0 UCL S = B6σ 0

X
LCL = B5σ 0
LCL X
= X − Aσ 0 S

S
W here σ0 =
ca
S = Standard Deviation/Sample
n = N o. of Samples

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State of Control

1. Process in Control
2. Process out of Control
A point is outside the 3σ
limits
A nonrandom behavior is
observed in the points

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Interpretation of the Control Charts

Western Electric Rules (AT&T Rules) are

used to decide about out of control condition.
There are 10 rules were used.

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AT&T Rules

„ One or more points outside Control Limits

„ Two of three consecutive points outside of 2σ limits
„ Two of three consecutive points outside of 2σ limits
„ A run of 8 consecutive points on one side of the
center line
„ Six points in a row steadily increasing or decreasing

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AT&T Rules Continued

„ Eight points in a row in zone C or beyond

„ Eight points in a row in both sides of the center line
with none in zone C
„ Four points in a row alternating up and down
„ Fifteen points in a row in zone C
„ An unusual and nonrandom pattern

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SPC “Attributes Charts”

Types of Attributes
„ Non-measurable Characteristics

„ Measurements that could not be made due-

to:
a) Time b) Cost
OK Easier to use “go-no-go”
go-no-go gage

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Non Conformity

Definition

Departure of quality characteristics from

required

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The Objectives of Attribute Charts

„ Determine the average quality level

„ Bring to the attention of any changes in the
average level
„ Improve the product quality
„ Evaluate the quality performance
„ Determine the acceptance criteria of a
product
d t

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Attribute Charts Type

„ P-Chart
„ np-Chart
„ C-Chart
„ U-Chart

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P- Chart

„ P- Chart can be produced to measure the quality

produced
p oduced by
by:
a) A Work Center
b) A Department
c) A Shift
d) The entire Plant
„ Also used to report the quality performance of an
operator, a group of operators, or management.

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P-Chart Construction

„ Constant Sample Size

At least 25 subgroups should be collected
P =
∑ nP
n
Where nP is the number of Nonconforming units in each subgroup
n is the sample size for each subgroup

P(1− P) P(1−P)
UCL= P +3 LCL= P −3
n
n

If LCL is negative, replace it with zero value

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P-Chart Construction

„ Variable Sample Size

P =
∑ P
N
where P = Fraction of nonconforming in a single subgroup
N = Number of subgroups

P(1− P) P(1−P)
UCL= P +3 LCL= P −3
n n

where is the average sample size of the subgroups

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nP - Chart

„ nP-Chart is similar to P-Chart

„ It is easier for personnel to understand

„ Sample size must be constant

Center Line = nP

Control Limits = nP±3 nP

P± P(1− P)

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C-Chart

Example for C-Chart

„ No.
No of nonconforming rivets on an airplane
„ Imperfections in a large roll of paper

„ Rust sports on a steel sheet

„ Billing errors

„ Errors in forms

„ Seeds or air pocket in a glassware

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C-Chart Construction

Center Line = C
UCL = C + 3 C

LCL = C − 3 C

Where C = Average number on

nonconformities for a number of subgroups

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U-Chart

If subgroup size varies, U-Chart would be

appropriate
app op ate to use.
use
U=
C
U =
∑C
n ∑n
U
UCL = U + 3
U
LCL = U − 3
n n

Where C = Count of nonconformities in a subgroup

n = Number of unit inspected in a
subgroup

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A Quality Rating System of Nonconformities

(MIL-STD-105D)
1.Critical Nonconformities
2 Major Nonconformities
2.Major
3.Minor Nonconformities

A weight of 9, 3 and 1 points are assigned to

critical, major and minor nonconformities.

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Guidelines for Implementing Control Charts

„ Determine which process characteristics to control

„ Determine where the charts should be implemented
„ Apply control charts to important characteristics
„ Add new charts if necessary
„ Implement and maintain control charts as close to
the work center as possible

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Uncertainties

Definition:
uncertainty
t i t off measurementt is
i a parameter,
t associated
i t d
with the result of a measurement, that characterizes
the dispersion of the values that could reasonably be
attributed to the measured.

Ass a ge
general
e rule,
u e, thee implementation
pe e o of
o thee concept
co cep
of uncertainty of measurement should go in line with
the implementation of ISO/IEC17025.

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Factors contributing to uncertainty

of measurement
1.definition of the measured
2.Sampling
p g
3.transportation, storage and handling of samples
4.preparation of samples
5.environmental and measurement conditions
6.the personnel carrying out the tests
7.variations in the test procedure
8.the measuring instruments
9.calibration standards or reference materials
10.software and/or, in general, methods associated with the
measurement
11.uncertainty arising from correction of the measurement results
for systematic effects.
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Estimating the Minimum Number

of measurements Needed
How do y
you decide how many
y measurements yyou need?

Since X ± (Z*S)/sqrt(n)

E = (Z*S)/sqrt(n)

n = (Z*S/E)2

Round up the n value to the next integer

Ashraf Youssef

Uncertainty Budgets

Source of Standard
Uncertainty Uncertainty
An uncertainty
budget can consist
of only tow
columns

Combined
Uncertainty
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Uncertainty Types

Type A: Uncertainty estimates are those

determined using statistics in the current
measurement Processes.

Type B: Uncertainty estimates are those

determined by any other means.

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Important Definitions (1/2)

Precision: is the closeness of agreement between

independent test results obtained under stipulated
conditions.
conditions

Repeatability: is precision under repeatability

conditions; same laboratory by the same operator
using the same equipment.

Reproducibility: is precision under reproducibility

conditions; different laboratories by different
operators using different equipments

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Important Definitions (2/2)

Bias: is the difference between the expectation of

the test results and an accepted reference value.
value

Trueness: is the closeness of agreement between

the average value obtained from a large set of test
results and an accepted reference value.

Ashraf Youssef

Measurement Equation

y = X + Sum(C
( i)

Where Y is the corrected Value

X is the measured value
Ci are corrections to be added to the
measured value

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Uncertainty Examples

Ures = a/sqrt(3) Follows Rectangular Dist.

Utemp = a/sqrt(6)
/ t(6) F ll
Follows Triangle
Ti l Dist.
Di t
if lab temperature is
controlled by a continuous cooling variable re-
heat system

Utemp = a/sqrt(2)
q ( ) Follows U Dist.
if lab temperature is
controlled simply by an on/off air conditioning
system

Ashraf Youssef

Uncertainty Forms (1/2)

Repeatability Follows Normal Dist.

S l Factor
Scale F t F ll
Follows rectangular
t l Di
Dist.
t
Elastic Deformation Follows rectangular Dist.
Force Setting May be not significant if the caliber
and measured object are made from the same
materials.
p
Temperatures Mayy be follows either U or
Rectangular Dist.
Coefficient of thermal expansion.

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Uncertainty Forms (2/2)

Probe Misalignment Follows Rectangular

Dist. (From Recognized organization (NIST, Or
Manufactures) You can get the value as
estimator)
Calibration Follows Rectangular Dist. (From
historyy of calibration data,, choose the worst
case as estimator).

Ashraf Youssef

Coefficient of Thermal Expansion

∆L = L * ∆T *∆α

Where:

∆L is the error in length

L is the normal length
∆T is the deviation from 20 oC
∆ α is the difference between the coefficients of
expansion of the measured subject and the
coefficient of expansion of the gage.

Ashraf Youssef

47
 3/8/2010

Ex. Uncertainty Budget for 0.5 XX Plain Plug

Gage
Source of Uncertainty Standard
Uncertaint
y (µin)
Master gage block uncertainty (B) 2.0
Repeatability (A) 2.0
Scale error (B) 1.2
Elastic deformation (B) 0.06
Force Setting
g ((B)) 0
Coefficient of thermal expansion (B) 0.48
Part an Master temp. Diff. (B) 0.33
Combined standard Uncertainty uc=SQrt(sum(ui2)) 3.13
Expanded Uncertainty, U=2uc (k=2) @C.L. 95% 6.26

Ashraf Youssef

Ashraf Youssef

48