USE OF CONTROL

CHARTS IN LABS AND

TREND ANALYSIS

BY:
YAMINI BHARDWAJ
SIGMA TEST & RESEARCH CENTRE
Email: [email protected]
 Why control charts and trend
analysis
 According to ISO/IEC 17025:2017 clause 7.7.1
Ensuring the Validity of Results.
 The laboratory shall have a procedure
for monitoring the validity of tests
results.
 The resulting data shall be recorded in
such a way that trends are detectable
and, where practicable, statistical
techniques shall be applied to review the
results.
WWW.SIGMATEST.OR
 CONTROL CHARTS
• The control chart: chart on which some
statistical measure of a series of sample is
plotted in a timely order to steer the
process with respect to that measure and
to control and reduce variation.
• By comparing current data with existing
control charts, one can draw conclusions
about whether the process variation is
consistent (in control) or is unpredictable
(out of control, affected by special causes
of variation). 
WWW.SIGMATEST.OR
 Theoretical basis of control chart
• The control chart is a graphical display of data from process which allow a
visual assessment of the process variability.
• At defined intervals, subgroup of items of a specified size are obtained and
value of characteristic or feature of the item is determined. The data obtained
is summarized through use of statistics and these statistics are plotted on
control chart.
• A control chart consists of :-
Central line : it reflects the level around which plotted statistics are expected to
vary.
Warning Limits : it reflect that increased attention to be paid to the process when
the point of observations fall outside the warning limit but inside the control
limits.
Control Limits/ Action Limits: these are placed on both side of the central line
defining the band within which the statistic can be expected to lie randomly when
process is in control.

WWW.SIGMATEST.ORG
Theoretical
Theoreticalbasis
basisof
ofcontrol
controlchart
chart

WWW.SIGMATEST.ORG
Benefits of using control
charts
• A very powerful tool for internal quality control
• Changes in the quality of analysis can be detected very rapidly
• Easier to demonstrate ones quality and proficiency to clients and
auditors.
• Indicate if the process is stable or not
• Estimate the magnitude of the inherent variability of the process.
• Identify, investigate and reduce the effect of special causes of
variability.
• Identification of patterns of variability such as trends, cycle, runs
etc.
• Assist in the assessment of the performance of a measurement
system.

WWW.SIGMATEST.ORG
 Types of control charts
CONTROL CHARTS

PROCESS PROCESS
STABILITY ACCEPTANCE

Shewhart and related Acceptance control

control charts charts

Control charts with no

pre-defined control Control charts with
limits. specified control limits

WWW.SIGMATEST.ORG
 Shewhart control chart: Control chart with shewhart control
limits intended to distinguish between variation in a plotted
measure due to random causes and that due to special causes.
It is a graph of the values of a given subgroup characteristic
versus the subgroup number.
The control limits used are 3-sigma control limits.
Control charts with no pre specified control limits : It is used
to detect any lack of control in R&D stages, or in earlier pilot trials
or initial studies.
Control charts with pre specified control limits : it is based on
adopted standard values applicable to statistical measures plotted
on the chart. The standard values are based on:
a) Prior representative data.
b) Desired target value defined in specification.
c) An economic value derived from consideration of needs of
service and cost of production.
 Acceptance control chart: Control charts intended to evaluate
whether or not the plotted measure can be expected to satisfy
specified tolerance. WWW.SIGMATEST.ORG
Shewhart Control
chart

WWW.SIGMATEST.ORG
 Types of Shewhart control
charts
Average and range chart
or standard deviation
chart

Variables
Charts for individuals
Control
and moving range
Chart

Shewhart Median and Range Chart

control
chart
Fraction nonconforming
chart (p) or number of
non-conforming units
Attributes (np) chart
Control
Chart Number of
nonconformities chart
(c) or non conformities
per unit (u) chart

WWW.SIGMATEST.ORG
Variable Control Chart
Control charts for variables is a means of
visualizing the variations that occurred in the
central tendency and mean of a set of observation.
Benefits:-
• Most of the process have the output characteristic
that are measurable. So applicability is broad.
• The measurement value contains more information.
• The performance of the process can be analysed
without regard to the specification.
• The subgroup size of variables are much smaller
than that of attribute charts so are more efficient.

WWW.SIGMATEST.ORG
 Control limit formulae for
shewhart variables control charts
STATISTIC NO STANDARD VALUES STANDARD VALUES
GIVEN GIVEN

CENTRAL UCL AND LCL CENTRAL UCL AND LCL

LINE LINE

X X xxx ± A2R or xxx ± Xo or µ X0 ± Aσ0

A3s

R R D3R , D4R R0 or d2σ0 D1σ0 , D2σ0

s s B3s , B4s s0 or d4σ0 B5σ0 , B6σ0

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
Mean charts
○This type of chart graphs the means
(or averages) of a set of samples,
plotted in order to monitor the mean of
a variable.
oMainly for precision check

1. This graph shows changes in process and is

affected by changes in process variability.

2. It shows erratic and cyclic shifts in the

process.

3. It can also detect steady process changes

WWW.SIGMATEST.ORG
 RANGE CHARTS (R-CHART)

• An R-chart is a type of control chart used to monitor the

process variability (as the range) when measuring small
subgroups (n ≤ 10) at regular intervals from a process.

• It is important for repeatability precision check.

• For better understanding of the trend and variation in

the process -R charts are used together.

WWW.SIGMATEST.ORG
 -RANGE CONTROL CHARTS

• CASE -1: No standard values given.

Table 1 shows measurement of outside radius of a
plug. Four measurements are taken every half an
hour for a total of 20 samples. And the specified
tolerance are 0.219 dm and 0.125 dm.

WWW.SIGMATEST.ORG
Subgroup No. Radius Mean Range
(R)
X1 X2 X3 X4

1 0.1898 0.1729 0.2067 0.1898 0.1898 0.0338

2 0.2012 0.1913 0.1878 0.1921 0.1931 0.0134
3 0.2217 0.2192 0.2078 0.1980 0.2117 0.0237
4 0.1832 0.1812 0.1963 0.1800 0.1852 0.0163
5 0.1692 0.2263 0.2066 0.2091 0.2028 0.0571
6 0.1621 0.1832 0.1914 0.1783 0.1788 0.0293
7 0.2001 0.1927 0.2169 0.2082 0.2045 0.0242
8 0.2401 0.1825 0.1910 0.2264 0.2100 0.0576
9 0.1996 0.1980 0.2076 0.2023 0.2019 0.0096
10 0.1783 0.1715 0.1829 0.1961 0.1822 0.0246
11 0.2166 0.1748 0.1960 0.1923 0.1949 0.0418
12 0.1924 0.1984 0.2377 0.2003 0.2072 0.0453
13 0.1768 0.1986 0.2241 0.2022 0.2004 0.0473
14 0.1923 0.1876 0.1903 0.1986 0.1922 0.0110
15 0.1924 0.1996 0.2120 0.2160 0.2050 0.0236
16 0.1720 0.1940 0.2116 0.2320 0.2024 0.0600
17 0.1824 0.1790 0.1876 0.1821 0.1828 0.0086
18 0.1812 0.1585 0.1699 0.1680 0.1694 0.0227
19 0.1700 0.1667 0.1694 0.1702 0.1691 0.0035
20 0.1698 0.1664 0.1700 0.1600 0.1666 0.0100

WWW.SIGMATEST.ORG
R-Chart

Central line R 0.0287

UCL D4R 2.282 x 0.0287= 0.0655

LCL D3R 0 X 0.0287 =0 (since n< 7)

X-chart

Central line X 0.1924

UCL X + A2R 0.1924 +(0.729 x 0.0287)

=0.2133
LCL X-A2R 0.1924 - (0.729 x 0.0287)
=0.1715

WWW.SIGMATEST.ORG
AVERAG E
0.2200
0.2150 UCL
0.2100
0.2050
0.2000
0.1950
0.1900
0.1850
0.1800
0.1750
0.1700
0.1650 LCL
0.1600
0 2 4 6 8 10 12 14 16 18 20

SUBGROUP NUMBER
RANGE

0.0650
0.0600
0.0550 UCL
0.0500
0.0450
0.0400
0.0350
0.0300
0.0250
0.0200
0.0150
0.0100
0.0050
0.0000
0 2 4 6 8 10 12 14 16 18 20

SUBGROUP NUMBER

WWW.SIGMATEST.ORG
• On examination the chart reveal
that last three points are out of control
and it indicate that some cause of
variation may be operating.

• At this point remedial action is

required and charting is continued by
establishing revised control limits by
discarding the out of control points.

WWW.SIGMATEST.ORG
• Revised control limits
Revised X = ∑ X /k = 3.3454/17= 0.1968

Revised R= ∑ R /k = 0.5272/17= 0.0310

R-Chart
Central line R 0.0310
UCL D4R 2.282 x 0.0310= 0.0707

LCL D3R 0 X 0.0287 =0 (since n< 7)

X-chart
Central line X 0.1968
UCL X + A2R 0.1968 +(0.729 x 0.0310)
=0.2194
LCL X-A2R 0.1968 - (0.729 x 0.0310)
=0.1742

WWW.SIGMATEST.ORG
Averag
0.22

0.21

0.2

0.19

0.18

0.17

0.16
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Subgroup
Range

0.07

0.06

0.05

0.04

0.03

0.02

0.01

0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

Subgroup number

WWW.SIGMATEST.ORG
• CASE 2 -: Standard values given.

The tea importer wants to control his

packaging process such that the mean weight
of packages is 100.6 g and based on previous
packaging processes the standard deviation is
1.4g.
Table 2 shows the subgroup average and
subgroup average of 25 samples of size 5.

WWW.SIGMATEST.ORG
Subgroup No. Subgroup Subgroup Range
average
1 100.6 3.4
2 101.3 4.0
3 99.6 2.2
4 100.5 4.5
5 99.9 4.8
6 99.5 3.8
7 100.4 4.1
8 100.5 1.7
9 101.1 2.2
10 100.3 4.6
11 100.1 5.0
12 99.6 6.1
13 99.2 3.5
14 99.4 5.1
15 99.4 4.5
16 99.6 4.1
17 99.3 4.7
18 99.9 5.0
19 100.5 3.9
20 99.5 4.7
21 100.1 4.6
22 100.4 4.4
23 101.1 4.9
24 99.9 4.7
25 99.7 3.4

WWW.SIGMATEST.ORG
R-Chart

Central line d 2σ0 2.326 X 1.4 = 3.3 g

UCL D2σ0 4.918 x 1.4 = 6.9 g

LCL D1σ0 0 X 1.4 =0 (since n< 7)

X-chart

Central line X 100.6

UCL X + Aσ0 100.6 +(1.342 x 1.4)

=102.5

LCL X - Aσ0 100.6 - (1.342 x 1.4)

=98.7

WWW.SIGMATEST.ORG
Averag

103

102.5

102

101.5

101

100.5

100

99.5

99

98.5

98
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28

Subgroup
Range

0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28

Subgroup

WWW.SIGMATEST.ORG
Control charts for
individuals, X and moving
range R
• Control charts for individuals are plotted
when there is no rational subgroup possible
to provide inter batch variability or when cost
required for measurement is high so that
repeated observations are not possible.
• Moving range is the absolute difference
between successive pair of measurements in
a series.

WWW.SIGMATEST.ORG
Moving Ranges, R

Central line R

UCL D4R

LCL D3R

Individuals, X

Central line X

UCL X + E2R

LCL X - E2R

WWW.SIGMATEST.ORG
• Cautions while preparing moving range charts:-

a) This chart is not sensitive to process change as mean

and range chart.
b) Care should be taken in interpretation if the process
distribution is not normal
c) This chart does not isolate piece-to-piece repeatability
of a process.

WWW.SIGMATEST.ORG
 • Case study :-
The table shows the result of laboratory
analysis of % moisture samples of 10
successive lots of skim milk powder. As the
sampling variation is negligible, so it was
decided to take only one observation per lot.

Lot No. 1 2 3 4 5 6 7 8 9 10
X:%
moisture
2.9 3.2 3.6 4.3 3.8 3.5 3.0 3.1 3.6 3.5
R: Moving
Range
0.3 0.4 0.7 0.5 0.3 0.5 0.1 0.5 0.1

WWW.SIGMATEST.ORG
Moving Ranges, R

Central line R 0.38

UCL D4R 3.267 x 0.38 = 1.24

LCL D3R 0 x 0.38 = 0

Individuals, X

Central line X 3.45

UCL X + E2R 3.45 + (2.66 x 0.38) =

4.46

LCL X - E2R 3.45 - (2.66 x 0.38) =

2.44

WWW.SIGMATEST.ORG
% Moistur 5
4.8
4.6
4.4
4.2
4
3.8
3.6
3.4
3.2
3
2.8
2.6
2.4
2.2
2
0 2 4 6 8 10 12

Lot Number
M oving Range

1.4

1.2

0.8

0.6

0.4

0.2

0
0 2 4 6 8 10 12
-0.2

Lot Number

WWW.SIGMATEST.ORG
RECOVERY CONTROL CHARTS

• These are charts created using a blank matrix

that has been spiked with a known
concentration of analyte.
• We chart the percent recovery of the spike.
As long as the results fall within specified
criteria, the QC passes.
• A typical acceptance for matrix spikes is 70 –
120%, but for large screens with many
analytes, often 50 – 150% is acceptable

WWW.SIGMATEST.ORG
  The following data were obtained for the repetitive spike recoveries of
field samples.

Sample % recovery Sample % recovery Sample % recovery

1 94.6 8 96.2 15 101.5

2 93.1 9 73.8 16 74.6

3 100.0 10 104.6 17 108.5

4 122.3 11 123.8 18 104.6

5 120.8 12 93.8 19 91.5

6 93.1 13 80.0 20 83.1

7 117.7 14 99.2 21 100.8

WWW.SIGMATEST.ORG
% Recovery

150

140

130

120

110

100

90

80

70

60

50
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22

Subgroup No.

WWW.SIGMATEST.ORG
 CONTROL CHART FOR DUPLICATE
SAMPLES
• An effective method for determining the precision
of an analysis is to analyze duplicate samples.
• Duplicate samples are obtained by dividing a
single gross sample into two parts
• We report the results for the duplicate samples,
X1 and X2, by determining the standard deviation
and relative standard deviation, between the two
samples

WWW.SIGMATEST.ORG
ILLUSTRATION
Consider the following analysis data of duplicate samples
Months Measurements Mean Std . Dev. %CV
Y1 Y2
1 10.22 10.9 10.56

0.481 4.55
2 10.25 10.37 10.31

0.085 0.82
3 10.27 11.05 10.66

0.552 5.17
4 10.35 9.28 9.815

0.757 7.71
5 10.28 11.08 10.68

0.566 5.30
6 10.36 10.23 10.30

0.092 0.89
Grand Average
10.39 0.422 4.07
WWW.SIGMATEST.ORG
Determination of central line and control limits.
Central line = Std. Dev ( s )/Grand Average { X }*100
Upper control limit (UCL)= (UCL)s/ X *100
(UCL)s = B4 s
Lower control limit (LCL)= (LCL)s/ X *100
(LCL)s = B3 s
Here, B4 is the function of number of observation in
subgroup. (n)
Here, n=2 so from table B4 =3.267
Central line 4.07

Upper Control Limit 13.27

WWW.SIGMATEST.ORG
 15.00
14.50
14.00
13.50
13.00
UCL
12.50
12.00
11.50
11.00
10.50
10.00
9.50
9.00
8.50
8.00
%CV

7.50
7.00
6.50
6.00
5.50
5.00
4.50
4.00 CL
3.50
3.00
2.50
2.00
1.50
1.00
0.50
0.00
1 2 3 4 5 6

Months
WWW.SIGMATEST.ORG
APPLICATIONS IN
TESTING
LABORATORY

WWW.SIGMATEST.ORG
• Estimation of Measurement Uncertainty.
Results from the control charts can, together with other data be used
for calculating the measurement uncertainty, it may give a realistic
estimate of the measurement uncertainty.

• Method Validation /Verification

When the method has been changed only slightly, or if a standard
method is adopted in the laboratory, control charts can be used to
complement that the process is still under control.

• Performance of equipment.
Equipment control charts can be drawn to monitor the bias, changes
due to ageing, wear, drift & noise.

WWW.SIGMATEST.ORG
Method Comparison
By plotting control charts for two methods in parallel, it is easy to compare
important information:
• spread (from the standard deviation or from the range)
• bias (if a CRM is used)
• matrix effects (interferences), if spiking or a matrix CRM is used
• robustness, i.e. if one method is more sensitive to temperature shifts,
handling etc.

• Method Blank and Reagent blank Monitoring.

The control chart drawn for matrix blank/reagent blank can help to
monitor the contamination occurring in a process due to cross
contamination, gradual build-up of the contaminant, procedure failure or
instrument instability.

WWW.SIGMATEST.ORG
• Person comparison or qualification
Control charts are helpful in comparing the performance of different
persons in the laboratory. control charts can be employed during
training and qualifying new staff in the laboratory. It is a powerful tool
to estimate inter-analyst variation.

• Environmental parameters checks.

The control charts give a very simple graphical presentation of any
trends or unexpected variation that might influence the analyses.

• Control charts can also help to identify the effect of matrix on the
recovery of the analyte.

WWW.SIGMATEST.ORG
PROCESS
CONTROL

WWW.SIGMATEST.ORG
 WESTGARD RULES
• Westgard Rules are multirule QC rules to help analyze
whether or not an analytical run is in-control or out-of-
control.
• It uses a combination of decision criteria, usually 5 different
control rules to judge the acceptability of an analytical run.
• The advantages of multirule QC procedures are that false
rejection can be kept low while at the same time
maintaining high error detection. This is done by selecting
individual rules that have very low levels of false rejection,
then building up the error detection by using these rules
together

WWW.SIGMATEST.ORG
• Rule 1-2s
Definition: The 1-2s Control Rule indicates one control result has
exceeded the established mean +/- 2SD range. This is a “warning rule,”
which does not indicate an “out-of-control” condition, but is intended
to initiate further testing.
Interpretation: If no other control rule is violated, then the warning
is attributed to normal random error. Patient results are acceptable.
Corrective Action: No corrective action is required. However, the
“warning” suggests a system error may be in the development. A
comprehensive check of the routine maintenance schedule and
review of the quality control & handling and sampling technique is
recommended.

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule 1-3s
Definition: The 1-3s Control Rule indicates one control result has exceeded the
established mean +/- 3SD range. This is a “rejection rule,” which is sensitive to random
error.
Interpretation: Excessive random error exists. The analyzer is “out-of-control.” The
results are not acceptable and should be re-analyzed after corrective actions have solved
the problem.
Corrective Action: Rerun the quality control level that is in question, emphasizing proper
technique. If the repeated level is within +/- 2SD range then the problem can be
attributed to random error. If the repeated level exceeds the +/- 2SD range, then further
corrective action should be conducted. The following are probable causes:
• Inadequate or wrong +/- 2SD range.
• Improper storage temperature correction of quality control results.
• Improper technique when handling the quality control. Change of quality control
batch.
• Inadequate maintenance of the instrument.

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule 2-2s
Definition: The 2-2s Control Rule indicates that two consecutive control results have
exceeded the same mean +/- 2SD limit. This is a “rejection rule,” which is sensitive to
systematic errors.
Interpretation: A systematic error exists. The analyzer is “out-of-control.” This may be an
early indicator for a “shift” in the mean value. Patient results are not acceptable and should
be re-analyzed after corrective action has solved the problem.
Corrective Action: To resolve systematic errors, corrective action should be conducted to
address the following probable causes:
• Inadequate or wrong +/- 2SD range.
• Improper technique when handling the quality control.
• Improper storage temperature correction of the quality control results.
• Change of the quality control batch.
• Inadequate maintenance of the instrument.

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule R-4s

Definition: The R-4s Control Rule indicates that one result has
exceeded the mean - 2SD limit and the adjacent result has
exceeded the mean + 2SD limit. This is a “rejection rule,” which is
sensitive to random error.
Interpretation: Excessive random error exists. The analyzer is “out-
of-control.” The results are not acceptable and should be re-
analyzed after corrective action has solved the problem.
Corrective Action: As per Rule 1-3s

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule 4-1s

Definition: The 4-1s Control Rule indicates four consecutive

control results have exceeded the same mean +/- 1SD limit. This
is a “rejection rule,” which is sensitive to systematic errors.
Interpretation: A systematic error exists. The analyzer is “out-of-
control.” This may be an early indicator for a “shift” in the mean
value. The results are not acceptable and should be re-analyzed
after corrective action has solved the problem.
Corrective Action: As per Rule 2-2s.

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule 8-x,9-x,10-x,12-x

Definition: These Control Rule indicates eight, nine, ten or

twelve consecutive control results have fallen on the same side
of the mean. This is a “rejection rule,” which is sensitive to
systematic errors.

Interpretation: A systematic error exists. The analyzer is “out-of-

control.” The results are not acceptable and should be re-
analyzed after corrective action has solved the problem.

Corrective Action: As per Rule 2-2s.

WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
WWW.SIGMATEST.ORG
• Rule 7-t
Definition: reject when seven control measurements trend in the same
direction, i.e., get progressively higher or progressively lower.
Interpretation: More than one process present (e.g. shifts, machines, raw
materials)

WWW.SIGMATEST.ORG
• 2 of 32s
Definition: reject when 2 out of 3 control measurements
exceed the same mean plus 2s or mean minus 2s control limit.
Interpretation: represent sudden, large shifts from the
average. These are often fleeting – a one-time occurrence of a
special cause.

WWW.SIGMATEST.ORG
 Control Data

In-control  Report Results

12s
No

Yes no

no no no no
13s 22s R4s 41s 10x

yes yes yes yes yes

Out-of-control, Reject analytical run

WWW.SIGMATEST.ORG
Illustration of rules

WWW.SIGMATEST.ORG
Day 21, 22, 24, 26, 27, 30, 31, 33, 34, 36-44 – in
control

Day 23, 28, 29 – 12s

Day 25 - 13s
Day 32 – 22s
Day 35 - R4s

WWW.SIGMATEST.ORG
 REFERENCES

• ASTM manual on presentation of data and control

chart analysis.
• FAO: Internal Quality Control Of Data
http://www.fao.org/docrep/w7295e/w7295e0a.ht
m

WWW.SIGMATEST.ORG
Thank you!

WWW.SIGMATEST.ORG