ANALYZER

PERFORMANCE

MONITORING

By
M.S.Mani
N.A.Baxi
H.Madhvani
J.F.D’Souza
V.R.Patel
1
 Objective
• To understand the need of Analyzer
Performance Monitoring

• To understand common terms associated

with Analyzer Performance Monitoring

• To understand Control charts

• How to prepare Control charts.

2
 Introduction
• The present era is the era of global trade, where goods are crossing
national boundaries. The quality of these goods rely on quality of
measurements carried out at different stages.

• On line Analyzers have been developed and applied to measure

continuously the quality of material within or drawn directly from the
flowing line. The benefits are as follows:
– Reduced sampling
– Reduced testing time & effort / / lab load
– Continuous on line monitoring of quality
– Improved precision
– The opportunity for automatic control of quality

• An analyzer differs from the standard test apparatus and even the basic
measurement technique may be different. Thus the analyzer and the
standard test should give identical results, provided that due account is
taken of any difference in the precision of the two methods. 3
Why Analyzer Performance Monitoring ?

• Once an analyzer is in routine service, its performance

must be monitored to confirm its continuing satisfactory
operation and detect any drift from initial calibration.

• Some record of regular checks on the performance of an

analyzer are not only of value for maintenance planning
but also for continual performance assurance .

• Performance monitoring for identification of drift well

before spec violation and execution of corrective action
and recorded procedure and proof of same can ensure
customer satisfaction and ultimately the goal of release
of product under “QMI Release” can be achieved.
4
 Terms to know
• Measurement
A set of operations having object of determining the value of a given quantity.

• True value
The value which characterizes a perfectly defined quantity in the condition which
exists when that quantity is considered.

• Measurement uncertainty
It is an estimate characterizing the range of values within which the error is
asserted to lie.
It is an expression of the fact that, for a given result of measurement there is not
one value, but an infinite number of values dispersed about the result with a
varying degree of credibility.

• Accuracy
Accuracy describes the nearness of a measurement to the standard or true
value, i.e., a highly accurate measuring device will provide measurements very
close to the standard, true or known values.

• Precision
Precision is the degree to which several measurements provide answers very
close to each other. It is an indicator of the scatter in the data. The lesser the
5
scatter, higher the precision.
 Terms to know
 Bias
A consistent difference (either on positive side or negative side) between the
actual value and the measured value is called the bias or offset.

 Confidence level
The probability expressed as a decimal or percentage that the true value lies
within a specified range of values.

 Accepted Reference Value

An agreed upon value directly or indirectly derived from the accepted reference
method, which can be:
–A theoretical or established value
–An assigned value based on work of standard bodies.
–A consensus value, based on collaborative experimental work.

• Availability Rate
It is the percentage of the time during which the instrument is functioning
correctly during actual operation of the plant.
.

6
 Terms to know
EXAMPLE Accuracy Vs Precision:

If we measure the length of a foot-ruler and get

values of

12.01 in, 12.00 in, 11.99 in, 12.00 in.

These numbers are precise enough for us to

believe that if we measure it again we would get
12.00±0.01 in. These measurements are precise
but not necessarily accurate.
7
Difference between Accuracy & Precision

Accurate but not Precise Precise but not Accurate- Biased

Accurate and Precise

8
 Terms to know
 Repeatability
Closeness of agreement between independent test result obtained
on identical material in a short interval of time, by the same
operator using the same instrument in the same laboratory. The
difference between two successive results that would be exceeded
in the long run in only 1 case in 20 ( 95% confidence level) when the
analyzer is operating normally.

 Reproducibility
Closeness of agreement between independent test result obtained
on identical material, by different operators using different
instruments in different laboratories. The difference between two
successive results that would be exceeded in the long run in only 1
case in 20 ( 95% confidence level) when the analyzer is operating
normally.

9
 General Terms
• Variance
The expectation of the
deviation of a random
variable about its
expectation

10
 Calibration / Validation
 Calibration
It is adjusting the analyzer output to agree with a
standard introduced into the analyzer.

 Validation
It is observing and noting the difference ( if any )
between the analyzer reading and the reference
standard / sample used. But with no adjustments made
to the analyzer. When a difference is recorded , random
statistical error can be estimated and accurate
adjustments made. This avoids the practice of too
frequent adjustments in an attempt to tune out normal
system fluctuations.
11
 Calibration/ Validation methods
Reference sample method
 Samples which have been accurately prepared, tested and certified [ as
per well laid standards ] is used for calibration.

 This is the preferred method.

Paired/ Line sample method

 This method is applicable only when Reference sample method is not
feasible.

 Analyzer results are checked against a representative grab sample taken

from a stable process at that instant and analyzed by the laboratory in
accordance with the relevant standard test methods.

 The analyzer results must be constant, time stamped including delays of

the analyzer system and other conditions shall be taken into
consideration in order to ensure that for both results, the same process
conditions are valid

12
 Validation of analyzers

• Validation of an on-line analyzer is the checking

procedure in order to establish whether or not the
analyser results are within defined accuracy limits.

• Evaluation of the validation data gives valuable

information about the short and long-term performance
of the analyser, on basis of which preventive
maintenance cycle can be planned.

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 Validation planning for analyzers
• Periodic validation of the analyser running, on-line, with
process sample. The validation frequency shall be in
accordance with the Validation frequency flow-chart

• Compulsory validation when the analyser is brought

back on stream after trouble-shooting and/or
maintenance.

• Validation in cases that considerable deviation from the

normal conditioning and/or analyser conditions have
been observed, which could lead to erroneous analyser
result(s).

14
 Frequency of validation
• The frequency of validation will depend upon many
factors such as

– Application
– Type of analyzer
– The precision required
– Whether checking will be at regular intervals
or related to parcel transfers

• However the general guideline is given by the flow chart

15
 Start
Commissioning

Validation frequency Trouble shoot Consult Vendor

1 x per day Take corrective actions Vendor to troubleshoot
Record the action points Record the action points
Y
1 week
(or sooner) N
Performance
More corrective
Ok ? N
Actions required;
No solution
Y

Validation frequency
2 per week / 1 per week Y Trouble shoot
Take corrective actions
Record the action points
1 month
(Or sooner) N
Performance
Ok ?
Major
N corrective
Y
Actions required
Validation frequency
2 per month / 1 per month

A B C 16
 A B C

Trouble shoot
Take corrective actions
Record the action points

6 months N
Performance
Ok ? Y

Major
Y corrective
N
Actions required
Validation frequency
1 / month
1 / 2 months Trouble shoot
a & b as required Take corrective actions
Record the action points

Y Performance N
Ok ?

17
 Performance monitoring

• Calibration or validation are instantaneous verification

• Calibration or validation are normally single / dual point

• Performance monitoring helps in monitoring and

establishing behaviour of the analyser over a time period
and helps in establishing optimum :
-- PM frequency of the Analyzer system
-- Calibration / validation frequency

• Comparison of the analyser results with lab results is

fraught with own dangers
18
 How Online QMI Differ From Lab QMI
Type On-line Analysers
Process Continuous variation in process conditions
Process upsets during real time analysis
Sampling Application built Sample conditioning system
Sampling point from Sample conditioning system
Sample transportation and Handling fixed
Sample measured by QMI is representative of the actual Manual sampling has inherent sampling errors such as
process sample
Analyser type Difference in Analyser H/W & detection element
Ranges
Continuous reading
Direct reading
Correlates to ASTM stds
( standard gases, simulation method , optical method )
Other factors No human interference
Operator Bias Nil
Dedicated Instrument for dedicated stream to analise
Appartus Bias predetermined parameter
Laborotary Analysers
No response to process variation
Different sample preperation method in Lab
Sample collection point may be different
varies
a). Inadequate sample container purge
b). Evaporation of lighters
c). Removal of separable water from the sample prior
to analysis
Not identical H/W
Not identical ranges
discrete sampling -- n times / day
Normalisation / avraging may be carried out
Follows ASTM standard
Not unique
Operator interference
The result can very from Lab Technician to Technician
19
Different samples from the same stream may be analysed of
diofferent identical instruments
 Why Control Charts ?
• Every process varies. If you write your name ten times, your signatures
will all be similar, but no two signatures will be exactly alike. There is
an inherent variation, but it varies between predictable limits. If, as you
are signing your name, someone bumps your elbow, you get an
unusual variation due to what is called a "special cause". If you are
cutting diamonds, and someone bumps your elbow, the special cause
can be expensive. For many, many processes, it is important to notice
special causes of variation as soon as they occur.

• Variations due to special causes are

– localized in nature
– exceptions to the system
– considered abnormalities
– often specific to a
• certain operator
• certain machine
• certain batch of material, etc.
• Investigation and removal of variations due to special causes are key
to process improvement
20
 Why Control Charts ?
• There's also "common cause" variation. Consider a baseball pitcher. If
he has good control, most of his pitches are going to be where he wants
them. There will be some variation, but not too much. If he is "wild", his
pitches aren't going where he wants them; there's more variation. There
may not be any special causes - no wind, no change in the ball - just
more "common cause" variation. The result: more walks are issued, and
there are unintended fat pitches out over the plate where batters can hit
them. In baseball, control wins ballgames. Likewise, in most processes,
reducing common cause variation saves money.

Variations due to common causes :

• are inherent to the process because of:
– the nature of the system
– the way the system is managed
– the way the process is organized and operated
• can only be removed by
– making modifications to the process
– changing the process .
21
 Why Control Charts ?
• The point of making control charts is to look at variation,
seeking special causes and tracking common causes.
Special causes can be spotted using several tests:
– 1 data point falling outside the control limits
– 6 or more points in a row steadily increasing or
decreasing
– 8 or more points in a row on one side of the centerline
– 14 or more points alternating up and down

• The control chart provides a convenient , simple and

visual means for recording analyzer error and for
deciding what action ( if any ) is necessary.

22
 What Are Control Charts
• Happily, there are easy-to-use charts
which make it easy see both special
and common cause variation in a
process. They are called Control
charts, or sometimes Shewhart
charts, after their inventor, Walter
Shewhart, of Bell Labs

• All control charts have three basic

components:
– a centerline, usually the
mathematical average of all the
samples plotted.
– upper and lower statistical control
limits that define the constraints of
common cause variations.
– performance data plotted over
time.
23
 What Are Control Charts
• Control limits on a control chart are commonly drawn at 3sigma from
the center line because 3-sigma limits are a good balance point
between two types of errors:

– Type I or alpha errors occur when a point falls outside the control limits
even though no special cause is operating. The result is a witch-hunt for
special causes and adjustment of things here and there. The tampering
usually distorts a stable process as well as wasting time and energy.
– Type II or beta errors occur when you miss a special cause because the
chart isn't sensitive enough to detect it. In this case, you will go along
unaware that the problem exists and thus unable to root it out.

• All process control is vulnerable to these two types of errors. The reason
that 3-sigma control limits balance the risk of error is that, for normally
distributed data, data points will fall inside 3-sigma limits 99.7% of the
time when a process is in control. This makes the witch hunts infrequent
but still makes it likely that unusual causes of variation will be detected.

24
 Setting up a Control-chart
• Before starting the use of the Control Chart ensure that
the analyser is running.

• Perform an initial calibration of the analyser in

accordance with the relevant calibration procedure.
The average of a number of analyser readings, by
analysing the reference sample, shall be equal to the
reference value. A proven systematic error should be
eliminated.

• For each control chart some analyser data, e.g.

Standard Deviation of the collected validation data,
Reproducibility of the standard test method, needs to
be collected and entered in the Control Chart sheet.

25
 Setting up a Control-chart
• Calculate the average of the results plus the Standard
Deviation of the obtained values during the validation
period

• The Warning and Control limits are calculated as

respectively 2 and 3 times the Standard Deviation.

• Enter these calculated values, together with the

Reference Value and the Reproducibility R of the
relevant Laboratory standard test method into the
Control Chart sheet.
26
 Setting up a Control-chart
• Calculate the deviation ( Analyser value – Reference
value ) for each validation result.

• Plot the deviation curve in the control chart based on

the obtained validation results. The datum point in all
cases is the reference value of the test sample. The
deviation of the corresponding analyser value above or
below this datum is the basis of action.

• Evaluate the validation results after each validation for

possible systematic errors and/or faults. A proper
operating analyser will show randomly spread results
around the Reference value.
27
 Decision Rules for corrective actions
a) Points fall at random around the aim line( zero line) and with in
the warning limits. Instrument performance is correct and no
action required.

b) Four successive points fall between the aim line and one warning
limit. Suspect a systematic error: Shorten test interval.

c) Six successive points fall between the end line and one warning
limit. Systematic error present; adjustment desirable.

d) Two successive points fall outside one warning limit. Systematic

error present; adjustment desirable.

e) Two successive points fall between warning & control limit on

different sides of the aim line OR one point falls outside a control
limit. Instrument out of order. Repair necessary..

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 a b c d e e
Deviation
+
Upper Control Limit

+
Upper warning Limit

+ +
+ + +
+ + +
+
Reference Value

+ +

Lower warning Limit

+
+ +
Lower Control Limit

Adjusted Adjusted Repaired 29

Tag no: 623AT101 ( HK ) Reproducibility:- ( ASTM D86 ) 5.3 deg C Warning limit:- 5.481281

Plant: Crude Standard Dev.: - 2.74064064 Control Limit:- 8.221922

Reading
Sr no Date Time Lab Analyser Deviation Control Chart
10
1 01/01/2002 8:00 276 277 1
8
2 01/07/2002 8:00 275 274 -1
6

3 14/1/02 8:00 280 279 -1 4

4 21/1/02 8:00 276 278 2 Deviation 2

5 28/1/02 8:00 274 276 2 0

01/01/2002 01/07/2002 14/1/02 21/1/02 28/1/02 02/05/2002 02/12/2002 19/2/02 27/2/02 03/07/2002
-2
6 02/05/2002 8:00 272 271 -1
-4
7 02/12/2002 8:00 275 274 -1
-6
8 19/2/02 8:00 280 278 -2
-8

9 27/2/02 8:00 277 277 0 -10

Date
10 03/07/2002 8:00 280 281 1 Deviation

AVG 276.5 276.5 30

Tag no: 623AT101 Reproducibility:- ( ASTM D86 ) 5.3 deg C Warning limit 5.481281

Plant: Crude Standard Dev.: 2.74 2.740640639 Control Limit 8.221922

Reading
Sr no Date Time Lab Analyser Deviation Control Chart
10
1 01/01/2002 8:00 276 277 1
8
2 01/07/2002 8:00 275 277 2
6

3 14/1/02 8:00 280 281 1 4

4 21/1/02 8:00 276 278 2 2

Deviation

0
5 28/1/02 8:00 274 275 1 01/01/2002 01/07/2002 14/1/02 21/1/02 28/1/02 02/05/2002 02/12/2002 19/2/02 27/2/02 03/07/2002
-2
6 02/05/2002 8:00 272 273 1
-4
7 02/12/2002 8:00 275 276 1
-6

8 19/2/02 8:00 280 281 1 -8

9 27/2/02 8:00 277 279 2 -10

Date
10 03/07/2002 8:00 280 281 1 Deviation

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 Case Study- Flashpoint Analyzer- Before Bias i/p
Date & Time IP21 Value LAB Delta
10/1/03 8:12 57.81 68 10.19
10/1/03 15:55 62.28 71 8.72
10/2/03 0:00 59.07 69 9.93
RTF FP trend
10/2/03 7:54 58.20 70 11.80
10/2/03 15:58 59.36 71 11.64 90.00
10/2/03 23:43 57.71 68 10.29
10/3/03 7:58 61.40 70 8.60 85.00
10/3/03 16:01 63.35 71 7.65
10/3/03 23:43 56.45 71 14.55
80.00
10/4/03 7:53 60.24 71 10.76
10/4/03 16:04 58.19 71 12.81
75.00
10/5/03 7:44 59.27 71 11.73
10/5/03 15:35 59.36 68 8.64
11.80 70.00
10/6/03 0:04 58.20 70
10/10/03 7:48 58.68 69 10.32
12/10/03 08.036 59.44 72 12.56 65.00
10/13/03 15:48 60.33 69 8.67
Online
FP

10/13/03 23:38 55.57 72 16.43 60.00

10/15/03 23:48 59.47 70 10.53 LAB
16/10/03 07:54 59.07 69 9.93 55.00
15/10/03 15:47 57.90 70 12.10
18/10/03 15:53 61.79 70 8.21 50.00
19/10/03 07:43 63.25 71 7.75
19/10/03 16:11 61.11 72 10.89 45.00
19/10/03 23:58 61.12 71 9.88
20/10/03 08:01 59.66 71 11.34
40.00
20/10/03 23:54 59.95 70 10.05
21/10/03 23:55 64.70 72 7.30
35.00
22/10/03 15:52 60.73 69 8.27
22/10/03 23:46 60.14 72 11.86
13.12 30.00
23/10/03 07:48 58.88 72
23/10/03 16:02 60.33 74 13.67
23/10/03 23:58 62.48 73 10.52
24/10/03 07:58 60.14 71 10.86
25/10/03 00:59 59.08 70 10.92
25/10/03 23:58 59.37 71 11.63 Date
26/10/03 15:47 59.36 70 10.64
26/10/03 23:55 59.85 70 10.15
MIN 7.3 32
MAX 16.4
MEAN 10.7
 Case Study- Flashpoint Analyzer- After Bias i/p
Comparision Nov 2-9
Sr no Date& Time Online Lab Delta
1 2/11/2003_12:00 AM 67.8 67 -0.8
2 2/11/2003_8:00 AM 67.1 67 -0.1 Lab Vs Online after offset
3 2/11/2003_4:00 PM 67.4 68 0.6
4 3/11/2003_12:00 AM 68 67 -1 90
5 3/11/2003_8:00 AM 68.8 70 1.2
6 3/11/2003_4:00 PM 69.7 68 -1.7 80
7 4/11/2003_12:00 AM 72.3 70 -2.3
8 4/11/2003_8:00 AM 74.5 75 0.5 70
9 4/11/2003_4:00 PM 73.7 77 3.3
10 5/11/2003_12:00 AM 73 76 3
Flashpoint 60 Online
11 5/11/2003_8:00 AM 73.2 76 2.8
12 5/11/2003_4:00 PM 73.1 74 0.9 Lab
13 6/11/2003_12:00 AM 72 76 4 50
14 6/11/2003_8:00 AM 71.6 75 3.4
15 6/11/2003_4:00 PM 73.9 75 1.1 40
16 7/11/2003_12:00 AM 72.2 75 2.8
17 7/11/2003_8:00 AM 73.1 72 -1.1
30
18 7/11/2003_4:00 PM 73.9 71 -2.9
19 8/11/2003_12:00 AM 71 69 -2
20 8/11/2003_8:00 AM 71 74 3
21 8/11/2003_4:00 PM 73.5 74 0.5
22 9/11/2003_12:00 AM 72.3 72 -0.3
23 9/11/2003_8:00 AM 72.2 73 0.8
24 9/11/2003_4:00 PM 73.6 73 -0.6
Average 71.62083 72.25 0.629167
Max 74.5 77 4 Date & Time
Min 67.1 67 -2.9
33
 Bibliography
• IP 340/82 – IP code of practice for calibrating and
checking process analyzers
• ASTM D 3764 – Standard practice for validation of
process stream analyzer systems
• Article:- Process analyzers in hydrocarbon industry; by
Hans Benke.
• Shell Presentations on QMI and Performance monitoring
procedures.
• Websites on Statistical Process Control & Six Sigma
• Presentation on Uncertainties in measurement - EQDC

34
Thank You

35