Laboratory Quality Control and Assurance: An Integrated Approach

9/21/2010
Learning Objectives
Gain integrated perspective of quality in the lab
Laboratory Quality environment.
Understand the application of key quality concepts
Control & Assurance and statistical tools in labs.
Learn critical quality control and quality assurance
Integrated Approach activities.
Understand difference between registration and
Dr. Tariq A. Aldowaisan accreditation in labs via ISO 9001 & ISO 17025
models.
Dr. Ashraf S. Youssef
Office of Consultation & Career Development

Aldowaisan & Youssef
Our Objective Training Approach

You Enjoy While You Learn Focus on Basics
Interactive
Case Studies
Games
Exercises
Computer
Fun !!!!!!!!!!!!!!!!!!
Aldowaisan & Youssef Aldowaisan & Youssef
Agenda – Day 1 Exercise: What is Quality?
1. Basic Quality 2. Statistical Overview

Concepts Descriptive Statistics
Quality Inferential Statistics
Quality Dimensions 3. Computer Applications
Q lit Control
Quality C t l
Quality Assurance
Quality Cycle
uality
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Quality Dimensions
Totality of Meaning of quality cannot be captured in a

characteristics
of an entity that bear simple short statement
on its ability to satisfy
stated and implied
needs
Let us define some dimensions of quality for
labs
uality Source: ISO 8402
Exercise: Quality Dimensions Exercise: Quality Violations

-- Lab Service Situation Violation
Mohamad and Sami performed the same standard
test but used different steps
The solution viscosity is not as per the specification
The lab supervisor called the client to tell him that
the results won’t be ready for pick up today as
promised
Lab
The client decided to do business with another lab;
Service
his one-month complaint is still unanswered!
The secretary didn’t show any regret when she told
me that my lab report won’t be ready on time.
The client insisted that his request included
Lab Customer additional tests to be performed on the sample
Key Quality Dimensions Accuracy & Precision

-- Lab Measurements
Precision
Accuracy Reliability ____________ ____________ ____________ ____________
Lab ____________ ____________ ____________ ____________

Meas.
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Quality Control (QC) Quality Assurance (QA)

All the planned and systematic activities
Operational techniques and activities used to implemented to provide adequate confidence that
monitor product realization processes and to product, service, process, persons, and organization
eliminate causes of unsatisfactory performance. will satisfy the specified requirements for quality
The monitoring, inspecting and auditing to

The tools an analyst uses to measure the accuracy assure that the work is documented and
and precision of the methods and procedures conducted according to protocol and laboratory
SOPs from the conception
of a test to the review of the final report
Quality Management System Quality Concepts Relationships

(QMS)
Is a system for managing quality: Preventive Scope QMS … Whole Laboratory
Leadership Resources
System: a set of logically related processes Business Results
that turn input into output. QA … Realization Cycle
Managing: administering activities and Protocols
Procedures
resources to achieve an objective. Responsibilities
Preventive Actions
Quality: customer/user satisfaction. QC … Result
Corrective Actions
Out-of-control
Input Process Output
Quality Cycle Statistical Overview
Population
A large No. of N
Plan Do
Mean = µ
Standard Deviation = σ
Sample
A small No. of n
Sample Mean = X
Sample Standard
Act Check Deviation = s
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Descriptive Statistics Exercise: Centrality Measures

Centrality Measures
Calculate the sample
¾ Mode
mode, median and the
¾ Median
mean of the following
¾ Mean
data set
set.
Dispersion Measures
¾ Range Set A: 20, 20, 18, 17,
15, 17, 14, 17, 12, 10
¾ Variance
¾ Standard Deviation Set B: 10, 20, 12, 13, 13,
¾ Coefficient of Variation 16, 17, 12, 13, 17, 22
Exercise: Dispersion Measures Exercise: Descriptive Measures

Sample Percents
Calculate the sample The following Isooctane
range, variance, measurements were 1 3.83
obtained for the 2 3.94
standard deviation and
analysis of isooctane 3 3.88
coefficient of variation
variation. in gasoline. 4 3.97
5 3.90
Set A: 20, 20, 18, 17,
6 3.94
15, 17, 14, 17, 12, 10
Set B: 10, 20, 12, 13, 13, • Calculate X , S, and the C.V
16, 17, 12, 13, 17, 22
Estimate of Standard Deviation from Estimate of Standard Deviation from

a Pair of Results (X1 and X2) Duplicate Measurements
In case of a single duplicate pair of For a set of measurements consisting of pairs of
measurements, the equation for the standard duplicate results, the standard deviation can be
deviation can be significantly reduced as follows estimated as follows:
S=
D X − X2
= 1 S=
∑D 2
n 2 2k
Where K = the number of sets of
duplicates
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Combining (Pooling) Estimates of Exercise: Duplicates & Pooling

Standard Deviations
Sample Percents Percents
The following pairs of Isooctane Isooctane
It is possible to pool (combine) several estimates duplicate results were
of standard deviation using the following obtained for the
1 3.81 3.83
equation: analysis of isooctane

2 3.88 3.94
3 3.85 3.88
in gasoline.
∑ν S 2 4 3.97 3.89
Sp = i i
∑ν i
• Calculate S, and Sp
Where vi = the number of sets of
duplicates
Hypothesis Testing Test 1: Comparing the Mean With

the True Value
Common questions that can be answered using The largest difference that could be expected
the null hypothesis approach: as a result of indeterminate error is given by:
s
¾ Is the mean of the data set significantly different from ± t( )
the true value?
n
¾ Are the means of two different sets significantly
different? −
H o : ( X − μ ) p± t (
s
)
¾ Are the precisions of two different data sets n
significantly different? − s
H1 : ( X − μ ) f ± t ( )
n
Test 2: Comparing Two Means Exercise: Comparing Two

Means
There are two occasions when we wish to Compare the two
determine if two independently obtained results
means, of the following
are essentially the same.
− − n1 + n 2 data set.
H o : ( X 1 − X 2 ) p ± ts p
n1 n 2 Set A: 20, 20, 18, 17,
− − n1 + n 2 15, 17, 14, 17, 12, 10
H 1 : ( X 1 − X 2 ) f ± ts p
n1 n 2
Set B: 10, 20, 12, 13, 13,
Where Sp is the pooled standard deviation of the two samples. 16, 17, 12, 13, 17, 22
(n1 − 1) S 1 + (n2 − 1) S 2
2 2
Sp =
n1 + n2 − 2
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Test 3: Comparing Two Exercise: Comparing Two

Precisions Precisions
To determine if the standard deviation from A ship of copper ore was purchased by a
one data set is significantly different from the local metal refiner. The analysis certificate
standard deviation of another data set made out while the ship was being loaded,
show that %Cu =14.66 with a standard
H o : Fc p Ft deviation of 0.07%
0 07% for 5 measurements.
measurements
H 1 : Fc f Ft When the ore arrived at the refinery, it was
2 analyzed and the following results were
Fc =
Var1
= S 1
obtained: %Cu = 14.58, 14.61, 14.69,
2
Var 2 S 2 14.69, and 14.64. Should the refiner accept
•The larger variance is always numerator.
the ore?
•Ft is the expected tolerance base on Normal distribution.
Regression Analysis Method of Least Square

Regression Analysis is a technique used for
Y
obtaining the “best” line from a set of data, and
for specifying the uncertainties of that line.
Th simplest
The i l t regressioni analysis
l i ffor a straight
t i ht
a
line is called the least squares method of.
X
Where: a is the intercept (Value of y when X=0)

b is the slope of the line
Exercise: Regression Analysis Computer

The following calibration data, assuming
a linear relationship exists and the Application
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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Agenda – Day 2 Lab Results Realization Cycle

What could go wrong?
1. Laboratory Results Realization Cycle
2. Sampling and Items Handling
3. Measurement
4. Equipment
q p
Receive Prepare Perform Analyze Prepare Give
5. Calibration
Order Sample Test Results Report Report
6. Lab Conditions & Safety
7. Personnel
8. Computer Applications
LRRC & QA LRRC & QA Program

Personnel
Lab Conditions Receive Prepare Perform Analyze Prepare Give
Supplies Order Sample Test Results Report Report
Equipment & Maintenance During Testing

Safety
Sample Handling Sample Analysis
Choice of Method
Before Testing Control Charts
Other Statistical Applications
LRRC & QA Program QC, QA & QMS Requirements

Evaluation & CA
Before Testing
MANAGEMENT
QA
D i
During T
Testing
ti QMS
QC
Accuracy Checks
Results Monitoring
TECHNICAL
System & Performance Audit
Corrective Actions
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Sample Collection Sample Collection

Most common source of analysis error. The laboratory personnel and sample
Sample should be representative. collectors cooperate in establishing
Use sampling plans that are based on Sampling Protocol.
appropriate statistical methods, whenever The samples preparation and storage must
reasonable. be made away from analysis area to avoid
contamination.
Sampling Protocol Sample Preparation & Analysis

Should include the following: All sample preparation steps are according to
¾ Sample size. the standard method.
¾ Container type. All reagents, acids, and water in the sample
preparation must be of that quality described in
¾ Labeling.
standard method.
method
¾ Preservation of sample.
Standard quality lab wares are used.
¾ How to transport sample to lab. No steps in analysis procedure are skipped.
Analysis are made in replicate. Method
Accuracy of method is checked. Validation
Significant Figures Rules Exercise: Significant Figures

Rule1: Include all digits that are
known with certainty plus the first 1
Measure
1
Measure
uncertain digit. These digits are Uncertainty Uncertainty

called significant figures. 2 2
Sig.
g Fig.
g Sig.
g Fig.
g
3 3
Rule 2: The last digit in a number is
assumed to be uncertain by +/- 1
unless otherwise specified. Which measurement is more precise?
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More Significant Figures Rules Rounding Rules

Rule 3: Zeros that lie to the left of Rule1: If the digit to be discarded is
the first nonzero digit are not 5 or greater, increase the retained
counted as significant figures. preceding digit by 1. If it is less than
Rule 4: In a measured quantity, a 5, do not change the preceding digit.
zero that lies to the right of the Round one digit
g 1.047 =
decimal point, and which also lies to Rule 2: When more than one digit is
the right of the first non-zero digit, to be dropped, Rule 1 is applied only
counts as a significant figure. one time to the first digit following
the last retained digit.
Significant figure is the number
0.0054070 Round two digits 1.047 =
are _________
Addition & Subtraction Addition & Subtraction

Rule1: The absolute uncertainty in a Rule 2: When the numbers to be added
sum or difference cannot be smaller or subtracted have exponents, they must
than the largest absolute uncertainty be made to have the same exponent
before addition or subtraction is carried
in any of the terms in the calculation. out
In other words,, retain as manyy digits
g
to the right of the decimal as is found
in the number with the fewest digits (5.6 x 10-2) + (3.2 x 10-1) =
to the right of the decimal.

12.2 + 0.365 + 1.03 =
8.35 - 0.365 =
Multiplication & Division Mixed Operation

Rule 1: Keep as many significant
figures in the final answer as is General rule: The rules for problems
found in the value with the least combining addition/subtraction and
number of significant figures. multiplication/division are applied
individually to each operation as it is
6.2 x 7.00 = 3.142 / 8.05 =
performed.
p
Rule 2: Keep as many significant
figures in the final answer as is 144.3 + (2.54 x 8.3) =
found in the measured value when
using an exact number.
5.0367 kg = _________________ gm
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Data Presentation: Exercise: Measurement

ASTM Recommendations
Operation Results
Presents as a minimum, the average, the (4.16x10-3) + (1.724x10-1)
standard deviation, and the number of 1.074 X 0.993
observations.
(40.1 X 0.1633)/204.228
If the number of observations is large,
((21.6 X 0.317)/4.1) + 16.037
present data in a grouped frequency.
(62.31 + 62.47)/2
Present as much evidence as possible
that the data were obtained under 9.1647 Round off to three significant digits
controlled conditions.
Measurement: Objectives Measurement: Basic

Requirements
To assess limits of error in measurements. Understand the nature of errors.
To reduce analytical errors to acceptable Understand the measurement system
levels. used.
To reduce amount of work needed to obtain Develop techniques and plans to
reliable results. minimize errors.
To provide basis for inter-comparison of Implement quality control measures.
data. Establish quality assessment and quality
assurance measures.
Measurements: Type of Measurement Errors

Quality Parameters
A laboratory is expected to be able to Systematic (or Determinate) Errors
specify the quality of its data in quantitative ¾ May cause the results to be high or low.
terms. This requires ¾ Can be constant or variable.
¾ Qualitative identification of the ¾ Can be determined and eliminated.
measurements
measurements.
Random (or Indeterminate) Errors
¾ Limits of certainty – needed to judge
¾ Occur in a symmetrical fashion around the real
confidence associated with the numerical
value.
value.
¾ Cannot be determined, controlled or eliminated.
¾ Quantitative accuracy.
¾ Probability distribution of data.
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Methods Used to Detect Measurement Accuracy &

Systematic Errors Precision (Reproducibility)
Use of standard samples of known The accuracy can be measured as:
Absolute error for a single measurement,
characteristics and performance. ¾
Eabs = |xi – μ|
Independent
p analysis
y ((use different method ¾ Absolute error for a mean,
Eabs = |x – μ|
or send your sample to other labs).
¾ Relative error = 100 * (Eabs/ μ)
Compare with different sample size. The precision can be measured as:
Absolute deviation for a single measurement
d=|xi – x|
Relative deviation, drel = 100 * (d / x)
Measures of Precision Equipment: Sampling & Testing

(more than one measurement) Capable of achieving required accuracy.
Range. Comply with specs relevant to tests.
Calibrated and/or checked prior to release
Relative range. into service.
Average
g deviation of a sample.
p Uniquely
q y identified,, whenever practicable.
p
Standard deviation of a sample. Operated by authorized personnel.
Safeguarded from tampering with.
Relative standard deviation (CV).
Readily available up-to-date instructions on
use and maintenance to relevant
personnel.
Calibration Process Requirements for Calibration

The calibration process refers to The use of appropriate and accurate
comparing the response of the standard is most important in
measurement system to known standard calibrating a measurement system.
concentration or amounts of the analyte of Standard requirements includes:
interest.
¾ Highest purity possible.
¾ Establish the relationship between the
response and the concentration or ¾ Accurately known and traceable
amounts of the analyte. concentration.
¾ Use this relationship to determine the
¾ Known stability and shelve-life-
concentration or amounts of the analyte expiration date.
of interest from the response of the ¾ Known impurities and breakdown
measurement system. products.
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Frequency of Calibration Mode of Calibration

Factors to consider in setting up a Calibration of measurement system
is a dynamic process in which both
calibration schedule: the method and the user are
¾ Accuracy required by data user. involved.
¾ Regulatory requirements. For Example:
¾ Experience of the laboratory with the ¾ A separate
p calibration myy be required
q
measurement system. for each analyst/instrument.
¾ Reported literature and experience at ¾ For class of test samples, the entire
other laboratories. analytical system may be calibrated.
¾ Recommendation of instrument ¾ Calibration materials may be used.
manufacturer. ¾ Method of standard additions of
¾ Time and cost needed for calibration. analyte to calibrate the measurement
system.
Basic Calibration Equipment How To Decrease Calibration

Balances & Meters
Uncertainty?
Thermometers Increase the number of calibration
Spectrophotometers points narrows the band, as does
Volumetric Glassware increasing the number of
Pressure and humidity
meters
t independent measurements of
Performance check on each calibration standard.
Chromatograph Whenever possible, using the line
Sieving and particle size in its region of smallest uncertainty.
equipment
pH meter Avoiding extrapolation.
Lab Conditions & Safety Metrologist Qualification

Lab facilities (e.g. lighting, energy
sources, environmental conditions) Can make good measurements.
support correct test performance. Can support and defend his/her
Lab working places and equipment must measurements …
be kept clean (good housekeeping) and ¾ Theyy are technicallyy sound
safe. ¾ They are legally defendable
Separation of areas with incompatible Can interpret his/her measurements.
activities; e.g. the samples preparation Can make value judgments, where
and storage must be made away from
needed.
analysis area to avoid cross-
contamination.
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Analyst & Supervisor Agenda – Day 3

1. ISO Overview
Analyst 2. ISO 9001 QMS – Quick Tour
¾ must have enough experience in lab operation.
3. Certificate Realization Cycle
¾ should report all the analysis work in his/her
g
logbook. 4. Accreditation/Registration
g System
y
Supervisor 5. ISO 17025 LQMS
¾ must review the bench top data and the final 6. ISO 17025: Key Success Predictors
data before approval.
¾ must make corrective actions in case of
7. ISO 17025 Requirements
inaccurate analysis results. Documentation
What is ISO? Why ISO?
ISO = International Organization for

Standards
Network of the national standards institutes of
some 140 countries
Central office in Geneva, Switzerland
Technical Committees, General Assembly
At least 75% voting to pass
www.iso.org
What is ISO 9000:2000 QMS? The ISO 9000 Family
ISO = International Organization for ISO 9000

ISO 9001 ISO ???
Standards Fundamentals Sector
QMS Model
9000 = code to denote QMS Family & Vocabulary Guidelines
2000 = year of last revision
Is a family of standards for implementing a ISO 9004 ISO 10013
Quality Management System (QMS) Continual Quality
Improvement ISO 19011
Auditing Manual
Guidelines
Guidelines
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ISO 9001 Model ISO 9001 Model & LRRC

Continual Improvement of the QMS
LRRC
UIREMENTS
UIREMENTS
SFACTION
SFACTION
info. flow management
responsibility QMS
CUSTOMER SATIS
CUSTOMER SATIS
CUSTOMER REQU
CUSTOMER REQU
resource meas., analysis info. flow
management improvement
Input product Output Input product Output

realization product realization product
value adding value adding
value value
activities activities
adding activities adding activities
ISO 9001 Requirements ISO 9001 Certificate Realization

Cycle
Clause 4. Quality Management System Identify Plan
Document
Gap
Clause 5. Management Responsibility
QM
Clause 6. Resource Management
Implement
Clause 7. Product Realization (LRRC)
Evidence
Clause 8. Measurement, Analysis and
Improvement Register Certificate
ISO 9001 Brief

USA Accreditation/Registration UK Accreditation/Registration

System System DIT
Certify Administer
Auditors Audit
(Register)
NRB Standards
UKAS BSI
Employ
Train &
•DIT = Department of
Satisffy
Accredit
E
Register
i
Industry and Trade
ANSI Standards Accredit Certify Employ (Government)
RAB Registrars Organization Auditors Registrars
ASQ (Register) •UKAS = United
Kingdom Accreditation
Certify Service
(Register) •BSI = British
•ANSI = American National Standard Institute Standards Institute
•ASQ = American Society for Quality Audit Organization Satisfy •NRB = National
•RAB = Registrar Accreditation Board Registration Board
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What is ISO/IEC 17025:1999? ISO 17025 Accreditation
General Requirements for the competence of

testing and calibration laboratories
Formal recognition of an organization competency
replaces ISO/IEC Guide 25:1990 to perform specific tests, types of tests, or
replaces EN 45001 calibration
Meeting requirements demonstrate that the lab
operates a quality system
is technically competent
is able to generate technically valid results
Example: ISO 9001 Certificate Example: ISO 17025 Certificate
CERTIFICATE OF REGISTRATION TO ISO 9001:2000 CERTIFICATE OF ACCREDITATION TO ISO/IEC 17025: 1999

COASTAL TESTING LABORATORIES, INC
307 East Pasadena Freeway COASTAL TESTING LABORATORIES, INC
Pasadena, TX 77506 307 East Pasadena Freeway
Henry Pena Phone: 713 477 0121 Pasadena, TX 77506
Henry Pena Phone: 713 477 0121
GEOTECHNICAL
Valid To : December 31, 2005 Certificate Number: R-045 Valid To: March 31, 1999 CertificateNumber: 0036-02
In recognition of the successful completion of the A2LA evaluation process, accreditation is granted to
this laboratory to perform the following tests under the ASTM recommended practice D3740:
This quality system meets the requirements of the ISO 9001:2000 standard for
mechanical and chemical testing (SIC 8734) on cold rolled and hot rolled steels. Soils:
ASTM: D420 D421 D422 D448 D558 D5 59 D560 D698 D854
D1140 D1452 D1556 D1557 D1587 D1883 D2166 D2167 D2216
D2217 D2419 D2434 D2435 D2487 D2488 D2850 D2922 D3017
D3282 D3668 D4219 D4221 D4318 D4429 D4546
ISO 17025:1999 Requirements ISO 17025 or ISO 9001

• Generic
Main Clause 4 ISO 9001 • Facility/ Product Type
Sound Management Requirements • Management
• Certification
14 clauses • Assessor not normally field expert
Main Clause 5
Technical Competency Requirements
10 clauses • Testing & Accreditation Labs
ISO 17025 • Tests/Type of Tests
• Management + Technical
• Accreditation
• Assessor is field expert
ISO 17025 Brief

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Watch for MRA Accreditation Requirements

A2LA IANZ ISO/IEC 17025 Requirements
(USA) (New Zealand) Specific Technical Field
NVLAP
Requirements
NATA Guide 58
(Australia) (USA) Accreditation Body Policies; e.g. Check with
MRA
advertising, traceability, off-premise Selected
KOLAS Accreditation
UKAS
(UK) (S. Korea) Specific Test/Calibration Methods Body
Requirements
JAB ISRAC
(Japan) (???) Proficiency Testing
www.ILAC.org
Key Success Predictors LRRC & ISO 17025

Requirements
Quality Internal Management
Organization
System Audits Review
Client Document Records
Subcontracting Purchasing
Service Control Control
Control of Corrective Preventive
Order Review Complaints
p
Nonconforming Work Action Action

Items Methods & Results Reporting

Personnel Documentation Auditing Sampling
Handling Validation QA Results
Personnel Equipment Calibration Accommodation
LRRC & ISO 17025 LRRC & ISO 17025

Management Requirements Management Requirements
Quality Internal Management Organization
Organization
Receive Prepare Perform Analyze Prepare Give Receive Prepare Perform Analyze Prepare Give
Order Sample Test Results Report Report Order Sample Test Results Report Report
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4.1 Organization From ISO to Quality Manual

Can be held legally responsible
Meet requirements of client, regulatory 4.1.5 “The laboratory SHALL
authority and accreditation body d) have policies and procedures to
Identify potential conflicts of interest & avoid involvement in any activities
countermeasures
that would diminish confidence in its
Protect client confidentiality
p
competence, impartiality,
p y jjudgment,
g
Define management structure of lab
Organization chart
or operational integrity”
Include managerial and technical personnel e) define the organization and
Define responsibility and authority of management structure of the
personnel
Have a quality manager laboratory, its place in any parent
Include technical management organization, …”
Have deputies for key managerial personnel
Sample: CETC QM 6 of 14, WIN 100
LRRC & ISO 17025 4.2 Quality System (Documentation)

Management Requirements Document, as necessary, to ensure quality
Have a quality policy statement
Organization
Quality Commitment to professional practice and
System quality service to client
Objectives of quality system
Directive that all lab personnel understand
quality system & comply
State documentation structure
Highlight roles of technical management
and QM
Sample: CETC QM 3,4 of 14
Exercise: Why Document? Documentation Structure

Key success predictor shall Level
shall
________________
shall
shall
shall
shall
QM I
________________ ISO 17025

Procedures Level
Requirements
II
Work Instructions
Level
III
Forms/Records, External Level

Documents (Other than technical SOPs) IV
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Exercise: Documentation Levels LRRC & ISO 17025

Management Requirements
What level of documentation (I, II, III, or IV)
are each of the following? Organization
Quality
System
Corrective Action Procedure Document
Control
Customer Complaint form
Quality policy of lab

Instructions on completing a purchase order
4.3 Document Control Writing a Procedure

Have a master list or equivalent
Document Control Procedures to Title/Header Procedure/Method
cover: Purpose Responsibilities
Document identification; i.e. title, date of Requirements
issue, revision no., total no. of pages, Scope
Performance indices
authority
th it for
f issue.
i D fi iti
Definitions
Document change; i.e. revision date, rev. Forms/Records
no., total no. of pages, hand amendments,
computerized sys.
Supporting documents
Obsolete documents removal Flowcharts (Optional)
Obsolete documents retention policy
Documents access & availability
Sample: CETC SOP 150, 1 of 3
LRRC & ISO 17025 4.4 Review of Requests, Tenders,

Management Requirements Contracts
Adequately define order handling
Organization
Quality methods
System
Document
Methods meet clients requirements
Control Adequate capability and resources
Order Review Differences resolved before work
commences
Maintain record of order review
Responsible for work performed by
subcontractors
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LRRC & ISO 17025 4.5 Subcontracting of Tests or

Management Requirements Calibrations
Client approval, preferably in writing,
Organization
Quality when subcontracting
System
Document
Ensure and demonstrate
Subcontracting subcontractors competence and
Control
Order Review compliance

li with
ith ISO 17025
Responsible for subcontracted work
Maintain a register of all
Receive Prepare Perform Analyze Prepare Give subcontractors
LRRC & ISO 17025 4.6 Purchasing Services and Supplies

Management Requirements Procedures for selection and
purchasing of service and supplies that
Organization
Quality affect the quality of tests
System
Procedures for checking & handling
Document
Control
critical consumables & supplies
Adequate descriptions on purchasing
Order Review
documents
Records of inspected or verification that
product complies with specifications
Record of evaluation of suppliers of
critical consumables, supplies, and
services.
LRRC & ISO 17025 4.7 Service to Client

Client is allowed to clarify
Organization
Quality requirements and monitor
System
performance of laboratory without
Client Document
Service
Control
compromising the confidentiality
of other clients
clients.
Order Review
Access to witness tests
Permission to verify test items
Receive Prepare Perform Analyze Prepare Give Communication throughout LRRC
Order Sample Test Results Report Report Order status and modification
update, if any
Client surveys
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LRRC & ISO 17025 4.8 Complaints

Policy and procedure for resolution of
Organization
Quality complaints from client and other
System
stakeholders
Client Document
Subcontracting Purchasing Maintenance of records of complaints,
Service Control
Order Review Complaints i l di allll iinvestigations

including ti ti and
d
corrective actions.

LRRC & ISO 17025 4.9 Control of Nonconforming

Management Requirements Testing and/or Calibration Work
Policy and procedures for
Quality
Organization
System
nonconformance in testing. Procedure
include
Client Document
Subcontracting Purchasing Definition of responsibilities and authorities
Service Control
for proper disposition
disposition.
Control of
Order Review Complaints Evaluation of significance.
Nonconforming Work
Corrective actions to be taken immediately.

Recall of nonconforming work released to
Receive Prepare Perform Analyze Prepare Give clients, when necessary.
Order Sample Test Results Report Report Responsibility for work resumption.
Activate Corrective Action (4.10) to
prevent recurrence.
LRRC & ISO 17025 4.10 Corrective Action

Management Requirements Policy, procedures and authorities for
implementing corrective actions when:
Quality non-conformances in work
Organization
System
departure from policies and procedures in QS
Client Document
Service Control Procedure starts with root cause analysis.
Control of Corrective
Order Review
Nonconforming Work
Complaints
Action
Select actions that
eliminate the problem (i.e. prevent recurrence)
are appropriate to magnitude and risk
Monitor corrective actions results for
effectiveness.
Special audit, if necessary.
20
9/21/2010
LRRC & ISO 17025 4.11 Preventive Action

Triggered by likely nonconformance.
Quality
Organization
System
Procedures
Triggers of preventive action; e.g.
Client Document
Subcontracting Purchasing management reviews, internal audits,
Service Control
Control of Corrective Preventive employee/client suggestion,
suggestion etc
etc.
Nonconforming Work Action Action controls to ensure effectiveness

LRRC & ISO 17025 4.12 Control of Records

Record keeping procedures; identification,
Organization
Quality collection, indexing, access, filing, storage,
System
maintenance, and disposal of quality &
Service
Control Control
technical records.
Order Review
Control of
Complaints
Corrective Preventive Q lit records
Quality d iinclude
l d
Internal audit reports
Management reviews
Receive Prepare Perform Analyze Prepare Give Corrective actions
Order Sample Test Results Report Report Preventive actions
4.12 Control of Records (Cont.) 4.12 Control of Records (Cont.)

Test record include
Record retention and disposition policy Enough information, if possible, to allow
Technical records include: repeat of the test under similar conditions
Original observations, derived data, etc to Identification of personnel involved
establish an audit trail. Observations, data, and calculations
C lib ti records
Calibration d recorded at the time they
they’re
re made and
Staff records traceable to task.
Test reports or calibration certificates Mistakes are crossed out, corrections
Test record.
entered alongside, and signed/initialed
by person making amendment
Similar provisions for computer
records
21
9/21/2010
Agenda – Day 4 Quality Control (QC) Charts

A graphical representation of test data in
1. Quality Control Charts 2. Validation of Samples,
Advantage of QC Charts Methodology, and
such a manner that the variability of all
Control Limits Data results is compared with the average
Types of QC Charts What is Validation? variability within arbitrary small groups of
Property Charts What to Validate? the test data
data.
Precision Charts Validation of Samples

Basic tools for quality assurance for the
Control Charts Validation of
Interpretation Methodology evaluation of analytical measurements,
Possible causes of out Validation of Data scientific and engineering data.
of control Situation 3. Computer Application
Advantages of QC Charts Control Limits

Provide graphic means to demonstrate statistical
control (in or out of control) In normal Distribution
Monitor measurement or product manufacturing ¾ 68% of values will be in: X 1 S
process ¾ 95% Values will be in: X 2S
Diagnosis measurement or manufacturing ¾ 99.7% Values will be in: X 3 S
problems ¾ Warning limits are sets at 2 S
Provide feedback for immediate corrective action ¾ Control limits are set at 3 S
Document measurement uncertainty
Provide important record for laboratory QA
Control Limits Types of QC Charts

There are two basic types of QC charts
UCL 3σn
¾ A “property chart” that utilize single
WL 2σn measurement (X-chart) or the mean of sets
1σn of measurement (X-bar chart)
CL ¾ A “precision chart” that utilize estimates of
1σn standard deviation (s) or the Range (R) of
WL 2σn the set of measurement
LCL 3σn
22
9/21/2010
Property Charts Precision Charts
The property charts monitor the process The precision charts monitor the process
mean. The basic two types of the Variability. There are three types:
property charts are: ¾ Individual charts ( MR-Chart )
¾ Individual charts ( X
X-chart
chart ) ¾ R
Range Ch
Chartt (R
(R-Chart)
Ch t)
¾ X-bar chart ¾ Standard deviation chart (S-Chart)
Guidelines for Implementing Selection of Quality Characteristics

Control Charts Must be measurable and expressed in
Determine which process numbers
characteristics to control Seven basic units were used
Determine where the charts should a) Lengths e) Substance
be implemented
b) Mass f) Time
Apply control charts to important
characteristics c) Current g) Length intensity
Add new charts, if necessary d) Temperature
Implement and maintain control Variables can be treated as Attribute
charts as close to the work center One Characteristic only is selected
as possible
Establish X-Chart Establish MR Chart
For the control chart for individual For the control chart for individual
measurements, the parameters measurements, the parameters for
are: − MR
−
MR are:
UCL = X + 3 −
d2 UCL = D 4 MR
−
−
CL = X CL = MR
−
− −
MR
LCL = X − 3 LCL = D 3 MR
d2
If Moving range of n=2, d2=1.128 D4=3.267, D3=0 for n = 2
23
9/21/2010
Exercise: X & MR Charts Establish X-bar Chart
The following data is

taken from the results Sample No. Assay Value For the X-bar control chart, the
posted in an actual 1 17.09 parameters are:
laboratory notebook. The 2 17.35 Based on R Based on S
readings represent the 3 17.40 =
UCL = X + A2 R
− = −
UCL = X + A3 S
Assay value. 4 17.23
= =
Plot an appropriate Control 5 17.09 CL = X CL = X
Chart for the data 6 16.94
= − = −
7 16.68 LCL = X − A2 R LCL = X − A3 S
8 17.11
9 18.47 A2 & A3 are constants values for
10 17.08 each sample size
Establish R Chart Exercise: X-bar & R Charts

The following data is
For the R control chart, the taken from the results Sample No. 1 2
parameters are: posted in an actual 1 97.0 97.1
− laboratory notebook. The 2 97.1 97.5
UCL = R D4 readings represent the 3 97.3 98.2
− observed percent 4 98.0 98.9
CL = R transmission with a 1.0 µg 5 99.0 99.5
Hg reference standard 6 99.0 98.9
−
sample being used.
LCL = R D3 7 99.0 97.8
Plot an appropriate Control 8 99.0 97.8
D4 & D3 are constants values for Charts for The data. 9 99.5 98.9
each sample size 10 100.0 100.0
Establish S Chart Control Charts: Interpretation
For the S control chart, the Process in Control

parameters are: Process out of Control:
−
UCL = B4 S ¾ One or more points outside 3σ
− ¾ A run of at least eight points
CL = S ¾ Two of three consecutive points outside 2σ
− ¾ Four of five consecutive points beyond 1σ
LCL = B3 S
¾ An Unusual or nonrandom pattern in the data
B4 & B3 are constants values for
each sample size
24
9/21/2010
Possible Causes for Possible Causes for

Out of Control Situation Out of Control Situation
Situation Causes Situation Causes
Shift in mean ¾Incorrect proportion of Std and Range ¾Concentration of standard due to
Trend of
¾Contamination of sample evaporation of solute
mean
¾Incorrect
I t instrument
i t t calibration
lib ti ¾Deterioration of reagent
downward
¾Analyst error
Increase of ¾Analyst performance

Trend of ¾ Deterioration of standard and reagent variability ¾Poor technique, or Deviation fro
procedure
mean upward
What is Validation? What to Validate?
Sample and sampling procedure

Methodology
Validation is the process of determining the
suitability of a measurement system for providing
Data and associated process
useful analytical data
Validation of Samples & Objectives of Sample validation

Sampling Procedure
To accept an individual sample as a
Sample validation should be based on objective member of a population under study
criteria to eliminate subjective decisions. To admit samples to the measurement
Generic criteria for acceptance may include: process
¾ Positive identification T minimize
To i i i llater
t questions
ti on sample
l
authenticity
¾ Conformance with physical/chemical
specifications
To provide an opportunity for re-sampling
when needed
¾ Proper sampling procedure
25
9/21/2010
Validation of Methodology Types of Method Validation

Validation of methodology is a value
judgment in which the performance Full validation of a new method.
parameters of the method are compared ¾ Requires more steps, including multi-
with the requirements for the analytical laboratory collaborative study
data
The performance parameter include:
On-Site demonstration of method
¾ Sensitivity
applicability
¾ Bias and precision
¾ Reproducibility, and elimination of
interferences (Selectivity or Specificity)
Methodology Validation: Validation of Data & Associated

Approaches Processes
Use of reference samples Data validation is the process by which data are
Compare the results with another method filtered and accepted or rejected based on
defined set of criteria
Use of split samples of the actual test
samples
In all cases, sufficient tests must be made
to evaluate the methodology for the variety Validation of associated process include
of matrices and ranges of composition statistical analysis of the data, software,
expected during the measurement process data storage and accessibility
Techniques for validation of Data Agenda – Day 5

& Associated processes 1. ISO 17025 Requirements
Internal Audit
Inter-comparison with similar sample Personnel
data 2. Accreditation Fees
Check for reasonableness of values with 3. GLP & Regulations Realization Process
respect to a priori and or posteriori limit
4. CETC Case Study
Data plots, regression analysis
5. LABEX Award Case Study
Tests for outliers
6. Course Wrap-Up
26
9/21/2010
LRRC & ISO 17025 4.13 Internal Audits

Management Requirements Internal audit procedure include
Periodic, predetermined schedule
Quality Internal Purpose to verify continuous compliance with
Organization
System Audits requirements of quality system and 17025
Client Document Records Covers all elements of quality system;
Service Control Control management & technical
Order Review Complaints Planned & managed by QM
Performed by trained and qualified
personnel, where resources permit, are
Receive Prepare Perform Analyze Prepare Give independent
Order Sample Test Results Report Report Records maintained of audits findings
and corrective actions
Game: Collecting Clues! Why Audit?

Key laboratory success predictor
Name Car Clothing
Registration/Accreditation requirement
Butcher
evel
Teacher
Lab Performance Le
Nurse
Surgeon
Time
Audit Types Certification Process

1st Party
Field Corrective
Self Registrar selection audit action
Peer
Management Formal application
Internal Audit Registration
2nd Party
Corrective Office
Customer Surveillance
action audit
3rd Party audit
Registrar/ Accreditation Body

Not OK
Optional pre-audit
Regulator (Inspection) CA/Suspension/
Termination
27
9/21/2010
Audit Process Corrective Action

Plan audit
SAMPLES •Identify NC
Sign NCR
•CETC Audit Plan •Issue NCR
Execute audit •CETC On-Site Audit Checklist
•CETC FRM 450-1
•CETC Internal Audit Report
A
Agree?
? Propose CA
Report findings not OK
OK
Review CAs
•Verify CA Implement
•Close NCR CA
Close-out
Objective Evidence Sources LRRC & ISO 17025

Observation Management Requirements
Show me how …
Equipment inspection Organization
Documentation Client Document Records
Most verifiable Service Control Control
Records focus Order Review
Nonconforming Work
Complaints
Action Action
Interview
Be prepared
5W+H Order Sample Test Results Report Report
Checklist
4.14 Management Reviews LRRC & ISO 17025

Periodic, predetermined Management Requirements
schedule and procedure
Conducted by lab’s executive Organization
management System Audits Review
Agenda includes Client Document Records

QS suitability and effectiveness Control of Corrective Preventive
Resources & staff training Nonconforming Work Action Action
Audits outcome
Inter-laboratory comparisons or
proficiency testing Receive Prepare Perform Analyze Prepare Give
Client feedback, complaints Order Sample Test Results Report Report
Management Review records
are kept
28
9/21/2010
LRRC & ISO 17025 LRRC & ISO 17025

Technical Requirements Technical Requirements
Receive Prepare Perform Analyze Prepare Give Receive Prepare Perform Analyze Prepare Give
Order Sample Test Results Report Report Order Sample Test Results Report Report
Items Methods & Results Reporting Items Methods & Results Reporting
Sampling Sampling
Handling Validation QA Results Handling Validation QA Results
Personnel Equipment Calibration Accommodation Personnel Equipment Calibration Accommodation
5.2 Personnel Why Train?

Ensure competency of all personnel
Appropriate supervision when using personnel in
training Key laboratory success predictor
Formulation of goals - policy and procedure for Legal requirement; e.g.
the identification of training needs
Personnel shall be employed by or under contract right-to-know &
to the lab
right-to-be
i ht t b ttrained
i d
Contract employees shall be supervised and
operate in accordance with quality system Registration/Accreditation requirement
Job descriptions
Maintain records of all personnel involved in
technical operations, including date of
authorization and/or competence
Records readily available
Competency & Care I TRUST

employees Selection & Training
who are
competent
and caring.
EFFECTIVE
•may not work for low- •winner lab

attitude trainee.
•more costly relative to the
HIGH
Training
cost of proper selection.

Attitude
•decreased competency in
•weak lab
the long run
run.
T
WEAK
K
•dissatisfied employees and

high employee turnover.
LOW
•deteriorating lab.
WEAK EFFECTIVE
LOW HIGH L
E Selection
A
D
Competency E
R
29
9/21/2010
What Do You Think? Training Tenets

It’s lab worker responsibility; management
support is necessary but not sufficient
petency Level
Training is for all

Current job description is a prerequisite
Comp
Competency assessment
Prior to developing a training plan
Time After completing the training program
4 Levels training assessment
Training Cycle Training Subjects

Responsibility Records
Site-related
No Job
Develop
Desc.? Know your organization (physical & management)
Yes
Lab-related
Assess
Competency Know the lab (adequate detail)
Develop
Job-related
Train. Plan
Know your job (high detail)
Execute
Career-development-related
Personal skills
Assess Related subjects and skills
Plan
Lab Analyst Training Program Lab Analyst Training Plan

1. Orientation (company & labs)
Training Responsi Schedule Trainee Trainer
2. Job introduction Element bility Signature/ Signature/
Date Date
3. Regulations
Orientation
4. General SOPs ((management)
g ) Lab-related
Safety
5. Job-related SOPs (technical) Mgt SOPs
6. Equipment & hands-on training Job-related

ASTM … test
7. Refresher & Career Development
Writing Skills
Training
Verbal Skills
30
9/21/2010
Trainers Training Material Sources

Self Conferences
Most ignored Company & labs material
Most informal

Technical Institutes standards (e.g. ASTM, BSI)
Mentor Regulations
g ((e.g.
g EPA))
Supervisor Manufacturers
Vendor Web
Some leave it out of the procurement contract!
Professional Trainer (external)
Training Modes LRRC & ISO 17025

Let me read about it Requirements
Company, vendor material Quality Internal Management
Organization
Web, books, journals, etc. Client Document Records
Show me how Control of Corrective Preventive
p
Instructions
Internal
External
Items Methods & Results Reporting
Sampling
Videos Handling Validation QA Results
Personnel Equipment Calibration Accommodation

Let me show you how
Accreditation Fee: Factors Accreditation Fee: A2LA

Application fee
No. of facilities (sites), $1000 for first facility + $800 for additional ones
No. of labs Annual fee (on and after accreditation)
$1,300 for first field/lab + $900 for additional fields
No. of fields Discounts for and/or labs (within a facility) each
• multiple fields
No. of tests • multiple labs Assessment fee (accreditation or surveillance)
Facility size Based on man-days ($800)
More time/cost for accreditation
Adequacy of preparation Less time/cost for surveillance
Travel & Accommodation Travel & Accommodation
Depends!!
31
9/21/2010
GLP & Regulations Realization General Principles of GLP

Process Government Compliance
1. GLP Qualified person
Regulations Acts
2. Compliance Adequate Facility
Properly maintained and calibrated
equipment
i t
Impact
Adherence to SOPs and protocols
Independent and qualified QA Staff
• Parliament produce Acts.
•
•
President sings into a Law
Government (e.g. OSHA, EPA) interpret and enforce laws
Validated data
•
through Regulations and GLPs.
Labs must Comply with GLPS. If they don’t , they go to court.
An easy retrievable archival system
Why ISO 17025?
To pioneer
Case Study For market advantage
To improve performance
ISO 17025 in CETC T anticipate
To ti i t future
f t
opportunities
Internal or External Consultants Our ISO 17025

Realization Approach
External
1. Form team & develop plan
Dubai: Do ISO 9001 instead!
UK: Expensive!
2. Select accreditation scope & define
client team
3. Select accreditation bodyy
Decision: Go Internal
4. Develop QM & verify
Allocate resources … Still much
cheaper 5. Implement
Learn as you realize … Be patient 6. Conduct awareness
7. Conduct internal audit
Gain: Certificate + Consultants 8. Send application package
32
9/21/2010
Our ISO 17025 Experience Case Study
Start small & focus on system.

Insist on total involvement of Mgt. Rep.

The LABEX Award
Select accreditation body up-front.
Review equipment
q p status up-front.
p
Select credible organization to do
proficiency testing & calibration.
Need local or regional accreditation body
with MRA.
What is it? What is the Purpose?
Is an annual award Reward excellent

program for laboratory efforts and practices by
excellence in the laboratory personnel
College of Engineering
& Petroleum (CEP).
Each year the Dean of Promote awareness of
CEP awards up to 3 excellent laboratory
LABEX Awards. practices in CEP.
The criteria are high.
Only the very best will
succeed
Who is Eligible? The Award
Any laboratory in the CEP is eligible to Honorarium of 1250 KD to be distributed

apply for the award, provided that it has not between the laboratory team members in
received the LABEX Award in the last year. accordance with an “honorarium
A laboratory that has previously been distribution plan” to be submitted with the
awarded the LABEX Award has to show a application
remarkable improvement across the
LABEX Award Criteria. LABEX Certificate given to each member
The LABEX Award is presented to a LABEX Trophy given to the lab.
laboratory team that consists of one or LABEX Training Voucher issued by OCCD
more technical staff members (i.e. teaching to each member to attend one training
assistant, lab engineer, scientific assistant,
course offered by OCCD
technician).
33
9/21/2010
Award Criteria Design Award Criteria
Personnel improvement focus 1. Organization & Documentation

Documentation improvement focus 2. Housekeeping & Safety
Customer service improvement focus 3. Laboratory Access & Resources Utilization
4
4. Technical Staff Development
5. Users Services
Auditing Process 2002/2003 Timetable
Receive application Review the Give Awareness Seminars 17 & 18 Nov. 2002
Screen 1
package application package Receive Application Packages 1 March 2003
Review Application Packages – 1st 2 – 29 March 2003

Review the Screen
Screen 2
Laboratory Review Laboratories – 2nd Screen 30 March – 19 April 2003
Review Presentations – Final Screen 20 April – 3 May 2003

Nominate the Review Final Nominate and Announce Winners 14 May 2003
winners presentation Screen
Winners Give Public Presentations 24 – 28 May 2003
2002/2003 Main Changes
More time to prepare

Publicize audit protocol
Provide examples
p of p
proofs/ evidences
Provide training
All on the web page
Aldowaisan & Youssef
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9/21/2010

Office of Consultation & Career Development

Our Objective Training Approach

Aldowaisan & Youssef Aldowaisan & Youssef

Agenda – Day 1 Exercise: What is Quality?

1. Basic Quality 2. Statistical Overview

Aldowaisan & Youssef Aldowaisan & Youssef

Totality of  Meaning of quality cannot be captured in a

Aldowaisan & Youssef Aldowaisan & Youssef

Exercise: Quality Dimensions Exercise: Quality Violations

Aldowaisan & Youssef Aldowaisan & Youssef

Key Quality Dimensions Accuracy & Precision

Accuracy Reliability ____________ ____________ ____________ ____________

Lab ____________ ____________ ____________ ____________

Aldowaisan & Youssef Aldowaisan & Youssef

Quality Control (QC) Quality Assurance (QA)

The monitoring, inspecting and auditing to

Aldowaisan & Youssef Aldowaisan & Youssef

Quality Management System Quality Concepts Relationships

Aldowaisan & Youssef Aldowaisan & Youssef

Quality Cycle Statistical Overview

Aldowaisan & Youssef Aldowaisan & Youssef

Descriptive Statistics Exercise: Centrality Measures

Aldowaisan & Youssef Aldowaisan & Youssef

Exercise: Dispersion Measures Exercise: Descriptive Measures

Aldowaisan & Youssef Aldowaisan & Youssef

Estimate of Standard Deviation from Estimate of Standard Deviation from

Combining (Pooling) Estimates of Exercise: Duplicates & Pooling

equation: analysis of isooctane

Hypothesis Testing Test 1: Comparing the Mean With

Aldowaisan & Youssef Aldowaisan & Youssef

Test 2: Comparing Two Means Exercise: Comparing Two

Aldowaisan & Youssef Aldowaisan & Youssef

Test 3: Comparing Two Exercise: Comparing Two

Aldowaisan & Youssef Aldowaisan & Youssef

Regression Analysis Method of Least Square

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

Aldowaisan & Youssef Aldowaisan & Youssef

Exercise: Regression Analysis Computer

Aldowaisan & Youssef Aldowaisan & Youssef

Agenda – Day 2 Lab Results Realization Cycle

Aldowaisan & Youssef Aldowaisan & Youssef

LRRC & QA LRRC & QA Program

Supplies Order Sample Test Results Report Report

Equipment & Maintenance During Testing

Aldowaisan & Youssef Aldowaisan & Youssef

LRRC & QA Program QC, QA & QMS Requirements

Sample Collection Sample Collection

Aldowaisan & Youssef Aldowaisan & Youssef

Sampling Protocol Sample Preparation & Analysis

Aldowaisan & Youssef Aldowaisan & Youssef

Significant Figures Rules Exercise: Significant Figures

uncertain digit. These digits are Uncertainty Uncertainty

Aldowaisan & Youssef Aldowaisan & Youssef

More Significant Figures Rules Rounding Rules

Aldowaisan & Youssef Aldowaisan & Youssef

Addition & Subtraction Addition & Subtraction

to the right of the decimal.

Aldowaisan & Youssef Aldowaisan & Youssef

Multiplication & Division Mixed Operation

Aldowaisan & Youssef Aldowaisan & Youssef

Data Presentation: Exercise: Measurement

Measurement: Objectives Measurement: Basic

Aldowaisan & Youssef Aldowaisan & Youssef

Totality of Meaning of quality cannot be captured in a

Accuracy Reliability

Lab

ISO = International Organization for

ISO = International Organization for ISO 9000

General Requirements for the competence of

________________ ISO 17025