Lecture 10

Metallurgical and Analytical Quality Control

What is QA/QC?
• Quality Assurance (QA)
– Are we doing the right things?
– Management
• Quality Control (QC)
– Are we doing things right?
– Technical
Quality Control
• Are we doing things right?

• A technical concept:
– Did we do the test?
– Did the results pass or fail the criteria?
– If the results failed did we perform a corrective action?

• QA refers to planned and systematic processes that provide confidence of a product's or service's
effectiveness.
• It makes ‘quality’ a main goal of a production.
• Lab QA: all of the procedures, actions, paperwork that take place to be sure the results given are
accurate.
Quality Assurance

• Are we doing the right things?

• A management concept:
• Planning
• Assessment
• Continued improvement
Purpose of QA/QC
• Determine precision and accuracy,
• Demonstrate absence of interferences,
• Demonstrate absence of contamination (from sampling equipment, glassware,
and reagents)
What Qualities do We Want to Control?
• Accuracy - closeness to the “true” value
• Precision – repeatability

• Accuracy
• Composed of precision and bias
• Measure of the overall agreement of a measurement to a known value
• – when random errors are tightly controlled, bias dominates the overall accuracy
• – when random errors predominate, variance (imprecision) dominates the overall accuracy
• Use bias and precision as separate measures rather than accuracy
Precision
• Precision is the measure of agreement among repeated measurements under identical conditions
• A precision QC is a quantitative indicator of the random errors or fluctuations in the
measurement process
– e.g., standard deviation or variance
- The variance is a measure of variability. It measures variability from the average or mean. It is
calculated by taking the average of squared deviations from the mean.

- The standard deviation (σ) is derived from variance and tells you, on average, how far each value
lies from the mean. It’s the square root of variance.
Sensitivity
• Usually regarded as detection limit
• Capability of a method or instrument to discriminate between measurement responses
– but this term is often used without defining what is intended (minimum detection or
quantitation)
• A sensitivity QC describes the capability of measuring a constituent at low levels
– a Practical Quantitation Level describes the ability to quantify a constituent with known
certainty
• e.g., a PQL of 0.05 mg/L for mercury represents the level where a precision of +/- 15% can be
obtained.
Bias
• Bias is systematic or persistent distortion of a measurement process that causes error in one
direction
• A bias can result from:
– biased sampling design
– calibration errors
– unaccounted-for interferences
– chronic sample contamination
Influence of Bias and Imprecision on Overall Accuracy
Data Verification

• The procedures needed to ensure that a set of data is a faithful reflection of all the processes
and procedures used to generate the data
– verification entails the examination of objective evidence that the specified method, procedures,
and contractual requirements were fulfilled
Data Validation
• Analyte and sample matrix-specific process to determine the analytical quality of
a data set
– inspection of data handling practices for deviations from consistency,
– review of quality control (QC) information for deviations,
– assessment of deviations,
– assignment of data qualification codes
• Validation can entail the examination of the data with respect to the QA Project Plan
Calibration System
• In a calibration system, the following items shall be defined.
1. Classification of calibration
2. Standard and levels of standard.
3. Interval of calibration and limit of correction
4. Procedures of calibration
5. Action after calibration
6. Conditions to use measuring instrument
7. Procedures of measurement
Why Measurements?
Measurements are basic tools
• If I can define it, I can measure it.
• If I can measure it, I can analyze it.
• If I can analyze it, I can control it.
• If I can control it, I can improve it.

Measurements are needed to :

• Choose, develop and validate models used to predict, control or improve various
phenomena.
Measurements provide the very basis of all control actions.
What are Measurements?
• A process that follows a defined sequence of steps/activities; involves physical,
material and technological resources; and results in a numerical value/a set of
numerical values that is assigned to an item in respect of a defined property/
parameter/ characteristic.
• Measurement : The output of a (measurement) process.
‐ a numerical value
Errors in Measurements
• The difference between the measured value and the true value is called error. Error
can have either positive or negative sign. Error can be regarded as being composed of
two parts – random error and systematic error
• Errors in the observed results of a measurements give rise to uncertainty about the
true value of the measured as is obtained from those results.
• Both systematic and random errors affecting the observed results contribute to this
uncertainty.
Errors in Measurements
• Random errors presumably arise from unpredictable and spatial variations of influence quantities.
- the way connections are made or the measurement method employed
- uncontrolled environmental conditions or their influences
- inherent instability of the measuring equipment
- personal judgment of the observer or operator, etc.
• These cannot be eliminated totally but can be reduced by exercising appropriate controls.

• Various other kinds of errors, recognized as systematic, are also observed.

• Some common type of these errors are :
- those reported in the calibration certificate of the reference standards/instruments used.
- those due to different influence conditions at the time of measurement compared with those
prevalent at the time of calibration of the standard.
Quality in Measurements
• Quality of measurements is comprehended in terms of Accuracy and Precision, based on
systematic/random errors respectively that get reflected in repeat measurements. A more recent
development takes care of both random and systematic errors and results in a measure of
Uncertainty about the true value.

• Accuracy is the critical parameter, and is not the same as precision. Accuracy is closeness to the
true value (of the measured), while precision implies consistency among repeat measurements .

• The quality of the measurement result, its accuracy, is characterized by measurement uncertainty
(or simply uncertainty), which defines an interval around the measured value CMEASURED, where the
true value CTRUE lies with some probability.
Uncertainty of measurement
• Uncertainty of measurement is the doubt that exists about the result of any measurement. You
might think that well-made rulers, clocks and thermometers should be trustworthy, and give the
right answers. But for every measurement - even the most careful - there is always a margin of doubt.

• Since there is always a margin of doubt about any measurement, we need to ask ‘How big is the
margin?’ and ‘How bad is the doubt?’ Thus, two numbers are really needed in order to quantify ; One is
the width of the margin, or interval. The other is a confidence level, and states how sure we are that the
‘true value’ is within that margin.
• For example: We might say that the length of a certain stick measures 20 centimetres plus or minus 1
centimetre, at the 95 percent confidence level. This result could be written:
20 cm ±1 cm, at a level of confidence of 95%.
The statement says that we are 95 percent sure that the stick is between 19 centimetres and 21
centimetres long.
NABL Requirements :Technical Criteria
• National Accreditation Board for Testing and Calibration Laboratories (NABL) is
an autonomous body under the Department of Science & Technology (DST),
Government of India. The objective of NABL is to provide third-party assessment
of the quality and technical competence of testing and calibration laboratories.

• Standard required : ISO/IEC 17025 : 2005

• What are Technical requirements ? Need to be satisfied in order to establish
technical competence of a Laboratory to carry out the Testing and Calibration
activities of the Organization
• In ISO/IEC 17025, the Technical requirements are elaborated in Section 5.0.
Quality Assurance in Metallurgical Industries
Quality Assurance in Metallurgical Industries
• High-quality raw materials – the plant needs to carry out strict internal controls which prevent
the use of inappropriate raw materials
• Technological processes – the plant’s production technology should be implemented by high-
quality experienced specialists with knowledge of modern practices
• Control systems – controlling mechanisms need to work at every stage of production
• Qualified workforce – the plant should implement systems for the selection of qualified
personnel and professional training, thus ensuring a high level of individual competencies
• Advanced laboratory – control of quality should be carried out in a laboratory equipped with
modern equipments where the characteristics and qualities of the products are tested
Quality Assurance System in Metallurgical Industries
• The quality assurance system assessment is done during inspections.
• The assessment takes into account :
- The effectiveness of previously determined corrective actions based on internal
and external audits
- Progress of quality improvement plans undertaken
- Identification of non-conformities and low effectiveness
Raw Material Quality
• Assessment of raw materials based on the reports provided
• In house analysis of raw material quality
• The data obtained is entered in the system
• For example in steel making plant, raw materials such as :
- steel scrap
- ferro alloys, pig iron
- alloying additions
- refractory mixtures
Inspection and Testing
• Different stages of production
require inspection and testing
• At each stage, the data is obtained
and recorded
• The ‘Quality records’ are created
and stored
• Inspection and testing activities
have procedures and instructions
Inspection and Testing in Steelmaking plant
Metallurgical Quality Control Tests

• Chemical tests
- Control of incoming raw materials – inclusions and composition
- Product certification
- Client requests and orders

• Mechanical Tests
• Tensile Test at RT and High Temperature
• Hardness Test (Brinell – Rockwell – Vickers)
• Creep and Stress Rupture Test
• Fatigue Tests
Metallurgical Quality Control Tests

Non destructive tests (NDT)

• Ultrasonic testing
• Magnetic particle testing
• Eddy Current testing
• Dye penetrant testing
• Visual testing