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Calibration
 

Calibration

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    Calibration Calibration Presentation Transcript

    • Calibration Pradeep Kumar. G.T
    • DefinitionCalibration is the set of operations that establish, under specified conditions, the relationship between values indicated by a measuring instrument, a measuring system or values represented by a material measure, and the corresponding known values/standard value of a measurand.
    • Steps1. Identify instruments/glassware2. Identify sources of calibration facility/procedures3. Calibration procedure4. Documentation5. sources of error6. correction
    • 1. Identify instruments/glassware • Instruments /glassware which –Directly influence the results –Measure physical quantities –Detect the residue –Used for CRM preparation –Used for reconstitution
    • 2. Identify sources of calibration facility/procedures• Calibration procedures • IS, ASTM, BS• Manufacture’s instruction •GC, GC-MS, LC-MS
    • • NABL accredited calibration laboratories •SCTIMST, Poojappura, Trivandrum •STIC, CUSAT, Cochin •FCRI, Palakkad
    • 3. Calibration procedure• General rules• One-point calibration • Volumetric glassware• Two-point calibration • pH meter• Multi-point calibration • GC,GC-MS, LC-MS
    • CRMs/Standards for calibration• Certified Reference Material• Certificate• Correction in the reading• Calibration Curves • graph which relates reference value to the instrument’s output
    • Documentation• Name of equipment and identification number• Observed reading/value• Reference value• Difference between reference value and observed value• Corrective action may include servicing, labeling, or disposal
    • Sources of error• Stabilisation• Normal position• Avoid sources of interference• Avoid traces of leftover• Calibration accuracy should be 3 to 10 times the accuracy required for the measurement .
    • Traceability• Traceable to a national standards. • In India it is with National Physical Laboratories, New Delhi• SI system
    • Uncertainty
    • Calibration of balance• Stabilization• Accuracy test• Repeatability test• Eccentricity or off-centre loading• Acceptance criteria
    • Calibration of GC, LC• Calibration of Instrument performance –Flow calibration using flow meter –Temperature calibration –Detector signal/sensitivity –Mass calibration for mass spectrometer
    • • External/Internal calibration using CRMs – Find out the retention time. (RT, compound parameters and spectrum for MS) – Prepare the pesticide CRM mixture (min 5 levels) – Inject this mixture in GC or LC » Cont.
    • –Give the names, retention time, compound parameters and concentration–Draw the calibration curves.–This calibration curve can be used for the quantitation of pesticides.