Determination of the total inorganic cyanide content of industrial waste water.pptx

Determination of the total inorganic cyanide content of industrial waste water in environment

1. ISO/IEC 17025:2005 Standard Requirements A. Fajgelj Quality Systems Manager Department of Nuclear Sciences and Applications Training Workshop on Quality Assurance for Nuclear Spectrometry F1-TR-52968, 19-23 June 2017 Vienna, Austria

2. ISO/IEC 17025:2005 General requirements for the competence of testing and calibration laboratories Management requirements Technical requirements Criteria for laboratories wishing to demonstrate that they are technically competent, operate an effective quality system and are able to generate technically valid calibration and test results

3. ISO/IEC 17025:2005 requirements – an example Determination of the total inorganic cyanide content of industrial waste water: Waste water UV-destruction: complex CN  HCN Distillation Colorimetric determination Automated system

4. From order to report Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control

5. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of order/contract Order Example Contract, record of agreement Correspondence with client Requirements clearly defined ? Capacity of lab Capability of lab Trackability order Which forms of cyanide ? Range, LOD To be checked Aspect

6. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of sampling Sampling Not necessarily done by the lab Requirements similar as for measurement: SOP, skills, quality controls … but also sampling plan Not included in this example

7. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of sample reception Sample Reception Aspect Logbooks Identification Internal communication To be checked Trackability Labels on actual samples Communication of requirements to analyst, SOP Example Method, precision ...

8. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of storage Storage Aspect Conditions To be checked Suitability Temperature/ climate control Stability Possible contamination ? Example Refrigerated Dark 0,01M NaOH Max. 14 days to analysis

9. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of sub sampling Example Identification Representative ? SOP Duplicates To be checked Aspect Homogenisation of the sample Sub sampling

10. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of sample preparation Sample preparation Aspect Skilled operator To be checked Observation Use of spikes, RM Example Included in measurement: - UV destruction - Distillation use of RM

11. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of measurement Example Method Execution of analysis Quality controls Validation Choice, SOP Competence Instrument checks Calibration To be checked Aspect NEN 6655 (1997) Check of base line, gain Calibration line, certificates Measurement

12. Requirements of measurement: validation Confirmation by examination and the provision of objective evidence that particular requirements for the intended use are fulfilled (client !) As extensive as needed By: calibration, interlabs, assessment of uncertainty ... Parameters: uncertainty, LOD, selectivity, repeatability, reproducibility, ... Example: Calibration (RM) Precision LOD Bias Interferences

13. Measurement uncertainty estimation Rigorous, metrological and statistically valid calculation or Reasonable estimation based on identification of possible components Degree dependent on: requirements test/method requirements client limits conformance decision From statement in standard method All components that are important in given situation Example: Identification sources Calculation combined uncertainty from precision and bias studies

14. Measurement traceability Example Calibration of equipment Reference Standards RM Calibration: traceable to SI (or via national measurement standard) Testing: unless of little contribution to total uncertainty When not possible/irrelevant: traceability to CRM, agreed method or consensus standard Programme/procedure for calibration Traceable to SI or CRM (when possible) To be checked Aspect Thermometers CRM traceable to NIST value Weights

15. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of calculation and evaluation Example Calculations Data transfers Evaluation Computer programs: integrity, confidentiality To be checked Aspect Commercial software Visual check of peak formation Evaluation of QC samples Calculation Evaluation

16. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of report Identification Contents Sampling Amendments Report, method, sample, client, … Uncertainty, method (deviations ?), opinions, interpretations For calibration: conditions, traceability To be checked Aspect Report

17. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Quality control Example 1st line: - regular use CRM and/or internal QC with secondary RM - blanks, replicates Trend analysis 2nd line: duplicate sub-sampling 3rd line: interlaboratory comparisons To be checked Working level standards, complex cyanide standard: control charts KSCN check standard CRM Aquacheck, Setoc Quality control

18. Non-conformity management Non-conformities, departures: Detected through complaints, audits, QC, ... Cause analysis and corrective actions Preventive actions Records

19. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Document control Of internal and external documents Quality manual, procedures, SOP’s, … Documents: identification, review, authorisation, changes All instructions, manuals, … up to date and available Control of records: retrievability, traceability of original data Document control

20. Accommodations - equipment Accommodations Equipment (when of influence) (Environmental) conditions Contamination Access Availability Identification, instructions on use Logbooks/programmes for: - maintenance, repairs - calibrations To be checked Aspect

21. Chemicals - reference materials Chemicals Reference standards, materials To be checked Aspect SOP for selection, purchase, storage Calibration, traceability SOP for use, handling, storage … (integrity !)

22. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Management and organisation Adequate supervision Quality manager Quality system Review Audits Customer satisfaction Purchasing Subcontracting Management Organisation

23. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of personnel Appropriate number and level of personnel Competence Training Administration Needs, programme, records Job description, file, authorisations (qualifications) To be checked Aspect Lab staff

24. Sample preparation Order Sampling Sample Reception Storage Sub sampling Measurement Calculation Evaluation Report Management Organisation Lab staff Document control Equipment Chemicals Ref materials Quality control Requirements of personnel Lab staff

25. All procedures to be revisited and than approved A distribution list of documentation to be prepared Consistency of the coding system required All reference listed in SOPs and Instructions need to be readily retrievable Records required need to be specified as well as who, where and for how long keeps them DRAFT  APPROVED  ACTIVE Procedures - Instructions

26. List of equipment (systems) to be prepared Instrument (system) logbooks to be arranged Calibration status to be identified where appropriate Responsibilities to be defined Equipment

27. Quality policy statement and objectives in the manual Management review meetings – records to be kept Management support and continuous involvement Job descriptions - review Communication Action plan: who, what, when…. ….do we know why? Management