Role of Planning & Communication in Obtaining Accurate Lab Results

1. 2009 KBC Advanced Software Applications for the Process Industries Conference Mexico City, Mexico The Role of Effective Planning and Communication in Obtaining Accurate Lab Results Jay Grills, Envantage, Inc.

2. The Role of Effective Planning and Communication in Obtaining Accurate Lab Results Jay Grills Envantage, Inc.

3. The Lab’s Dilemma • Needs of the process engineer vs Needs of Planning and Design Engineering • Turnaround requirements • Precision and accuracy requirements • Operational Efficiency of the Laboratory Envantage, Inc. 2009

4. Typical Lab Daily Sample Workload Envantage, Inc. 2009

5. Acceptable Precision • Precision – • The ability of a measurement to be consistently reproduced • What defines acceptable precision? • Process Control acceptable precision • Planning/Development Engineer acceptable precision Envantage, Inc. 2009

6. Acceptable Precision • Process Control Samples • Make up over 70% of daily sample load • 3 Standard Deviation control limits typical • %RSD >5% , <15% acceptable • Rapid Turnaround Primary Concern of Unit Engineers Envantage, Inc. 2009

7. Acceptable Precision Envantage, Inc. 2009

8. Acceptable Precision • Submitted/Ad Hoc Samples from Planning/Design Engineering • Higher precision requirements • Typically <2% RSD needed when possible • Data used to tune models and process variables • Higher level of accuracy on component level required Envantage, Inc. 2009

9. Lab Precision Weighted Towards Process Control Planning & Dev Engineering Process Control Envantage, Inc. 2009

10. Knowledge of the Sample is Key • Knowledge of the Sample by the Lab • Historical familiarity of sample results by lab technician • Laboratory Information Systems (LIMS) have predefined specification limits • Notify lab of near or off-spec result(s) • Instrument validation/Retesting before data released • Rely on historical information for the sample(s) Envantage, Inc. 2009

11. Impact of Analytical Techniques on The Accuracy of Lab Results • Analytical Tests can be divided into two primary groups: • Direct Instrument Measurement • Interpretative Measurement Envantage, Inc. 2009

12. Impact of Analytical Techniques on The Accuracy of Lab Results • Direct Instrument Measurement • Instrument provides results directly • Little or no interpretation required by the operator • Examples • Automated D86 Distillation • Automated Freezepoint • Digital density measurement Envantage, Inc. 2009

13. Impact of Analytical Techniques on The Accuracy of Lab Results • Interpretative Analytical Measurements • Data from instrument must be verified and/or interpreted by the user • Final results are typically at component level form (benzene content, toluene content, etc.) or may be grouped in bulk (Total Aromatics, N+A, etc.) • Knowledge of sample, process, source, and other information vital to accurate results Envantage, Inc. 2009

14. Impact of Analytical Techniques on The Accuracy of Lab Results • Interpretative Analytical Measurements • Examples: • Detailed Hydrocarbon Analysis (Gas Chromatography) • Gas Chromatography – Mass Spectrometer Analyses • Gas Chromatography LPG Analysis • APHA Color (manual) Envantage, Inc. 2009

15. Impact of Analytical Capabilities on The Accuracy of Lab Results • A typical modern gas chromatography system Envantage, Inc. 2009

16. Impact of Analytical Capabilities on The Accuracy of Lab Results Typical LPG GC Trace Envantage, Inc. 2009

17. Impact of Analytical Capabilities on The Accuracy of Lab Results Typical CRU Feed by Detailed Hydrocarbon Analysis Envantage, Inc. 2009

18. Impact of Analytical Capabilities on The Accuracy of Lab Results Detailed Hydrocarbon Analysis Interpretation Software Envantage, Inc. 2009

19. Impact of Lab Modifications to Methods for Fast Turnaround • Example: Process Control Samples Reformer Product • ExpectedVol% Standard DHA ‘Fast’ DHA • Total Paraffins <30 28.0 32.0 • Total Olefins <1 0.5 0.5 • Total Naphthenes <2 1.25 2.25 • Total Aromatics >55 70.25 62.25 • Result: Process Engineer Satisfied, Lab Satisfied Envantage, Inc. 2009

20. Impact of Lab Modifications to Methods for Fast Turnaround • Component level results: • Standard Method (Contract lab results) • 1,2,4-Trimethylbenzene 1.25 Vol% • ‘Fast’ Method (Plant Lab Results) • Isobutylcyclohexane 1.34 Vol% • Result: Design/Planning Engineer subjected to increase costs and time to receive the correct value; confidence in plant laboratory diminished Envantage, Inc. 2009

21. Impact of Lab Modifications to Methods for Fast Turnaround • Upside of Modified Test Methods • Faster turnaround • Lower cost per sample to the laboratory • Bulk property information not affected signficantly • Satisfaction at the units with more timely data Envantage, Inc. 2009

22. Impact of Lab Modifications to Methods for Fast Turnaround • Downside of Modified Test Methods • Increase errors at component level • Incorrect data for fine-tuning models • Inability to validate precision against published ASTM or other precision values for the standard method • Leads to time-consuming and costly re-testing and outside laboratory costs to rectify Envantage, Inc. 2009

23. Design Development and Budgeting Design Development and Budgeting Lab Involvement in Design, Sampling Implications, Analytical Requirements Role of Planning and Communication Purchase of Materials, Models, External Vendor Contracts, Lab Equipment, Software Purchase of Materials, Models, External Vendor Contracts Construction Construction Test Runs Test Runs Samples to Lab Samples to Lab Tune Process and Model Variables Tune Process and Model Variables Sample Results Sample Results Project Complete Process LIVE Project Complete Process LIVE Correct Approach Wrong Approach Envantage, Inc. 2009

24. Project Team Formation and Initial Planning • Gather all parties responsible for the project together. • This should include engineering, operations, and laboratory management including lab chemist(s). • The lab chemist should be a primary team member • Co-Ownership of the project plan • Valuable Insight from an Analytical Perspective Envantage, Inc. 2009

25. Project Team Formation and Initial Planning • Avoid fixing budgets and plans early on • Keep all team members informed • Avoid deviations from discussed plans until all team members, including the laboratory, can provide feedback Envantage, Inc. 2009

26. Project Team Leader Responsiblities • Describe the process to be developed or modified with the analytical lab chemist • Current/Expected Unit Structure/Function • Changes being proposed • Expected outcomes • Theoretical data on predicted changes to composition of products • Expected yields in bulk terms Envantage, Inc. 2009

27. Design/Planning Engineer Responsiblities • Detail expected precision requirements • Provide or suggest any additional resources to the chemists that will assist them • Knowledge of the process means that the correct tests and procedures will be selected by the laboratory at the beginning! Envantage, Inc. 2009

28. Design/Planning Engineer Responsiblities • If possible tour the current unit with all team members • Point out the various components of the unit • Point out current sample points and conditions • If the unit does not exist yet, provide simple diagrams of the unit • Include projected sample points and positions on piping or vessels Envantage, Inc. 2009

29. Design/Planning Engineer Responsiblities • Sample points should be identified and Tagged • Lab can further review the points later • Lab can map the locations and physical conditions • Expected sample pressure and temperature • Expected phase behavior of sample at this point • Geometric location of sample ports • Sample container/cylinder connection types available Envantage, Inc. 2009

30. Analytical Chemist Responsiblities • Research and develop proper procedures for sampling • Outline minimal sample documentation for these sample points • Determine the most appropriate tests required for this sample • Based on specific requirements of the design engineers • Utilize standard body recognized test wherever possible Envantage, Inc. 2009

31. Analytical Chemist Responsiblities • Outline the current capabilities of the lab to perform these tests • Specify potential instrument and/or software purchases necessary to meet the project’s needs • Obtain cost estimates for these purchases to inform the rest of the team for budgetary planning Envantage, Inc. 2009

32. Full Team Planning and Budgetary Review • Review budgetary requirements of laboratory • Justification for purchase • Competitive estimates of cost • Verify that timeline for receipt of purchased equipment or software meets project timeline Envantage, Inc. 2009

33. Value of Analytical Reference Samples • Obtain reference samples from the plant • Similar matrix and composition to expected samples • Sufficient volume for long term use by the lab • Begin statistical analysis of the reference materials • Analyze within plant lab on acquired instruments • Send to 2 or 3 outside laboratories currently running the same analytical methods Envantage, Inc. 2009

34. Value of Analytical Reference Samples • Build references into LIMS (if available) • Ensure off-spec results are flagged instantly • Ensure instrument performs optimally for actual unit samples • Facilitates adding actual samples later with similar method and specification requirements • Provides results in digital form for model tuning, etc. • Faciliates trend analysis on process unit performance Envantage, Inc. 2009

35. Value of Analytical Reference Samples • Useful for validating and monitoring performance • Both in plant laboratory and outside laboratories if used. • Provide trending information for deteriorating analytical system performance before inaccurate results are released • Ensures engineering receives accurate data everytime Envantage, Inc. 2009

36. Case Study 1 • Natural Gas Processing Platform in Asia • Designed without analytical chemist input • Sample points poorly chosen • Off-spec dewpoint gas sold to customer • Cost of Error: >$4, 000,000 Envantage, Inc. 2009

37. Case Study 2 • Virgin Naphtha Sales from US Refinery • Lab utilized ‘Modified’ Fast Analytical Method • Mis-identifed key naphthene component • Artificially lowered key pricing property (N+A) by over 12 Vol% • Cost to Refinery: >$5,000,000 per annum Envantage, Inc. 2009

38. Case Study 3 • Performance Test on Gas Platform • Attempt to increase process flowrate • Did not involve analytical chemists in planning of test • Wrong assumptions on sample composition shutdown all lab chromatographs on platform • Wrong sample phase collected, causing rupture and fire • Cost to Operator: $1,000,000+ Envantage, Inc. 2009

39. Case Study 4 • Novel reactor design by US Chemical Company • Included analytical chemists from start • Chemist pointed out issues with sample points locations and positions • Online instrument verified by horizontal and vertical material balances • Analytical instrument provided feed rate information when rotometer failed on unit • Cost to Company: $75,000 for Analytical Services • Value: Established a multimillion $ business stream Envantage, Inc. 2009

40. Conclusions • 1. The laboratory’s accuracy and precision requirements are driven by process control, their biggest customer • 2. This can lead to accuracy issues for submitted samples from planning and design engineering Envantage, Inc. 2009

41. Conclusions • 3. The laboratory should be considered an integral project team member from the start, not as an after thought • 4. The design engineers and unit operators must be willing to assist the lab chemists in developing an understanding of the process and equipment Envantage, Inc. 2009

42. Conclusions • 5. Project budgets should always take into account potential needs of the laboratory for additional equipment and software to ensure that they can meet the needs of the planning and design engineers • 6. Reference samples of similar matrix and composition should always be used to ensure ongoing proper method performance and accurate results Envantage, Inc. 2009

43. Conclusions • The costs of lack of planning and communication with the laboratory can and will exceed the small costs involved in providing budgetary monies for proper sample information, correct methods and instrumentation, and adequate analytical interpretation systems. Envantage, Inc. 2009