1. Iowa State University Grain Quality Lab Quality Control Maureen Suryaatmadja Graduate Research Assistant Agricultural Engineering Iowa State University February 14, 2005

2. Quality Control Items Daily NIR check sample Instrument Duplicates Equipment Check and Periodic Check of other instruments

3. Daily NIR Check Sample

4. Objectives to maintain the performance of the instruments to make sure that the instruments are stable to collect data as a part of NIRS research

5. Materials Grain corn (20030149) Grain soybeans (20030688) Thermometer Infratec 1225, 0065 Infratec 1229, 243108 Infratec 1229, 553075 Infratec 1229, 553792 Infratec 1241, 12410350 NIR System 6500, 3117 Perten DA 7200, 020102

6. Continue Perten 9100, 3170 Omega G, 106118 Omega AC, 301002 Omega G, 6110 Omega S, 201101 Zeltex 800,16125 Zeltex 800,16131 Zeltex 800,16179

7. Procedures Follow the procedures of every instrument (each instrument has slightly different procedures) Collect and record the data in the book and spreadsheet Build the control chart Make a 20 point moving average trend line Samples are changed periodically Data log is used to record other events

8. Control Charts Calculate mean, upper control limit and lower control limit. Upper and lower control limits were set according to this formula:

9. Data and Results The result summary \\Grainbin\QCData\QC Daily Check\Daily Check SummaryDaily Check Summary The data and the control charts for each instrument \\Grainbin\QCData\QC Daily Check\qc IT1225 00650065 \\Grainbin\QCData\QC Daily Check\qc IT1229 243108243108 \\Grainbin\QCData\QC Daily Check\qc IT1229 553075553075 \\Grainbin\QCData\QC Daily Check\qc IT1241 1241035012410350 \\Grainbin\QCData\QC Daily Check\qc NIRSystem 6500 31173117 \\Grainbin\QCData\QC Daily Check\qc Omega AC 3100231002 \\Grainbin\QCData\QC Daily Check\qc Omega G 106118106118 \\Grainbin\QCData\QC Daily Check\qc Omega G 61106110 \\Grainbin\QCData\QC Daily Check\qc Omega S 201101201101 \\Grainbin\QCData\QC Daily Check\qc Perten 9100 31703170 \\Grainbin\QCData\QC Daily Check\qc Perten DA 7200 020102020102 \\Grainbin\QCData\QC Daily Check\qc ZX800 1612516125 \\Grainbin\QCData\QC Daily Check\qc ZX800 1613116131 \\Grainbin\QCData\QC Daily Check\qc ZX800 1617916179

10. Daily Check Summary (Infratec 1229 553075) Sample Number Avera ge (%) High (%) Low (%) St Dev (%) Range (%)Count CORN 20030149Protein8.579.007.900.151.10193 (07/29/04- present)Oil3.444.602.400.672.20193 Starch60.5362.0059.500.412.50193 Density1.281.311.240.010.06193 SOYBEANS 20030688Protein38.3840.4034.401.296.00216 (06/29/04- present)Oil17.9419.2017.000.672.20216

11. Example

14. Conclusion When the sample is used in short period, the collected data will be more accurate and easy to be analyzed From the control chart, some instruments have out of control data. These do not mean that the instruments are not stable. These may be caused by: Using the wrong sample Using the wrong calibration ID Inadequate grain Untrained operators

15. Instrument Duplicates

16. Objective to measure reproducibility over time and samples of the instruments that are used for service

17. Materials Corn grain from variety sources Soybeans grain from variety sources Infratec 1225, 0065 Infratec 1229, 243108 Infratec 1229, 553075 Infratec 1241, 12410350 Grainspec 5174 (through 2003)

18. Procedures Prepare the samples Set up instrument that will be used Set up data files Run the samples twice for every tenth sample, record the sample number and source Save the files Build the control chart for every instrument

19. Control Charts Control charts are built for differences between first and second measurement Calculate mean, UCL and LCL for the differences Upper and lower control limits were set according to this formula:

20. Data and Results The result summary \\Grainbin/QCData/duplicate summary/QC Duplicate SummaryQC Duplicate Summary The data and the control charts \\Grainbin/QCData/duplicate summary/2000/Corn/Duplicate Corn 2000Duplicate Corn 2000 \\Grainbin/QCData/duplicate summary/2000/Soybeans/Duplicate Soybeans 2000Duplicate Soybeans 2000 \\Grainbin/QCData/duplicate summary/2001/Corn/Duplicate Corn 2001Duplicate Corn 2001 \\Grainbin/QCData/duplicate summary/2001/Soybeans/Duplicate Soybeans 2001Duplicate Soybeans 2001 \\Grainbin/QCData/duplicate summary/2002/Corn/Duplicate Corn 2002Duplicate Corn 2002 \\Grainbin/QCData/duplicate summary/2002/Soybeans/Duplicate Soybeans 2002Duplicate Soybeans 2002 \\Grainbin/QCData/duplicate summary/2003/Corn/Duplicate Corn 2003Duplicate Corn 2003 \\Grainbin/QCData/duplicate summary/2003/Soybeans/Duplicate Soybeans 2003Duplicate Soybeans 2003

21. Duplicate Summary (Infratec 1229 553075, Soybeans) YearFactoraverageSDSD - Diffn 2000Moisture9.3422.4000.300523 Protein36.7121.8100.326523 Oil18.4670.8450.192523 Fiber4.9090.2920.124523 RR0.4240.8240.189483 Sum55.1791.6900.274523 2001Moisture12.2241.5340.24123 Protein35.4261.1760.24223 Oil18.5090.8820.17423 Fiber4.7850.1600.10123 RR0.6330.4850.19416 Sum53.9350.8760.20923

22. Continue YearFactoraverageSDSD - Diffn 2002Moisture10.0822.9840.605659 Protein37.2772.7190.624659 Oil18.4381.5510.347659 Fiber4.5760.2350.145659 RR0.3341.0690.298659 Sum55.6861.7530.449659 2003Moisture8.5701.8200.2901480 Protein37.9282.5110.2701480 Oil17.7911.6140.2101480 Fiber4.6440.1950.0601480 RRn/a 0 Sum55.7181.5300.2691480

23. Example

25. Conclusion The precision of the instrument will decrease when it is often used for service Reproducibility make variation in the measurement, specially when the instrument is used for many samples

26. Equipment Check and Periodic Check of Other Instruments

27. Objective To demonstrate that all equipment qualifies to be used to support research and service

28. Materials Equipment/TestMaterial Balance Checks (yearly and single point monthly)balances (8), a standard weight set Thermometer Checks (monthly) IR thermometer, a certified mercury thermometer, water, glass container, stove or oven Divider check (weekly) divider, plastic container (4), corn sample from NIR daily check, balance (Mettler Toledo SB16000) Seed counter Check (weekly) seed counter, a glass container, precounted corn and soybeans seed (100,200,300,400,500)

29. Continue Equipment/TestMaterial Water test of test weight cup (yearly) water, stove, glass container, quart kettle, pint kettle, Mettler PM4400 Grain test of test weight cup (weekly) corn grain sample, quart kettle, pint kettle, balance Seedburo 8800, hickory striker, GAC 2000, GAC 2100

30. Procedures Prepare the materials that will be used Read and follow the procedures of every instrument/equipment Record the result in the Lab Q/C book and spreadsheet Build an appropriate chart

31. Data and Results The data and results: \\Grainbin\QCData\Equipment Check\BalancesBalances \\Grainbin\QCData\Equipment Check\ThermometersThermometers \\Grainbin\QCData\Equipment Check\DividersDividers \\Grainbin\QCData\Equipment Check\SeedcounterSeedcounter \\Grainbin\QCData\Equipment Check\testwttestwt

32. Balance Check

33. Thermometer Monthly Check ISU # 23027665 14-985- 5E Type IR Mercury Date Known ( C ) Meas. ( C ) Differences ( C ) Meas. ( C ) Differences ( C ) Ave10096.43.699.650.35 Std Dev 1.18 0.19 CV (%) 1.220.19

34. Rotary Divider Weekly Check (10%)(20%)(30%)(40%) Total Percentage Ave (%) (%) Ave9.8019.9430.1740.0099.90 Std Dev0.230.330.240.270.04 CV (%)2.361.650.800.670.04

35. Rotary Divider Chart

36. Seed Counter Weekly Check DifferencesPercentage Known and Meas. Average-0.02 Std. Dev1.170.43

37. Seed Counter Chart

39. Water test of test weight cup (yearly) Date Water Wt (Quart)Deviation Water Wt (Pint)Deviation Average1102.124.02550.681.73 St Dev4.04 2.522.43 CV (%)0.37 0.46

40. Water test of test weight cup chart

41. Grain test of test weight cup (weekly) QuartPint GAC 2000 GAC 2100 Test Weight Test WeightMoisture Test WeightMoisture Test Weight Average58.3858.2013.2958.2012.9158.75 St Dev0.430.490.820.510.710.51 CV (%)0.740.856.150.875.460.87

42. Quart/Pint

43. GAC 2000/2100

44. Conclusion EquipmentConclusion Balances All the balances need to be checked annually for full scale and monthly at one point Thermometer Mercury thermometer is more accurate than IR thermometer IR thermometer need to be adjusted to get a better accuracy Need to be check monthly at various temperature (boiling water, refrigerator, room) DividerRotary divider shows a good accuracy Need to be checked monthly

45. Conclusion EquipmentConclusion Seed CounterSeed counter chart shows a bad variance curve Need to be checked annually for all samples and weekly for one sample Water test ofShow a quite big deviation test weight cupNeed to be checked annually Need operator training Grain test of Show that grain density decrease over time Need to change sample periodically (at least 1 year) Quart and Pint show almost a same value test weight cupGAC 2000 and 2100 shows a big difference Need to be done weekly

46. Future Works Make sure that every instrument/equipment in the lab has a right procedure, improve the procedure as needed Set the tolerance for each item of quality control Decide what action should be taken if data is out of tolerance