Frá Vorráðstefnu FÍF 2014

1. NIR Analyses in fishmeal
An Icelandic Network
2014-03-27
Stefan Lundgren
Perten Instruments AB
Perten Instruments Group

2. AGENDA
• Briefly about Perten, really briefly...
• NIR Analyzers from Perten Instruments
• Parameters analyzed in Fishmeal by NIR
• Results from trial at Matis 2013
• NIR Networks

3. Our History
Harald Perten,
a cereal chemist,
founded the
company in 1962.

4. Analytical solutions for Agri Food Industries
Grain Flour Food Feed

5. A long history in NIR
In 1980 Perten Instruments
developed its first NIR instrument.

6. Global – Local
Icepack Ehf
Reykjavik

7. DA 7250 NIR Analyzer
• 6-second analysis
• Grains, slurries,
powders and more
• No sample preparation
• SEE IT OUTSIDE!

8. DA 7300 Online NIR Analyzer
• Inline analysis
• Grains, pastes,
powders and more
• Built-in camera

9. DA 7300 Online NIR Analyzer
• Over-belt analysis
• Grains, meals,
powders and more

10. Plus Platform overview
NetPlus
server
NetPlus - Reports
Reports on e.g. production
Production manager
NetPlus - Remote
Instrument performance
and configuration
Instrument manager
NetPlus - Application
Organize calibrations,
find data, export/import
Application specialist
Results Plus
Sample analysis, with GUI
Process Plus
Process analysis,
No GUI
Results Plus?
Future additions
Instrument software Browser software

11. NIR in Fishmeal – Analysis parameters
Parameter Unit Reference method
Moisture % by weight Drying Oven
Protein % by weight, as is Kjeldahl
Fat % by weight, as is Soxhlet
Ash % by weight, as is Ashing Oven
Salt % by weight, as is Titration
TVN
Cadaverine
mg/100g
g/kg
Steam distillation
HPLC

12. NIR in Fishmeal – Trial at Matis
• Some 200 samples were provided by SVN and Matis
• All samples were scanned on DA7250
• Analyzed for Moisture, Protein, Fat and Ash, using Perten’s global
calibration models
• Results were good but not optimal
• Matis provided samples with Salt and TVN values
• New calibration models were developed by Perten
• Feasibility study carried out on Cadaverine in Fishmeal

13. Moisture
Parameter SEC SEP R2 Range C-set V-set
Moisture 0.43 0.35 0.93 2.1-9.3 184 38

14. Protein
Parameter SEC SEP R2 Range C-set V-set
Protein 0.87 0.83 0.87 65.9-74.3 184 38

15. Fat
Parameter SEC SEP R2 Range C-set V-set
Fat 0.52 0.51 0.95 6.3-15.4 182 38

16. Ash
Parameter SEC SEP R2 Range C-set V-set
Ash 0.39 0.40 0.97 9.5-17.8 184 29

17. Salt
Parameter SEC SECV R2 Range C-set
Salt 0.31 0.55 0.97 2.2-8.4 53

18. TVN
Parameter SEC SEP R2 Range C-set V-set
TVN 1.9 1.9 0.92 0.7-30.0 123 24

19. Cadaverine
Parameter SEC SEP R2 Range C-set V-set
Cadaverine 109 218 0.96 100-1800 35 8

20. NIR Networks
• Basic Ideas
• Advantages
• An example
• Organisation
• Calibration Monitoring
• Standardisation
• Instrument Monitoring
• Costs

21. NIR Networks – Basic ideas
• Ensuring a uniform, fair and cost
effective form of quality assurance and
basis for payment
• A common accredited reference
laboratory
• Rapid analyses based on international
standard methods
• Easy-to-use analytical instruments with
identical specifications
• Minimized operator influence on
results
• ’Approved’ calibration models
• All instruments are compared to a
’Master Instrument’

22. NIR Networks - Advantages
• Centrally controlled calibration models and
reference analyses
• No local influence on results gives a uniform and fair
classification of products
• Simplified quality assurance for the users
• Calibration monitoring through the network using
web based software
• Daily check sample
• Powerful tool for implementing an Icelandic
standard
• Harmonized quality control on produced fishmeal

23. NIR Networks - Advantages
• Building a common sample database
• Better and more robust calibration models gives
reliable analysis results
• Few reference samples per network member
-> Lower analysis costs!
• Yearly updates
• Reduced development costs for new analysis
parameters and products, eg
• Cadaverine
• Raw materials
• Same calibration models used for both process
control and out-loading

24. NIR Network - Organisation
Calibration Center
Perten Applications
Group
Administration Center
NetPlus Network
Manager
Networked
Local instruments
Reference Laboratory
Master instrument

25. NIR Network - Organisation
• Steering Committee
• Representatives from users, reference laboratory and instrument
supplier
• Reference Laboratory
• Matis Laboratories
• Accreditations: ISO 17025, SWEDAC
• Certification in acc. With ISO 9001 och ISO 14001
• Controls:
• Ring tests in Iceland and Europe
• Third party revisons by customers
• Calibration Center
• Perten Applications Group – Stockholm / Matis Reykjavik
• Administration Center
• Matis Neskaupstadur
• Technical Support
• Perten Technical Group – Stockholm & Icepack - Reykjavik

26. NIR Network – Calibration Monitoring
• The Master Instrument is compared to reference
analyses at the accredited laboratory
• Samples are sent in by network members on a regular
basis
• Some 100 control samples collected from all
participating factories each year
• Results are available on the internet
• NetPlus Reports – Web based reports software
• Updated regularly with new samples

27. NIR Network - Standardisation
• The Master is validated and adjusted against reference
analyses
• The Reference Laboratory sends out reference samples once
a year for instrument control
• Typically 10 samples per product type
• Scanned on every instrument in the network
• Scans collected via internet by the Admin. Center
• Predicted results are compared to the Master
• Individual instruments are adjusted via internet if needed

28. NIR Network - Standardisation
• The Master is validated and adjusted against reference
analyses
9.8
9.9
10
10.1
10.2
10.3
10.4
10.5
Reference lab DA7200 Master

29. NIR Network - Standardisation
• Individual instruments are adjusted against the Master via
internet if needed
8,5
10,0
11,5
m
asterslave1slave
2
slave3
slave4
slave5
slave6
slave7
slave8
slave9slave10

30. NIR Network– Instrument monitoring
Continuous monitoring of instrument stability
• Instrument Self-Diagnostics
• Daily Check Samples
• Relevant sample material
• Synthetic sample (Polystyrene)
• Analyzed daily to confirm stability
• Statistics in Results Plus instrument software

31. NIR Network – Outlier handling
• ’Outliers’ during analysis
• Samples that deviate from samples in the calibration
sample database
• Spectral difference or difference in content (range)
• Sent to Reference Lab for chemical analysis
• Added to calibration sample database for updating
and improving calibration models

32. NetPlus Reports
• Information on all reference samples is available
for all participants in the network via internet

33. NIR Network – Costs
Network price for the instrument
• DA7250 NIR Analyzer: € 48 000
Annual fee
• Xx xxx ISK per instrument
Includes
• Yearly standardisation against Master instrument
• Specified number of reference analyses per year
• Updated calibration models
• Annual maintenance service of instruments
• Remote support via internet

34. NIR Network – Summary
Participating in an NIR Network cooperation
• Simplified and cost-effective quality assurance
• Increased credibility for NIR analyses
• Quality certified by accredited laboratory
• Reduced time spent and costs for upkeep of NIR
analyses for product controls
• Lower costs for developing new NIR analyses

35. Questions?

36. Your partner in Agri Food Quality Control