This document discusses using near infrared (NIR) spectroscopy in a network to analyze fishmeal. Key points: - A trial at Matis in 2013 analyzed over 200 fishmeal samples for moisture, protein, fat, ash, salt, TVN, and cadaverine using a DA7250 NIR analyzer. New calibration models were developed that showed good results. - An NIR network involves accredited reference labs, standardized instruments calibrated to a "master" regularly, and web-based software to monitor instruments and share calibration models and reference data. - Benefits include uniform quality assurance, robust calibration models, lower analysis costs, and simplified implementation of standards across members. The proposed Icelandic network would be

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