trials on nir perten 2014
TRANSCRIPT
NIR Analyses in fishmeal An Icelandic Network
2014-03-27
Stefan Lundgren Perten Instruments AB
Perten Instruments Group
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
Our History Harald Perten, a cereal chemist, founded the company in 1962.
Analytical solutions for Agri Food Industries
Grain
Flour
Food
Feed
A long history in NIR
In 1980 Perten Instruments developed its first NIR instrument.
Global – Local
Icepack Ehf
Reykjavik
DA 7250 NIR Analyzer
• 6-second analysis
• Grains, slurries, powders and more
• No sample preparation
• SEE IT OUTSIDE!
DA 7300 Online NIR Analyzer
• Inline analysis
• Grains, pastes, powders and more
• Built-in camera
DA 7300 Online NIR Analyzer
• Over-belt analysis
• Grains, meals, powders and more
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
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
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
Moisture
Parameter SEC SEP R2 Range C-set V-set
Moisture 0.43 0.35 0.93 2.1-9.3 184 38
Protein
Parameter SEC SEP R2 Range C-set V-set
Protein 0.87 0.83 0.87 65.9-74.3 184 38
Fat
Parameter SEC SEP R2 Range C-set V-set
Fat 0.52 0.51 0.95 6.3-15.4 182 38
Ash
Parameter SEC SEP R2 Range C-set V-set
Ash 0.39 0.40 0.97 9.5-17.8 184 29
Salt
Parameter SEC SECV R2 Range C-set
Salt 0.31 0.55 0.97 2.2-8.4 53
TVN
Parameter SEC SEP R2 Range C-set V-set
TVN 1.9 1.9 0.92 0.7-30.0 123 24
Cadaverine
Parameter SEC SEP R2 Range C-set V-set
Cadaverine 109 218 0.96 100-1800 35 8
NIR Networks
•Basic Ideas
•Advantages
•An example
•Organisation
•Calibration Monitoring
• Standardisation
• Instrument Monitoring
•Costs
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’
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
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
NIR Network - Organisation
Calibration Center
Perten Applications
Group
Administration Center
NetPlus Network
Manager
Networked
Local instruments
Reference Laboratory
Master instrument
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
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
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
NIR Network - Standardisation
• The Master is validated and adjusted against reference analyses
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Reference lab DA7200 Master
NIR Network - Standardisation
• Individual instruments are adjusted against the Master via internet if needed
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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
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
NetPlus Reports
• Information on all reference samples is available for all participants in the network via internet
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
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
Questions?
Your partner in Agri Food Quality Control