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BRUINS INSTRUMENTS. Training Near Infrared Transmission Whole Grain Analyzer. Targets:. History and Basics of NIR Calibration development Toubleshooting & Maintainance. History of NIR. First detected by William Herschel beginning of 19th century

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Bruins instruments

BRUINS INSTRUMENTS

Training

Near Infrared Transmission

Whole Grain Analyzer

BRUINS INSTRUMENTS


Targets
Targets:

  • History and Basics of NIR

  • Calibration development

  • Toubleshooting & Maintainance

BRUINS INSTRUMENTS


History of nir
History of NIR

  • First detected by William Herschel beginning of 19th century

  • First instrument built by W.W. Coblentz about 1900

  • First practical use in the 1930s

  • First agriculture usage by Karl Norris 1968

  • First commercial scanning instruments 1978

  • First BRUINS NIR spectrophotometer 1979

  • First BRUINS NIT spectrophotometer 1982

BRUINS INSTRUMENTS


Basics of nir
Basics of NIR

NIR = Near InfraRed Spectroscopy

Wavelength of Light

UV > VIS > NIR >(M)IR

nm 380 750 / 1100 2500

(NIT / NIR)

Energy of Light

BRUINS INSTRUMENTS


Basics of nir1
Basics of NIR

Typical properties analysed by NIR are

organic compounds like

Oil

Protein

Starch

And

Water

Useful concentration are in % range,

ppm or ppb level are normally impossible.

BRUINS INSTRUMENTS


Basics of nir2
Basics of NIR

  • NIR active groups

O-H Water, Alcohol

C-H Carbohydrates (Starch, Sugar, Cellulose)

Fat / Oil

N-H Protein

BRUINS INSTRUMENTS


Basics of nir3
Basics of NIR

Molekular Vibrations

O

H

H

BRUINS INSTRUMENTS


Basics of nir4
Basics of NIR

Molekular Vibrations

BRUINS INSTRUMENTS


Basics of nir5
Basics of NIR

Molekular Vibrations

BRUINS INSTRUMENTS


Calibration
Calibration

  • Reference Analysis

  • Sample selection

  • Sampling

  • Sample Preparation / Homogenisation

  • Sample Presentation

BRUINS INSTRUMENTS


Calibration reference analysis
Calibration: Reference Analysis

  • NIR calibration will be dependend from reference analysis, so

  • Select best possible method

  • Investigate „real“ method error

  • Make sure that the same sample material will be analysed

  • Use at least double analysis

  • Comment all specialities of actual sample

BRUINS INSTRUMENTS




Calibration sample selection
Calibration: Sample Selection

  • The complete interesting concentration range must be covered by calibration samples.

  • The calibration set must also include samples with changes from other constituents, eg. low protein with high moisture, low protein with low moisture etc.

  • Further samples must be included which are representing influences from climate, soil, cultivars etc.

  • Due to the effect of temperature to NIR also cold and warm samples should be added.

BRUINS INSTRUMENTS


Calibration sampling
Calibration: Sampling

  • The sample must be representative for the total amount.

  • Take subsamples from different locations.

  • Thoroughly mix these to get a homogene sample.

BRUINS INSTRUMENTS


Calibration sample preparation
Calibration: Sample Preparation

  • No extra preparation needed for most grain and oil seeds.

  • Samples with thick shell must be ground (e.g. sunflower seeds).

  • The same sample preparation must be used for calibration and routine analysis.

  • By grinding a sample the moisture content will decrease.

  • Select the best grinder to reduce this moisture loss.

  • If a grinder with a sieve will be used, control the size of the mesh.

BRUINS INSTRUMENTS


Calibration sample presentation
Calibration: Sample Presentation

  • OmegAnalyzer and AgriCheck uses the NIR transmission, so for such meal the MultiCheck will be the better choice

  • As an alternative, but less efficient, a micro sample cup for meal or powders can be used

BRUINS INSTRUMENTS


Calibration sample presentation1
Calibration: Sample Presentation

In all cases, if fine powder or ground sample:

  • Thoroughly mix the sample before filling

  • In cases of components with different density make sure, that no material separate

    If a micro sample cup is used:

  • Make sure that the sample is filled without wholes

  • Knock a bit, that the sample will slide together, but not to often because different components may separate

BRUINS INSTRUMENTS


Calibration standardisation
Calibration: Standardisation

Before using the instrument in routine, it must be compared against the reference method with a set of samples.

These samples should cover the range of concentrations and normal variations in moisture, area and genotypes.

In order to get a good adjustment, the sample must be well mixed that the same material will be analysed with both methods.

The data for the reference analysis need to be well controlled, at least a double analysis must be performed.

BRUINS INSTRUMENTS


Calibration standardisation1
Calibration: Standardisation

The easiest comparison of accuracy and necessary adjustment can be made with Excel.

Just two columns need to filled , one with reference analysis the second with predicted NIR data.

Using the Excel functions for mean, standard error xy and correlation will calculate all necessary information.

Additional the Excel graph can be used to show how good the predicted values fit to the reference analysis.

BRUINS INSTRUMENTS


Calibration bias
Calibration: Bias

BRUINS INSTRUMENTS


Calibration bias1
Calibration: Bias

BRUINS INSTRUMENTS


Calibration bias2
Calibration: Bias

BRUINS INSTRUMENTS


Calibration bias 0 43 added
Calibration: Bias, 0.43 added

BRUINS INSTRUMENTS


Calibration bias3
Calibration: Bias

BRUINS INSTRUMENTS


Calibration slope
Calibration: Slope

While the bias will move all data parallel, the slope will change the extreme values more than the values around the middle.

So adjusting the slope will much more influence the predicted result.

For the slope adjustment the sample set must really cover the full calibration range.

Normally this adjustment should not be used. If it seems to be necessary, look for the reason. It might be better to select or built another calibration.

BRUINS INSTRUMENTS


Calibration slope1
Calibration: Slope

BRUINS INSTRUMENTS


Calibration slope2
Calibration: Slope

BRUINS INSTRUMENTS


Calibration corrected slope
Calibration: corrected Slope

BRUINS INSTRUMENTS


Calibration corrected slope1
Calibration: corrected Slope

BRUINS INSTRUMENTS


Calibration slope3
Calibration: Slope

BRUINS INSTRUMENTS


Calibration slope4
Calibration: Slope

BRUINS INSTRUMENTS


Calibration slope5
Calibration: Slope

BRUINS INSTRUMENTS


Calibration corrected slope2
Calibration: corrected Slope?

BRUINS INSTRUMENTS


Calibration corrected slope3
Calibration: corrected Slope?

BRUINS INSTRUMENTS


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