Predictive Quality Protocol

Protocol QUAL TESTS CEREALS (EXC OATS) & WR OILS 17-21

AHDB Recommended List (RL)

Market suitability predictive quality tests for cereals (except oats)and oil content of oilseed rape

Protocol

AHDB, Stoneleigh Park, Kenilworth, Warwickshire, CV8 2TL

Contents

1.Trials and varieties

2.Responsibilities

3.Predictive quality tests: cereals (excluding oats)

4.1Receipt and storage of samples

4.2Moisture content of samples

4.3Sample records

4.4Sample storage

4.5Preparation of samples prior to analysis

4.6Quality tests

4.6.1Specific weight

4.6.2Protein content

4.6.3Hagberg falling number

4.6.4Thousand grain weight

4.6.5Sieving fraction

4.Oilseed rape oil content

5.1Receipt and storage of samples

5.2Preparation of samples prior to analysis

5.3Oil content tests

5.Submission of data

Appendix 1 - RL tests and NL tests for RL purposes with (approximate) example test numbers

Predictive quality tests for cereals (except oats) and oilseed rape oil content tests

1.Trials and varieties

This protocol details the basic and predictive quality tests used for RL variety evaluation for cereals (except oats, which are under a separate contract) and oilseed rape oil content. Laboratories are invited to tender for this work which starts from August 2016 and continues until November 2021 (covering harvests 2017 to 2021).

Whilst most of the tests are on samples from RL trials, some are undertaken on samples from BSPB National List trials for RL purposes.

Provisional details of trials and varieties and the tests required will be supplied by the Trials Coordinatorin May with a final list of test requirements prior to the commencement of harvest.

2.Responsibilities

Cereal samples are taken from field plots, either from trials or from plots specially grown for the purpose. Oilseed rape samples are taken from yield plots. Arrangements for the collection of these samples, labelling and the provision of suitable bags is the responsibility of the RL Trials Coordinator.

3.Predictive quality tests: cereals (excluding oats)

It is the responsibility of the trial manager to ensure that the samples are taken according to protocol, dried (if necessary) to a moisture content at which they can safely be stored and then stored in dry conditions, free from contamination by pests and any contaminants that may render the samples unusable. It is also the responsibility of the trial manager to ensure that the samples are transported without damage or loss to the testing laboratory when required.

It is the responsibility of the testing laboratory to receive the samples and to store them in suitable conditions in readiness for the tests.

After use for grain quality testing, some samples may be selected for further testing by end-users (for example barley samples for micromalting by MAGB labs) and the cost of handling and transportation of these should be included in cost assumptions (assume 20 sets of samples will need to be handled in this way).

4.1Receipt and storage of samples

On the receipt of samples spot-checks should be carried out toensure that the grain is:

• At a moisture content suitable for storage i.e. 12% moisture content for barley and 15% for other cereals. This check can be carried out using an electronic moisture analyser.See 3.1.

• Well-filled and in good condition. They should be free from physical defects and discolouration caused by any factor, such as damage by machine, pests, disease (especially moulds) and excessively hot drying. A record should also be taken of high numbers of green, broken, sprouted and/or very small grains, weed seeds, barley awns, unthreshed ears, dirt, straw and other debris.

4.2Moisture content of samples

Whilst cereal samples should be at a suitable moisture content when received by the laboratory, it may be necessary to dry some samples. If this is the case this should be carried out straight-away and the fact reported to the RL Trials Coordinator. This should be included in your cost assumptions (assume 5 sets of samples need to be dried from 15% to 12%).

4.3Sample records

The samples received should be checked against the list of those required. If any samples are missing or the quantity supplied is incorrect this should be reported to the RLTrials Coordinator immediately. A record should be kept, detailing the date the samples are received, their condition and any shortfall, such that the information can be made available quickly on request to any member of the RL Team.

4.4Sample storage

Samples should be stored in stored in dry, pest-free conditions; an application of an approved pesticide may be necessary (subject to risk-assessment) when all of the samples are present in the store to prevent insect infestation.

Only trials that have been validated by the RL Trials Coordinator should be used for tests. Notification of validation will be by e-mail.

4.5Preparation of samples prior to analysis

The samples should be cleaned to remove combining debris such as straw, chaff, unthreshed ears and weed seeds. The cleaning may be by hand or with hand-held or mechanical sieves.

The top screen size should be of a suitable size to remove unthreshed ears and large debris.

The following bottom screen sizes should be used for cereals: 2.0mm.

4.6Quality tests

The tests conducted on each trial series is shown in appendix 1 and the number of tests conducted in 2015 is shown (as an example for quotation purposes) in Appendix 2.

a. Control tests

These tests are used to assess the suitability of the samples for further end-user tests (e.g. by BRI Campden and nabim).

Wheat (all controls tested)

Protein content

Hagberg falling number

b. Market suitability and grain quality tests

Specific weight

Protein content

Hagberg falling number

Thousand grain weight (wheat NL2 varieties only)

Sieving fraction

4.6.1Specific weight

This can be determined using a chondrometer, Dickey-John analyser or by approved NIR methodology.

4.6.1.1 Chondrometer

The chondrometer has two compartments divided by a slide. The lower compartment is of a known fixed volume (usually 1 litre) and is removable. The upper compartment has greater capacity.

The slide is put in place while the upper chamber is filled with grain. The slide is then removed quickly, allowing the lower compartment to fill after which the slide is re-inserted. The weight of grain trapped in the lower compartment is measured and converted into kg/hl using conversion tables.

4.6.1.2 Dickey-John analyser

The Dickey-John analyser must be usedaccording to the manufacturer's instructions. The instrument must be calibrated annually and possess a current ‘Certificate of Calibration’.

4.6.1.3 NIR fitted with a Test Weight Unit

The use of an NIR instrument fitted with a test weight unit is permitted for the measurement of specific weight. The operator must also participate in the monthly UK Grain Network ring checks for the various species being evaluatedto demonstrate that the instrument and operating practices are performing within specification. Records of the results of the monthly ring checks should be available for inspection if required.

Correction of specific weight data for moisture content

In the case of wheat, adjustment has to be made to the kg/hl value to take account of moisture content. The calculation procedure for this is as follows:

Add 0.35 kg/hl for each 1% moisture above 15%.

Subtract 0.35 kg/hl for each 1% below 15%.

In the case of barley and oats, no adjustment should be made to the kg/hl value to take account of moisture content.

4.6.2Protein content

Hammer milling of grain prior to analysis

The mill must be a hammer mill fitted with a 1mm screen. 300g of sample is milled and the material must be totally removed from the receptacle. The sample must be spread thinly, either with a printer’s roller or with a wide blade spatula. The sample must be re-formed into a pile and the process repeated four times. After mixing, a representative sub-sample must be taken in the following manner:-

A sample jar of 250ml capacity should be filled in small stages re-mixing the bulk between stages and blending each stage within the jar.

The sample jar must be filled and then sealed with a close fitting lid.

Determination of Crude Protein or Total Nitrogen Content

Determination of Crude Protein or Total Nitrogen Content may be by International Standard chemical method, recognised by competent authorities (IGB, AOAC, ISO, etc.) and which makes direct measurement of nitrogen content. The instrumentation used should be capable of analysing sample sizes greater than 0.5g.

Systematic errors in Kjeldahl nitrogen analysis must be controlled by the inclusion of blank analyses and by the analysis of a suitable analytical standard (Ammonium Sulphate, Methionine in a suitable bulking agent) for which the nitrogen content is known.

Instrument drift in Dumas nitrogen must be controlled by standardisation against a suitable analytical standard (EDTA, Glycine), for which the nitrogen content is known.

Alternatively FOR WHEAT ONLY an approved NIR methodology (ICC Recommendation No 202) can be used, provided that the instrument uses current UK NIR Network calibrations. The operator must also participate in the monthly ring checks for the various calibrations being used to demonstrate that the instrument and operating practices are performing within specification. Records of the results of the monthly ring checks should be available for inspection if required.

Quality assurance of the analytical procedures must include regular analysis of a suitable test material - for example, a sample of flour or grain maintained for that purpose.

4.6.3Hagberg falling number

The ICC Standard Method No 107 should be used.

4.6.4Thousand grain weight

The weight of a representative 1000 grains at 85% dry matter from a cleaned grain sample is recorded.

4.6.5Sieving fraction

A minimum of 100 grams of harvested grain, with large debris and weed seed removed, is passed over the following sieve sizes:

2.0 mm

2.2 mm

2.5 mm

2.8 mm

The % of grain remaining on each sieve is recorded by the operator and reported as:

Sieving % grain < 2.2 mm

Sieving % grain < 2.5 mm

Sieving % grain < 2.0 mm

Sieving % grain 2.0 - 2.2 mm

Sieving % grain 2.2 - 2.5mm

Sieving % grain 2.5 – 2.8 mm

Sieving % grain > 2.8 mm

4.Oilseed rape oil content

5.1Receipt and storage of samples

It is the responsibility of trial managers to ensure that one sample per yield plot is collected and dried to 0% moisture content before being bulked together with equal amounts of the dried seed from the other replicates of the same variety and sealed in an airtight polythene bag. The trial manager will arrange for the transportation of the samples to the nominated laboratory as soon as possible after harvest.

The dry matter and oil measurements should be conducted within 2 working days of being delivered as high moisture oilseed samples in polythene bags are prone to going mouldy very quickly. The availability of a cold store (5oC approx.) is an advantage.

Some trial operators appoint a sub-contractor to determine the dry matter content of the seed from their yield plots. In this case the dried samples will be sent by the sub-contracted laboratory. It will be an advantage if the laboratory has sufficient drying capacity to conduct the dry matter assessments on the samples from these particular trial operators.

It is the responsibility of the laboratory to receive and record the samples (checking against a list supplied by the RL Trial Coordinator). A record must be kept, noting the date the samples are received, their condition and the date and method of disposal after testing.

Any missing samples must be reported immediately to the RL Trial Coordinator so that action can be taken.

5.2Preparation of samples prior to analysis

Oil content tests should be conducted only on validated trials and the RL Trial Coordinator will advise the laboratory of this via email. Due to the volume of work and the need to conduct oil content tests quickly it is accepted that if the laboratory has conducted the dry matter assessments the oil content analyses may be conducted immediately afterwards (i.e. before validation) to reduce the need for re-packaging and re-drying at a later date.

5.3Oil content tests

All analyses must be carried out on material which has been re-dried in an oven at 100C +/-4C for a minimum of 2 hours (except where the oil content analysis is conducted immediately after the dry matter assessment) this is to eliminate any moisture taken up during packaging, transport and unpacking stages. It may be necessary to clean the samples prior to conducting the oil content analysis. This is usually required where seed samples contain a significant amount of combine debris and weed seeds and is best carried out using a small air suspension seed cleaner rather than sieves.

Oil content analysis must be performed using continuous emission NMR following ISO 5511:1992. The instrument should be fitted with a magnet assembly which can utilise Nessler tubes which can accommodate 30g of calibration oil. The instrument must be standardised using an appropriate pure oil sample of the crop being analysed (‘normal’ fatty acid profile type for each crop i.e. not HEAR or HOLL types) by the manufacturers multipoint calibration method. The fatty acid profile of the oilseed rape and linseed varieties will have been established at the National List testing level by Fatty Acid Methyl Ester (FAME) analysis and this information should be used to correct the oil content measurements conducted on HEAR, HOLL etc. types being analysed. Results are expressed as apparent oil as a percentage at 0% moisture.

The stability of the equipment is checked at two-hourly intervals through the working day by the use of weighed oil standards. A single determination is normally performed on each test sample.

NIR oil content analysis is not permitted.

5.Submission of data

Data must be submitted in a format defined by AHDB (normally MS Excel) to soon as possible after completion of the tests.

Only acceptable units and measure names should be used. These will be given in the workbooks.

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Appendix 1 - RL tests and NL tests for RL purposes with (approximate) example test numbers

‘* Tests on NL samples exclusively for RL purposes.

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