Digital Re-print - September | October 2011

Sample preparation of feeds and forage for NIR analysis

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FEATURE Whereas an inhomogeneous sample leads to systematic errors in the subsequent analysis, a sample, which is too coarse causes statistical errors. This will be explained in the following. The penetration depth of NIR radiation in grain or forage is up to 1mm, measured in diffuse reflection. Thus, the composition of the samples deeper layers is not detected. That is not a problem if the sample/pellet is homogeneous in itself. When examining pellets coated with fat or grains and seeds, however, the ingredients of the analyzed layers are over represented in relation to the complete sample. If the material is homogeneous but does not have the required analytical fineness, the surface actually analysed is reduced. This is due to the fact that the light inside the sample is scattered and not returned back to the detector. The same happens with light, fibrous samples with a low bulk density. As this effect is influenced by the filling level of the sample container and the surface actually analyzed, the statistic error is rather big in such cases. 10 times, the spectrometer was refilled for every measurement. The samples were pulverized in Retschs cyclone mill Twister. This mill was specially designed for sample preparation of food and feed for subsequent NIR analysis. In the Twister size reduction is effected by impact and friction between the rotor and the friction surface of the fixed grinding ring. The feed material pass-

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Sample preparation of feeds and forage for NIR analysis

by Dr Andreas Theisen, Sales & Application, Retsch GmbH, Haan, Germany

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Test series with different samples

he feed quality has a decisive influence on the productivity of livestock farming. However, high-quality forage considerably adds to the costs of stock breeding. Consequently, economic considerations focus on the quality and quantity of the components used in the production process. This includes reliable analyses of feedstuff and ingredients from receipt of goods to final inspection as the best way to ensure a balanced feeding of the animals while keeping cost and profit orientation in focus. Near Infrared Spectroscopy (NIR) is the most important analytical method for the

Table 1: The measurement results of various parameters in ground and unground rabbit food pellets only show slight differences

Parameter

Ash

Moisture

Fiber content

Fat

Protein

The different properties of ground and unground samples when analysed with NIR are demonstrated exemplarily with three different materials: rabbit food pellets, wheat grains and hay. The samples were analyzed

Te Fa E-

Ground rabbit food pellets Average Standard deviation Average Standard deviation 8.58 0.07 8.67 0.10 10.20 0.23 10.81 0.15 11.68 0.34 11.46 0.59 3.11 0.03 3.16 0.03 13.70 0.18 13.19 0.13

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Unground rabbit food pellets

determination of protein content, moisture, fat and ash in feeds and forage. The advantage over classical methods

such as Kjeldahl is the simultaneous determination of several parameters. Moreover, NIR spectroscopy is a quick method, which requires neither consumables nor reagents. Therefore it is used whenever high sample throughput and great flexibility are required. The identification and qualification of raw materials as well as the quantitative analysis of convenience products can be carried out within seconds to guarantee highest product quality and safety. A much discussed issue related to NIR analysis is the necessity of sample preparation. Users often face the problem of having to decide whether sample preparation is required or not.

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What does sample preparation for NIR analysis involve?

Sample preparation for NIR does not require digestion or extraction; it is mainly about size reduction of the sample material. This involves two aspects: 1. Homogenising the sample 2. Achieving the required grind size
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Figure 1: Fiber content of the ground (blue) and unground (green) wheat sample resulting from 10 measurements. The analysis of the unground sample clearly shows a systematic as well as a considerable statistic error.
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FEATURE

NIR spectroscopy is a simple and suitable method to determine a series of relevant parameters in forage and grain. The general opinion is that it doesnt require any sample preparation
Table 2: The analysis of wheat grains shows a considerable difference in the ash and fiber content of the ground and unground sample

ground and unground samples hardly show any difference.

Parameter

Ash

Moisture

Fiber content

Fat

Protein

The results for wheat are different

The table shows a considerable discrepancy between ground and unground sample, particularly with regards to ash and fiber content. This is due to the fact that only the surface of the unground wheat grains is analysed resulting in an over representation of the kernel shell.

Ground wheat Average Standard deviation Average Standard deviation 2.80 0.03 0.10 0.10 9.68 0.09 9.80 0.25 1.10 0.05 6.90 0.62 1.17 0.03 1.38 0.16 9.02 0.07 8.46 0.45

Unground wheat

The third analyzed sample is hay

This sample shows a substantial difference for the average and the standard deviation of the protein content. This is because of the varying bulk density of the unground sample.

Table 3: The analysis of hay shows a strong difference in the protein content and standard deviation between ground and unground sample

Parameter

Ash

Moisture

Fiber content

Fat

Protein

Conclusion
Ground hay Average Standard deviation Average Standard deviation 9.53 0.07 9.31 0.07 5.70 0.12 6.25 0.09 28.56 0.29 26.26 0.68 1.36 0.04 2.44 0.18 6.17 0.12 Unground hay 9.94 0.43

es through the hopper (with splash-back protection) onto the rotor, which is rotating with high speed, and is thus submitted to preliminary size reduction. The sample is then thrown outwards by centrifugal acceleration and is pulverized between rotor and grinding ring. The two-step grinding ensures particularly gentle but fast processing so that the feed material only remains in the grinding chamber for a very short time. The integrated cyclone provides cooling of

the sample and the grinding tools which helps to preserve the moisture content. The sample properties to be determined are not altered in any way. The ground material is separated in the cyclone and collected in a sample bottle. The cyclone mill Twister is also suitable for processing large numbers of different materials as no cleaning between samples is required. The quantitative measurements were carried out with the NIR spectrometer TANGO from Bruker Optik GmbH. The first sample to be analysed was rabbit food pellets. The measurement results of the

NIR spectroscopy is a simple and suitable method to determine a series of relevant parameters in forage and grain. The general opinion is that it doesnt require any sample preparation. The results presented in this article show, however, that it does make a difference if the samples are ground in a suitable laboratory mill before being analysed, particularly if they are inhomogeneous. Only then is it possible to guarantee meaningful and reliable analysis results. More
inforMation:

Dr Andreas Theisen, Sales & Application, Retsch GmbH, Haan, Germany

Tel: +49 2129 /55610 Email: mk@retsch.com, website: www.retsch.com

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Guest - EDITORS O
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headsets and catering arrangements involved. The theme of the conference Guaranteeing food and feed safety through greater NEWS September - October 2011 ews use of technology in the control of product quality at each step of the milling process, from raw material collection-through processing-to-product dispatch. Grain milling focuses on food safety and HACCP programs both a USA and andwith simultaneous The conference will be in English work shop presenter. Combining those two factors international Keeping firmly in mind the need to provide informa- translation into/from the Thai language. hetion and new ideas in a timely and efficient way, the 2012 International Grains (IAOM), says Mark Fowler, participants and emphasizes the with the access we have to IAOMs Program collaborates with be held in two parts on one day Registration and further within GRAPAS Conference will IGP associate director and importance of safe practices details extensive network, it allows us to offer a course that is really unique industryopening dayto offer exhibition February 15, 2012; are the industry as a whole. organization of the workshop coordinator. We it For an updated programme, please visit the conference the Collaborating on http://conta.cc/nneulE HACCP certification and independent excited to continue this unique website to register this workshop to the industry. will comprise training on morning and an afternoon sesworkshop that both addresses for a third year has strengthened of To enroll,all delegates food safety in grain milling. can choose to attend either or both parts There is an early bird discount 33% for go to www.aibonline. sions. Delegates the relationship between the three the development of a HACCP registering online prior to Novemberorg. 2011. 30, The course is listed under depending on their timetable and their interests. organizations and the seminars and courses header. Grain milling professionals program and fits the has allowed them to Those interested in registering interested in answering the question food safety needs of grow their audience, can also call AIB International at of how to apply food safety practices our participants from while still presenting +1 800 242 2534. and implement hazard analysis the grain processing the curriculum in a This class is just one example of critical control points programs industry. Perendale Publishers Ltd, the publishershands- on, interactive the partnership courses offered of Grain & Feed mIlling Technology, (HACCP) that specifically relate to During the workshop, has set learn through IGP. In addition to flour environment. grain milling can do so at the Grain participants will up an online Amazon-based Book Shop that lets you browse a wide range of AIB books on Grain milling, relaed Milling: Food Safety and HACCP fundamentals of good recently-published reports and International & Feed IGP regularly offers short topics. You will h a s a review before making workshop planned for October manufacturing practices, soon be able to read an extended s t r o n g courses in feed manufacturing your selection and purchasing directly from Amazon. food and grain management, grain presence in 11-13 at the Kansas State University sanitation schedules and safety and the grain marketing and International Grains Program (IGP) HACCCP programs We will undertake to put forward for your consideration the most recent risk management, specificallypublications and as a resultscience department has endless and flour milling and grain related to the flour milling Conference Center. become a reference point for your reading and This workshop is the result of a industry, and then apply this knowledge resources in grain processing processing. research. partnership between K-State, AIB in designing a HACCP program for the and excellent facilities, says Bill For more information about IGP International and the International onsite Hal Ross Flour Mill. According Pursley, vice president of food programs, go to the IGP website Association of Operative Millers to Fowler, its curriculum caters to education for AIB International at: www.grains.k-state.edu/igp.

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