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Sample preparation of feeds and forage for NIR analysis

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Grain & Feed Milling Technology is published six times a year by Perendale Publishers Ltd of the United Kingdom. All data is published in good faith, based on information received, and while every care is taken to prevent inaccuracies, the publishers accept no liability for any errors or omissions or for the consequences of action taken on the basis of information published. ©Copyright 2010 Perendale Publishers Ltd. All rights reserved. No part of this publication may be reproduced in any form or by any means without prior permission of the copyright owner. Printed by Perendale Publishers Ltd. ISSN: 1466-3872 Digital Re-print - September | October 2011 Sample preparation of feeds and forage for NIR analysis www.gfmt.co.uk
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Page 1: Sample preparation of feeds and forage for NIR analysis

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Grain & Feed Milling Technology is published six times a year by Perendale Publishers Ltd of the United Kingdom.All data is published in good faith, based on information received, and while every care is taken to prevent inaccuracies, the publishers accept no liability for any errors or omissions or for the consequences of action taken on the basis of information published. ©Copyright 2010 Perendale Publishers Ltd. All rights reserved. No part of this publication may be reproduced in any form or by any means without prior permission of the copyright owner. Printed by Perendale Publishers Ltd. ISSN: 1466-3872

Digital Re-print - September | October 2011 Sample preparation of feeds and forage for NIR analysis

www.gfmt.co.uk

Page 2: Sample preparation of feeds and forage for NIR analysis

The 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 consider-ations focus on the quality and quantity of the components used in the production process.

This includes reliable analyses of feed-stuff 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

determination of protein content, moisture, fat and ash in feeds and forage.

The advantage over classical methods

such as Kjeldahl is the simultaneous deter-mination 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 prepara-tion. Users often face the problem of hav-ing to decide whether sample preparation is required or not.

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

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.

Sample preparation of feeds and forage for NIR analysis

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

Ground rabbit food pellets

Average 8.58 10.20 11.68 3.11 13.70

Standard deviation 0.07 0.23 0.34 0.03 0.18

Unground rabbit food pellets

Average 8.67 10.81 11.46 3.16 13.19

Standard deviation 0.10 0.15 0.59 0.03 0.13

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

Grain&feed millinG technoloGy18 | September - october 2011

FEATURE

GFMT11.05.indd 18 04/10/2011 15:14

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 sample’s 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 ingre-dients of the analyzed layers are over repre-sented 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 sam-ples 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.

Test series with different samplesThe 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

10 times, the spectrometer was refilled for every measure-ment.

The sam-ples were pulverized in Retsch’s cyclone mill Twister. This mill was spe-cially designed for sample preparation of food and feed for sub-sequent 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-

Grain&feed millinG technoloGy September - october 2011 | 19

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Contact us for more details:www.brukeroptics.com • www.tango-nir.com

Waiting is over.tango. anaLYsis to go.

Faster, simpler, more secure - with TANGO your NIR analysis speeds up. TANGO has exactly what users require of an FT-NIR spectrometer suitable for a feed analysis lab: robustness, high precision and straightforward operator guidance.

An intuitive user interface with touch screen operation makes the analysis of feed ingredients and finished feed available to everybody.

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GFMT11.05.indd 19 04/10/2011 15:15

Game Engineering Ltd has over the past 25 years, amassed the

experience required to carry out the design and installation of materials, processing and handling plants across a wide array of sectors including ; Animal & petfood, biomass & fuel generation, grain & seed, waste recycling and construction & quarrying.

Game have designed and installed numerous production plants over the years and made alterations for the major producers and built green field sites for the up and coming independent manufacturers. R aw m a t e r i a l s t o r a g e ; grinding ; mixing ; extruding and vacuum coating projects along with their control can all be undertaken by Game. “Our exper ience in th i s

industry is a guarantee of successful solutions to client’s requ i rement s , we work closely with major machine manufacturers t o p r o v i d e streamlined processes tailoring the design to the client’s budget and allowing for the future addition of equipment and processes as companies grow,” says the company. An example of a project which Game completed for a client consisted of a bulk storage block of six smooth walled bins (with a capacity of 60 cubic metres) , screw d i scharger s r ated at 20 tonnes per hour, weigh boat suspended under the bulk storage silos, discharge and transfer handling equipment

rated at 20 tonnes per hour, grinding system with twin one tonne live bins, mixing system and minor ingredients

and sack tipping station for adding sack additions directly into the mixing chamber, ex t ruder and pneumat ic conveying system suitable for transferring product to dryer at five tonnes per hour of wet product , dryer and conveying systems suitable for handling dried extrusions at four tonnes per hour, coater and screening and conveying systems suitable for handling dried extrusions and a cooler

and conveying systems suitable for handling dried extrusions at four tonnes per hour.The end result was a facility

that manufactured dry products to meet the ever-increasing product demand, with the clients range of dry pet foods stocked in most major supermarkets nationally.

More inforMation:Game Engineering LtdWitham St Hughs Business ParkWitham St HughsLincolnLN6 9TWUnited Kingdom

Tel: +44 1522 868021Fax: +44 1522 868027Email: sales @game-engineering.comWebsite: www.game-engineering.com

Game Engineering Ltd - 25 years of experience

News September - October 2011 NEWS

Grain&feed millinG technoloGy September - october 2011 | 7

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GFMT11.05.indd 7 04/10/2011 15:14

Page 3: Sample preparation of feeds and forage for NIR analysis

ground and unground samples hardly show any difference.

The results for wheat are different

The table shows a considerable discrepancy between ground and unground sample, par-ticularly 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.

The third analyzed sample is hay This sample shows a substantial dif-

ference for the average and the standard deviation of the protein content. This is because of the varying bulk density of the unground sample.

ConclusionNIR spectroscopy is a simple and suitable

method to determine a series of relevant parameters in forage and grain. The general opinion is that it doesn’t 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.

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

es through the hopper (with splash-back pro-tection) onto the rotor, which is rotating with high speed, and is thus submitted to preliminary size reduction. The sample is then thrown out-

wards by centrifugal accel-eration 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

More inforMation:Dr Andreas Theisen, Sales & Application, Retsch GmbH, Haan, Germany

Tel: +49 2129 /55610Email: [email protected], website: www.retsch.com

Table 2: The analysis of wheat grains shows a considerable difference in the ash and fiber content of the ground and unground sample

Parameter Ash Moisture Fiber content

Fat Protein

Ground wheat

Average 2.80 9.68 1.10 1.17 9.02

Standard deviation 0.03 0.09 0.05 0.03 0.07

Unground wheat

Average 0.10 9.80 6.90 1.38 8.46

Standard deviation 0.10 0.25 0.62 0.16 0.45

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

Ground hay

Average 9.53 5.70 28.56 1.36 6.17

Standard deviation 0.07 0.12 0.29 0.04 0.12

Unground hay

Average 9.31 6.25 26.26 2.44 9.94

Standard deviation 0.07 0.09 0.68 0.18 0.43

“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 doesn’t require any sample preparation”

Grain&feed millinG technoloGy20 | September - october 2011

FEATURE

GFMT11.05.indd 20 04/10/2011 15:15 GFMT11.05.indd 21 04/10/2011 15:15

Page 4: Sample preparation of feeds and forage for NIR analysis

GFMT11.05.indd 2 04/10/2011 15:14

The International Grains Program collaborates with industry organization to offer

HACCP certification and training on food safety in grain milling.

Grain milling professionals interested in answering the question of how to apply food safety practices and implement hazard analysis critical control points programs (HACCP) that specifically relate to grain milling can do so at the Grain Milling: Food Safety and HACCP workshop planned for October 11-13 at the Kansas State University International Grains Program (IGP) Conference Center.“This workshop is the result of a partnership between K-State, AIB International and the International Association of Operative Millers

(IAOM),” says Mark Fowler, IGP associate director and workshop coordinator. “We are excited to continue this unique workshop that both addresses the development of a HACCP program and fits the food safety needs of our participants from the grain processing industry.”During the workshop, participants will learn fundamentals of good manufacturing practices, sanitation schedules and HACCCP programs specifically related to the flour milling industry, and then apply this knowledge in designing a HACCP program for the onsite Hal Ross Flour Mill. According to Fowler, its curriculum caters to

both a USA and international

participants and emphasizes the importance of safe practices within the industry as a whole.Collaborating on this workshop for a third year has strengthened the relationship between the three

organizations and has allowed them to grow their audience, while still presenting the curriculum in a hands- on, interactive environment.“AIB International h a s a s t ro n g presence in food safety and the grain

science department has endless resources in grain processing and excellent facilities,” says Bill Pursley, vice president of food education for AIB International

and workshop presenter. “Combining those two factors with the access we have to IAOM’s extensive network, it allows us to offer a course that is really unique to the industry.”To enroll, go to www.aibonline.org. The course is listed under the seminars and courses header. Those interested in registering can also call AIB International at +1 800 242 2534.This class is just one example of the partnership courses offered through IGP. In addition to flour milling, IGP regularly offers short courses in feed manufacturing and grain management, grain marketing and risk management, and flour milling and grain processing. For more information about IGP programs, go to the IGP website at: www.grains.k-state.edu/igp.

Grain milling focuses on food safety and HACCP programs

For many years Flexicon Europe has maintained a dedicated test laboratory

to demonstrate the versatility and practicality of its bulk handling systems and show how it contributes to improved distribution of free-flowing and not-so-free-flowing materials to downstream processes or into intermediate storage hoppers.

Last month Flexicon Europe added a hydraulic Bulk Bag Conditioner to the recently expanded Test Facility at its production plant in Kent. The new equipment overcomes the problematical occurrence

facing many organisations when bagged bulk materials such as hygroscopic chemicals, certain types of spice blends, heat-sensitive products and many more have compacted and solidified during storage and shipment. They reach a point at which pneumatically actuated flow promotion accessories integral to bulk bag dischargers are inefficient or completely ineffective.The Bulk Bag Conditioner incorporates two hydraulic rams with specially contoured end plates, which gently press opposing sides of bulk bags reinstating a more free-flowing material state. Where more stubborn materials

are a regular occurrence Flexicon can equip the

Bulk Bag Conditioner with a hydraulically-actuated, variable-height turntable enabling in-frame bag rotation and conditioning at varying heights; the height of the turntable and the number of 90-degree rotations being user-adjustable.Having been treated in the Bulk Bag Conditioner loosened bulk solid material is then ready for induction into bulk bag unloaders with discharge through bag spouts.Measuring 2210mm high by 3378mm wide and 1981mm deep, the conditioner is designed to accommodate the most popular sized bulk bags. It is fully enclosed

on all four sides for operator safety and includes full-height doors that are interlocked preventing actuation when the doors are open.Visitors to the Flexicon Test Laboratory are now able to see the Bulk Bag Conditioner working alongside other Flexicon bulk handling systems such as the Company’s flexible screw and pneumatic conveyors, bulk discharger units and bag fillers. The functionality of the expanded test facility enables Flexicon to fully trial the handling of specific materials to maximise performance.

More inforMation:Website: www.f lexicon.co.uk

Big squeeze at Flexicon’s bulk handling test laboratory

News September - October 2011 NEWS

Grain&feed millinG technoloGy September - october 2011 | 9

GFMT11.05.indd 9 04/10/2011 15:14

For the first time Perendale Publishers Limited will host with GRAPAS a milling conference that is focused on rice, flour, cereals,

oilseeds and grain processing for Asia.

The GRAPAS Asia exhibition is co-hosted and co-locat-ed by Victam International to run alongside its VICTAM Asia and FIAAP Asia exhibitions. GRAPAS Asia is being held in Bangkok, Thailand from February 15 – 17, 2012 at BITEC – the Bangkok International Trade and Exhibition Centre. GRAPAS Asia will be complemented with a one-day conference for the grain processing sector.

Perendale Publishers Limited – the publishers of the International Milling Directory and the long-standing Grain and Feed Milling Technology magazine – is proud to be chosen as patron of this new conference. Perendale is also sponsoring the GRAPAS 2012 Award.

Keeping firmly in mind the need to provide informa-tion and new ideas in a timely and efficient way, the 2012 GRAPAS Conference will be held in two parts on one day

– the opening day of the exhibition – February 15, 2012; it will comprise independent morning and an afternoon ses-sions. Delegates can choose to attend either or both parts depending on their timetable and their interests.

“Establishing a new conference in these difficult eco-nomic times will not be easy. However, the expansion of Victam into related milling sectors, such as rice and pasta processing, means that a wider audience can benefit from technology presentations. We are keen to focus on topical issues of the day and keep the programme tight to deliver high value and quality information to industry professionals in a timely manner,” says Roger Gilbert who is organizing the event on behalf of GRAPAS.

“We will be providing a programme focused on address-ing issues facing the rice, flour and grain processing sectors in Asia.

“I’m proud that Perendale has been chosen as patron of the conference. We will be promoting the event widely and aiming to have in excess of 200 delegates in attend-ance. We are asking delegates to pre-register, for a small registration fee, so that we can accommodate speakers

and delegates accordingly, especially with translators, headsets and catering arrangements involved.”

The theme of the conference Guaranteeing food and feed safety through greater

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.

The conference will be in English with simultaneous translation into/from the Thai language.

Registration and further detailsFor an updated programme, please visit the conference

website to register http://conta.cc/nneulEThere is an early bird discount of 33% for all delegates

registering online prior to November 30, 2011.

Guest

- ED

ITO

R’S

OB

SER

VA

TIO

NS

Guest editor - Roger Gilbert

The GRAPAS Conference for Asia

Grain&feed millinG technoloGy

2 | September - october 2011

Are you a Perendale bookworm?Perendale Publishers Ltd, the publishers of Grain & Feed mIlling Technology, has set up an online Amazon-based ‘Book Shop’ that lets you browse a wide range of recently-published reports and books on Grain & Feed relaed topics. You will soon be able to read an extended review before making your selection and purchasing directly from Amazon.

We will undertake to put forward for your consideration the most recent publications and as a result become a reference point for your reading and research.

book store

Of course you will be charged for any books purchased, but you will be dealing directly with Amazon, which has a world-class ordering/payment gateway, packaging and mailing service.

Consult Perendale Publishers Online Book Store at:

www.perendale.com/books

GFMT11.05.indd 2 04/10/2011 15:14

Page 5: Sample preparation of feeds and forage for NIR analysis

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• Sample preparation of feeds and forage for NIR analysis

• 15-Year Celebration: Fortifying with folic acid prevents 22,000 birth defects annually

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October 2011

• Producing Flaked breakfast Cereals

• Direct Cold Plasma: The innovative answer to odour control in the food and feed industry

• Milling Technology Redefined

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