1、PUBLISHED DOCUMENT PD CEN/TR 15645-1:2008 Paper and board intended to come into contact with foodstuffs Calibration of the odour test Part 1: Odour ICS 67.250; 85.060 PD CEN/TR 15645-1:2008 This Published Document was published under the authority of the Standards Policy and Strategy Committee on 29
2、 February 2008 BSI 2008 ISBN 978 0 580 58769 6 National foreword This Published Document is the UK implementation of CEN/TR 15645-1:2008. The UK participation in its preparation was entrusted to Technical Committee PAI/11, Methods of test for paper, board and pulps. A list of organizations represent
3、ed on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Amendments/corrigenda issued since publication Date CommentsTECHNICALREPORT RAPPORTTECHNIQUE T
4、ECHNISCHERBERICHT CEN/TR156451 January2008 ICS67.250;85.060 EnglishVersion Paperandboardintendedtocomeintocontactwithfoodstuffs CalibrationoftheodourtestPart1:Odour Papiersetcartonsdestinsenentrerencontactavecles denresalimentairesEtalonnagedelessaideflaveur atypiquePartie1:Odeur PapierundPappevorge
5、sehenfrdenKontaktmit LebensmittelnKalibrierungderGeschmacksprfungTeil 1:GeruchundAroma ThisTechnicalReportwasapprovedbyCENon13August2007.IthasbeendrawnupbytheTechnicalCommitteeCEN/TC172. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Bulgaria,Cyprus,CzechRepublic,Denmark,Estonia,Finland, F
6、rance,Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,P ortugal, Romania,Slovakia,Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:r
7、uedeStassart,36B1050Brussels 2008CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.CEN/TR156451:2008:E2 Contents Page Foreword4 Introduction .5 1 Scope 6 2 Normative references 6 3 Terms and definitions .6 4 Principle7 5 Materials and reagents8 5.1 Gene
8、ral8 5.2 Base paper8 5.3 Spiking compound.8 5.4 Solvent 8 6 Equipment 8 6.1 General8 6.2 Micro-syringes .8 6.3 Glass flasks 8 6.4 Aluminium foil9 7 Preparation of calibration samples9 7.1 General9 7.2 Preparation of the spiking solutions .9 7.2.1 General9 7.2.2 Stock solution K (800 mg/l).9 7.2.3 So
9、lution K2 (40 mg/l) 10 7.2.4 Spiking solutions.10 7.3 Preparation of calibration samples10 8 Sensory tests .11 8.1 General test conditions.11 8.2 Sensory panel 11 8.3 Sample presentation .11 8.4 Sensory evaluation of odour 11 9 Test procedure for sensory panel12 9.1 General12 9.2 First step: Assessm
10、ent before training.12 9.3 Second step: Training of the panel13 9.4 Third step: Assessment after training.14 10 Data collection and reporting.15 10.1 General15 10.2 Data Format 15 11 Data analysis15 Annex A (informative) Experimental design for sample evaluation before training (Rep 1) .16 Annex B (
11、informative) Experimental design for sample evaluation before training (Rep 2) .17 Annex C (informative) Example of evaluation form for use during assessments (first step and third step) .18 Annex D (informative) Example of evaluation form for use during training (second step).19 CEN/TR 15645-1:2008
12、3 Annex E (informative) Experimental design for sample evaluation after training (Rep 1) 20 Annex F (informative) Experimental design for sample evaluation after training (Rep 2) 21 Annex G (informative) Example of data entry sheets for the first step .22 Annex H (informative) Example of data entry
13、sheets for the third step 26 Annex I (informative) Moods median test30 Annex J (informative) Tukeys Quick (Pocket) Test 33 Bibliography34 CEN/TR 15645-1:20084 Foreword This document (CEN/TR 15645-1:2008) has been prepared by Technical Committee CEN/TC 172 “Pulp, paper and board”, the secretariat of
14、which is held by DIN. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. CEN/TR 15645-1:20085 Introduction Paper and board, intended to b
15、e in contact with food, may have characteristic odour that can migrate via the airspace to the food packed in it. The purpose of testing the odour of paper and board is to establish whether the material to be tested possesses an inherent odour when kept at room temperature. In order to gain reliable
16、 results from the sensory evaluation, the performance of a sensory panel assessing the odour of paper and board needs to be validated. This can be implemented through a training procedure by using spiked calibration samples prepared according to the given instructions. This document consists of: pro
17、tocol to prepare the calibration samples (spiked paper) for sensory evaluation of odour; description of the training procedure for a sensory panel in the use of the calibration samples; instructions for sensory evaluation of calibration samples before and after training. This guide is meant to be us
18、ed in connection with the European Standard EN 1230-1. The guidance given in this document is only a recommendation. Please note that the calibration samples, the preparation of which is described, can be also applied in other ways than described in this document. This guide has been devised and col
19、laboratively tested in the context of the EU research project CALIBSENSORY (Growth programme, Measurement and Testing activity, GRD2-2000-30015) and it is the sole responsibility of its authors. It does in no way represent the views of the Commission or its services. Published results of the project
20、 are available at http:/www1.kcl.fi/euproj/calib.html . CEN/TR 15645-1:20086 1 Scope This Technical Report specifies a written protocol to prepare calibration samples for assessment of odour released by a paper or board sample, and how to train the panel in the use of these calibration samples. The
21、general outline of the testing procedure consists of sensory assessment of the odour samples without formal training by a selected panel, followed by training of the panel, and finally sensory assessment of the odour samples after training by the same sensory panel. 2 Normative references The follow
22、ing referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 5496, Sensory analysis Methodology Initiation and train
23、ing of assessors in the detection and recognition of odours ISO 6658, Sensory analysis Methodology General guidance ISO 8586-1, Sensory analysis General guidance for the selection, training and monitoring of assessors Part 1: Selected assessors 3 Terms and definitions For the purposes of this docume
24、nt, the following terms and definitions apply. 3.1 assessor any person taking part in a sensory test see ISO 5492:1992 3.2 base paper paper that has minimal number of sensory properties 3.3 calibration procedure protocol of calibration samples and written instructions to train selected assessors wit
25、h calibration samples i.e. calibrate the panel 3.4 calibration sample base paper that is spiked with spiking compounds at a certain concentration 3.5 control sample a hidden reference sample served blind coded to the assessors among the calibration samples, and prepared according to the procedure of
26、 the calibration samples but without the spiking compound CEN/TR 15645-1:20087 3.6 odour organoleptic attribute perceptible by the olfactory organ on sniffing certain volatile substances ISO 5492:1992 3.7 multicomparison test test where the assessor is asked to give a rating of the intensity of the
27、difference in taste or odour between test portions for analysis and a known reference sample 3.8 reference sample calibration sample without any spiking compound NOTE This is presented to the assessors labelled as “Reference“ and served to the assessors before the calibration samples. 3.9 selected a
28、ssessor assessor chosen for his/her ability to perform a sensory test see ISO 5492:1992 3.10 spiking compound a volatile chemical compound having a specific odour NOTE In this case hexanal is the selected spiking compound. 3.11 spiking method a method for spiking the base paper with spiking compound
29、s 4 Principle A training process validation for a sensory panel has to be conducted with freshly made calibration samples, prepared by spiking an odourless base paper with different concentrations of hexanal. The panel performance in evaluating the odour intensity of hexanal is determined before and
30、 after a formal training step. The effectiveness of training can then be determined. The test procedure consists of 3 steps: a) first step: assessment of calibration samples before training; b) second step: training procedure; c) third step: assessment of calibration samples after training. Detailed
31、 instructions for general test procedure, sample preparation and sensory evaluation are provided within this Technical Report, and must be carefully followed to ensure validity of results. CEN/TR 15645-1:20088 5 Materials and reagents 5.1 General Odourless base paper is used as a carrier for differe
32、nt concentrations of the spiking compound diluted with the solvent. In this Technical Report, hexanal is used as the spiking compound and triacetin as the solvent. 5.2 Base paper The base paper used in the odour test shall be suitable for food use. The paper shall respect the following criteria: odo
33、urless porous. One example for the base paper is coffee filter paper made of bleached chemical pulp, including wet strength resin and grammage of approximately 52 g/m 2 . 5.3 Spiking compound Hexanal (CAS number 66-25-1, 98 %) is used as the spiking agent in the odour test. The odour of hexanal is d
34、escribed as being green, fruity, bitter and grassy. Hexanal is often found in rancid fats (in foods) and in fibre- based materials. 5.4 Solvent Triacetin (CAS number 102-76-1) shall be used as a solvent for diluting the spiking compound. It is assessed to be almost odourless, and related to its othe
35、r characteristics, suitable for this purpose. 6 Equipment 6.1 General All equipment used shall be free from odour and only in use for sensory analysis (see ISO 6658). Special care is required to ensure that lids, seals and inserts do not become a source of odour. Equipment and glass flasks shall be
36、cleaned between sessions. Any glassware used shall be washed with minimum-odour cleaning agents and dried by placement in oven at a temperature 100 o C and left to evaporate for at least 2 h. All other equipment shall be washed with minimum-odour cleaning agents and left to dry at room temperature.
37、6.2 Micro-syringes Micro-syringes in capacity from 20 l to 100 l. 6.3 Glass flasks Glass flasks in 500 ml in capacity. The shape of the flask is not as essential as the volume. Brown glass bottles with lids of polytetrafluorethylen or Erlenmeyer flasks with narrow neck and conical ground joint and s
38、topper may be used. CEN/TR 15645-1:20089 The flasks (if needed) are covered by aluminium foil for preventing the influence of the appearance of the sample. Each sample is served to each assessor in a separate flask, therefore 5 flasks are required for each assessors at each session. 6.4 Aluminium fo
39、il Aluminium foil used for wrapping the glass flasks (if needed) shall be free from odour. 7 Preparation of calibration samples 7.1 General Prepare for each five sessions five samples: the reference sample plus four samples for assessment. These are summarised, along with their concentrations, in ta
40、ble 1. Table 1 Calibration samples and concentrations of hexanal (g hexanal/paper sample) sample g/sample reference 0 N 0 (control sample) 0 N 1 0,04 N 2 0,80 N 3 8,0 For the three spiked samples, base paper should be spiked at various concentrations of hexanal diluted in triacetin, the concentratio
41、ns being 0,04 g, 0,8 g and 8 g hexanal/sample. The reference (given reference) and control samples (hidden reference) shall be odour flasks with base paper and triacetin but without hexanal. For each of the five samples, the number of prepared test portions (flasks) has to be equal to the number of
42、assessors on the panel, the recommended panel size varying between 10 and 12. The flasks should be covered with aluminium foil and coded with three-digit random numbers prior to preparing the individual test portions. These have to be presented individually to each assessor. Examples for blinding co
43、des and experimental designs for each session are presented in the annexes. 7.2 Preparation of the spiking solutions 7.2.1 General The following sets of stock solutions will be needed. Stock solution K can be used over three consecutive days only. The other stock solution K 2 and the batch solutions
44、 for each sample have to be freshly made each day. 7.2.2 Stock solution K (800 mg/l) Dissolve 80 mg (100 l) of hexanal in about 50 ml of triacetin, then fill up with triacetin to make total volume of 100 ml. Stock solution K has to be stored at + 4 C, and can be used for three consecutive days. CEN/
45、TR 15645-1:200810 7.2.3 Solution K2 (40 mg/l) Dilute 1 ml of stock solution K in 20 ml of triacetin (i.e. 1 ml K/20 ml triacetin). Stock solution K2 has to be stored at + 4 C and shall be prepared daily. 7.2.4 Spiking solutions To create batch solutions for the spiked samples, dilute solution K 2 as
46、 presented in Table 2. Table 2 Preparation of batch solutions for spiking the calibration samples sample K 2 ml triacetin ml description N1 0,1 9,9 to create a batch of N1 solution, dilute 0.1 ml of K 2 stock solution with 9.9 ml triacetin N2 1 4 to create a batch of N2 solution, dilute 1 ml of K 2
47、stock solution with 4 ml triacetin K, ml N3 1 9 to create a batch of N3 solution, dilute 1 ml of K stock solution with 9 ml triacetin Sample batches for N1 to N3 shall be prepared daily. The reference and control samples, also presented to the assessors during the sensory assessment, will be prepare
48、d using triacetin without any added hexanal. 7.3 Preparation of calibration samples The sample flasks should be prepared in a completely odourfree space (see ISO 6658). To prepare the calibration samples the following scheme has to be followed: 1) Reference test paper must first be prepared by cutting into squares of 1 dm (10 cm 10 cm) cm. For each session, five pieces of test paper (each 1 dm) for each assessor (one for each sample) will be needed. 2) Reference test paper (1 dm) shall be folded in double thickness and bent in accordion style.
