What s that funky smell from my product? EURL-FCM ISPRA 29th Nov 11

Transcription

1 What s that funky smell from my product? EURL-FCM ISPRA 29th Nov 11 1

2 The work of ISO TC146 for the standardisation of sensory tests A support for the accreditation of material odour testing Dr Olivier Noiset Consultant / Quality Manager 2

3 Certech in few words Research and Technology Organisation (RTO) OUR MISSION : To provide help, support and services to small and large industrial enterprises by offering ad hoc analysis and measurements, problem-solving, contract research, product and process development capabilities. 3

4 Certech in few words Markets 4

5 Certech in few words Automotive industry Building industry (WW) Existing labels : -Blue Angel (Germany) -GuT (Carpets, Germany/Europe) -M1 (Construction products, Finland) -ICL (Construction products, Denmark) -CSTB O labels (construction products) -Natureplus (Construction products, Germany/Europe) -Japanese regulations -Hong Kong Green Label Scheme -Greenguard (USA) Requirements based on standards : - VDA270 : smell test on parts - Volvo : Odour of trim materials in vehicles - Renault D493001: Emissions d odeurs - Toyota TSM0505G: test method for smell - NISSAN NES M0160: smell of interior parts - PSA D Ford : Odour test for trim materials Packaging industry Materials and articles shall not transfer their components to foodstuffs in quantities which could deteriorate its organoleptic characteristics 5

6 The starting point INDOOR AIR QUALITY - ISO / TC146 / SC6 What the Construction Products Directive (CPD) says ER 3 : The construction work must be designed and built in such a way that it will not be a threat to the hygiene or health of the occupants or neighbours, The construction works must provide a healthy indoor environment for occupants and building users, taking account of pollutants including: These may be the cause of undesirable effects, ranging from discomfort and nuisance to adverse physical effects on health. / / Mandate M/366 Dangerous substances Harmonised approach Horizonta l standard Odour No harmonised approach 6

7 The starting point What are the needs for Europe No barriers to trade Harmonised technical specifications Harmonised EN standard Declaration of conformity CEN ISO (liaison) marking 7

8 Main objections to harmonisation of sensory tests The rating of odour is subjective Poor reproducibility of quantitative measurements Most of the tests are not representative of realistic conditions Odour characterisation is complex (several parameters) No estimation of the global smell by adding single contributions (no additive rule for combined/composite materials) 8

9 The ISO/TC146/SC6 works : WG14 submitted the proposal of a material testing method for final vote. ISO DIS «Determination of odour emissions from building products using test chambers» WG 17 finalised the draft document and submit for CD ballot. ISO WD Sensory testing of indoor air 9

10 Specific technical requirements Management of all the parameters that affect the perception Quantitative method with better reproducibility Test under realistic conditions in order to extrapolate product contribution Possible evaluation of the global smell with several products Subjective rating (qualitative) disconnected from the objective (quantitative) rating 10

11 Existing standards GLP in sensory testing : general standards : ISO 5492, ISO 5496, ISO8589 Harmonised approach of building material testing : emission standards : ISO , ISO Existing protocols in the European labeling schemes : Odour assessments in M1 and AgBB Existing standards for odour characterization : EN13725, VDI3882, ISO 5496, etc 11

12 Harmonised approach includes the following requirements : Sensory testing room (compliant to ISO8589) HVAC : T : 25 C max ( max : 3 C) RH : 50% ± 5 20 l/s/pers No direct sunlight, no colours on walls (neutral) No noise No odour : acceptability 0,5 intensity 3-4 pi 12

13 Harmonised approach includes the following requirements : Odour emission test on materials based on ISO Low adsorption (electropolished SS) General requirements (dynamic) + Temperature control Specific requirements : Tightness Vötsch Industrietechnik VCE 100 No-emissive materials Moisture control Air purity - No visual contact with samples - Outlet flow rate shall be 0,3l/s to 1 l/s for a direct assessment (option 1) - No odour background : acceptability 0,8 intensity 2-3 pi 13

14 Harmonised approach includes the following requirements : Assessment of the odour sampled in bag : Material to be used induces low adsorption of the sampled odour (Tedlar, PVDF, FEP, nalophane, etc) N.B. For film applications, the bag could be made of the material itself. The sample has to be analysed the same day Sampling container is made of Tedlar. The material is to be heated for min 12 h at a temp. of 80 C before use. No odour background : acceptability 0,8 intensity 2-3 pi 14

15 Harmonised approach includes the following requirements : Assessment of the odour sampled in bag : An important source of discrepancy is the presentation of the smell to the nose. Diffuser made of electropolished stainless steel or glass with an opening angle of up to 8 ensures a homogeneous outflow of sample air. Odournet GmbH The minimum flow rate through a diffuser is 0,3l/s to 1 l/s in order to avoid air mixing and dilution of the smell with the ambiant air. 15

16 Harmonised approach includes the following requirements : Management of odour panels : These aspects of good sensory practices are the minimum requirements to reliable method and accuracy : Panel leader Panel selection Code of behaviour Panel size 16

17 Harmonised approach includes the following requirements : Management of odour panels Code of behaviour: It shall be known and approved by all the panel members the panel member shall be available for a complete measurement session; from 30 min before and during measurement panel members shall not be allowed to smoke, eat, drink (except water) or use chewing gum or sweets; panel members shall take great care not to cause any interference with their own perception or that of others in the odour rooms by lack of personal hygiene or the use of perfumes, deodorants, body lotions or cosmetics; panel members suffering of a cold or any other ailment shall be excluded from participating in measurements; panel members shall be present in the odour testing room 5 min before the measurements start in order to get adapted; panel members shall not communicate with each other about the results of their rating. 17

18 Harmonised approach includes the following requirements : Management of odour panels Panel leader : He is in charge of the entire process of sample preparation, measurement session, registration of vote and treatment of data. He never takes part to the rating. Before starting a session, the panel leader has the responsibility to check that the code of behaviour is applied by all the panel members. The panel leader has the responsibility of the whole process regarding the preparation of samples to be presented and the measurement session. He shall check that the samples are suitable for the purpose of the test. The panel leader shall explain to the panel members the aim of the test and present the expected time schedule. The panel leader shall manage the assessment and registration of data in such a way that no influence between panel members can be assumed. The panel leader calculates and reports the arithmetic mean of the odour assessments. 18

19 Harmonised approach includes the following requirements : Management of odour panels Panel selection : In order to achieve better reproducibility, the following control operations shall be realise by the lab : Perform a Sensitivity test (no limitations of the sense of smell or hypersensitivity) Analyse the reproducibility on samples (interpersonal differences are considered with a tolerance and a retrospective screening) To check the performances on the CRM during the training sessions for the intensity trained panels. A panel member not compliant to the criteria shall be removed from the panel. 19

20 Harmonised approach includes the following requirements : Management of odour panels Panel size : The panel shall be large enough to meet the requirements regarding the accuracy of the odour measurement. The accuracy of the evaluation is determined by the standard deviation of the group and the panel size. Acceptability : more than 14 untrained panel members The standard deviation shall not exceed 0,4 (validation criteria) Intensity : more than 7 trained panel members The standard deviation shall not exceed 3 pi (validation criteria) 20

21 Harmonised approach includes the following requirements : Odour assessment protocol : The odour characterisation is done in two separate sessions! 1. Acceptability by untrained panel +1 0,5-0,5-1 Clearly acceptable Just acceptable Just unacceptable Clearly unacceptable Sr < 0,4 the panel members shall wait in the test room for at least two minutes before the first evaluation of the test air. the panel members shall answer to the question: Assume that you would daily, for several hours, be exposed to the air from the test chamber, how acceptable is the air quality? The panel members mark down their assessment by ticking down on the evaluation form. 21

22 Harmonised approach includes the following requirements : Odour assessment protocol : The odour characterisation is done in two separate sessions! Intensity by trained panels CRM (acetone) Sr < 3 0 First the panel members shall smell the unknown sample once. After this inhalation they have to smell at the corresponding reference concentrations in increasing order. To minimize adaptation effects, the panel members shall smell at clean air before smelling at the sample again. A single measurement value is written in a form. It would not take more than 90s. 22

23 Proposal for packaging odour test The protocole should integrate the GLP and requirements of the harmonised approach : STEP 1 - MATERIAL SAMPLING AND TRANSPORT Samples shall be protected from chemical contamination or any physical exposure, e.g. heat, light and humidity. For solid products, this can usually be achieved by wrapping each specimen separately in aluminium foil and in a polyethylene bag or alternatively, in aluminised packaging lined with polyethylene. Before test, the sample shall be kept in its package and stored at normal indoor conditions during any period of storage. Storage may affect the emission properties due to ageing of the sample. It is recommended to minimise the storage time. 23

24 Proposal for packaging odour test The protocole should integrate the GLP and requirements of the harmonised approach : STEP 2 PREPARATION OF TEST SPECIMEN See ISO

25 Proposal for packaging odour test The protocole should integrate the GLP and requirements of the harmonised approach : STEP 3 - EMISSION TEST Aging of the material in specified conditions (t, T, RH). Test in static mode with respect to the loading factor (L = S/V). Performed in a compliant bag (Tedlar, etc) or the testing bag made of the material itself (film application) 25

26 Proposal for packaging odour test The protocole should integrate the GLP and requirements of the harmonised approach : STEP 4 ODOUR ASSESSMENT Sensory testing room compliant to ISO8589 Presentation of the smell with the help of a diffuser at the minimum flow rate recommended (0,3l/s) Panel management in agreement with the GLP (panel leader, code of behaviour, etc) Intensity rating with trained panel (comparative scale based on CRM response) with validation criteria on accuracy. Quality may be rated global or decomposed into sensory profile (see ISO 5496 using chemical descriptors) 26