Environmental Competences VIAQ Training Day Dr G J

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Environmental Competence Project - Primary Objectives § Understand the issues and provide clear direction for the project partners to ensure an effective response to the Integrated Product Policy (IPP). § Develop capability within the supply base to satisfy the emerging requirements for vehicle interior air quality (VIAQ) © 2006 IARC 3

PARD Programme background • The Premium Automotive Research and Development (PARD) Programme consists of a portfolio of research and development projects. • Programme set up in 2003, project activity to be completed by end 2006 and deliverables achieved by 2010 • It is aimed at enhancing the manufacturing and design capabilities of automotive supplier companies, particularly in the West Midlands. • The programme is supported by the Regional Development Agency, Advantage West Midlands together with numerous partner companies, including a lead partner, Jaguar & Land Rover. • The International Automotive Research Centre was set up in the University’s Warwick Manufacturing Group to host the programme © 2006 IARC 4

Supplier Interaction Components (component testing) facia Headliner Materials (micro chamber) Assistance to suppliers Tests, reports, training, material choices trim carpets Adhesives Sealants © 2006 IARC 5

JAMA Guidelines Overview q Substances emitted from vehicle interior may be harmful q Japan (JAMA) are the first country to have released voluntary vehicle interior air quality guidelines– seen as potential future legislation. FULL LIST IN HANDOUTS. q Guideline limits are for 9 compounds including formaldehyde, acetaldehyde and toluene tested at 40°C Substance Concentration guidelines µg/m 3 Issue Formaldehyde Potential carcinogen, irritant Acetaldehyde 48 Irritant Toluene 260 Headaches, fatigue Xylene 870 Harmful irritant Ethylbenzene 3800 Toxic agent Styrene 220 Harmful irritant Di-n-butyl phthalate 220 Phthalates linked to cancer Di-n-ethylhexyl phthalate © 2006 IARC 100 120 and hormone imbalance Tetradecane 330 6

Definitions: In car air quality – what exactly do the terms mean ? VOC: q Sum of VVOC and VOC which easily evaporate from sample at test-temperature 25 << 100 ºC/1 barr and with in-car concentration at least > 2 times higher than outside FOG (Windscreen Fogging): q Sum of VOC and SVOC which evaporate from sample at testtemperature > 90 ºC/1 barr Odour compounds (OC’s): q Organic chemicals with very high vapour pressure and readily evaporating at normal pressures and temperatures and quite often not detected as VOC’s © 2006 IARC 7

Definitions: VOC Classification by the WHO Boiling point Term Examples < 50 ºC Very Volatile Organic Compounds (VVOC) Formaldehyde (- 21 ºC) Acetaldehyde (20 ºC) > 50 ºC Volatile Organic Compounds (VOC) < 260 ºC Benzene (80 ºC) Toluene (110 ºC) Styrene (145 ºC) Dabco (175 ºC) > 260 ºC Semivolatile Organic Compounds (SVOC) < 400 ºC > 400 ºC Di-n-butyl phthalate (340 ºC) Di-n-ethylhexyl phthalate (390 ºC) Particulate Organic Matter (POM) PCB © 2006 IARC 8

Evaluation strategy - Equipment and facilities § Vehicle Testing: performed at Gaydon § Volumetric § 1 m 3 chamber testing § Volumetric § test: ug/m 3 Micro-chamber testing § Emission rate test: ug/m 2/hr § Thermal desorption – GC/MS § HPLC – being installed later this week © 2006 IARC 11

Evaluation strategy - Test programme § Vehicle testing: - Complete vehicle testing performed in line with Japanese Automotive Manufacturers Association (JAMA) voluntary guidelines on a range of new vehicles § Component testing: - Complete car set being tested in chamber - Correlation tests being done to VDA 276 § Material testing being done using micro-chamber: - production material - component material © 2006 IARC 12

Test configuration / sampling process Air flow rate / sampling time very closely controlled to give consistency of results. Results in micrograms per m 3 These must be below values given in regulations. Will effect: health toxicity, odour and fogging. © 2006 IARC 14

Single µ- CTE Chamber Assembly Sample tube Micro-chamber • Diameter 45 mm • Depth 28 mm • Volume ~45 cm 3 Heated block • The µ-CTE contains 6 Chambers in Total Heated air/gas supply • Temps. up to 120°C Air/gas manifold supplying all 6 μ-Chambers Flow controlling device • 10 – 500 ml/min © 2006 IARC 17

Evaluation strategy - Equipment and facilities Micro-chamber benefits: § Can collect air samples from up to 6 material samples simultaneously § Highly repeatable and controllable § Can carry out sampling from ambient to 120 degs C § Need only small quantities of sample material (~∅40 mm discs) § Rapid sample turnaround (based on 30 mins sampling time) © 2006 IARC 18

Sampling and test protocol Materials sampling conditions Microchamber Parameters: § Micro-cell mode (planar sample, Ø 40 mm disc) § VOC-free compressed air § 40 0 C § 30 minutes § 21 ml/min flow rate § TENAX TA packed steel tubes (200 mg) © 2006 IARC 19

1 m 3 – VDA 276 Chamber Specifications § Treated stainless steel for best cleanliness. § Cleaning protocol, plus air samples taken before each test to confirm cleanliness results. §Testing: Chamber conditioning phase 75 C followed by sampling regime of 65 C. VDA test is at 120 mins after sample has been inserted. § Our testing takes air samples (15 mins) immediately the test material is inserted and continues for 220 mins. © 2006 IARC 21

Nominal chamber concentration VDA 276 expected concentration profile © 2006 IARC VOC levels minus Air exchange Oven conditioning Sample conditioning period sampling Steady state period Time during test 22

Other Methods § Tedlar bag, used by Honda and Nissan § Component placed in a tedlar bag which is filled with clean air. Left in the bag for the duration of the test. Air sampled onto a tube at the end of the test period § Direct desorption techniques § Direct pyrolosis of the material in to the MS. § Heating the material in thermal desorber which follows the usual GC/MS path. § We have been reluctant to do these are they can cause contamination and increase background levels. © 2006 IARC 23

Surface Interactions Surface air flow Rapid Removal of VOCs Air Diffusion Bulk diffusion Still air: surface boundary layer - area / topography Bulk Material: - Density - Surface area -VOC Molecular weights -Layered Structures - foams - adhesives © 2006 IARC 24

Important criteria Selectivity • Which VOCs can be identified and at which level => VOC list Test capability • How accurate => correctness / sensitivity (ppm, ppb, , . ) • How precise => repeatability (one lab, same conditions) => reproducibility (different labs, same conditions) In house studies to study these parameters © 2006 IARC 25

GC/MS - Analysis method § Run (Desorb & GC-MS): § 1 blank (clean) VOC tube § 1 pre-loaded calibration ‘standard’, contains 1 ug each of target analytes (16 total) § Collected sample tubes § Process: § Calibrate detector response according to 1 ug ‘standard’ § Detect and integrate peaks from chromatogram § Analyse mass spectra within those detected peaks § Mass ratios within mass spectrum allow identification of compound § Quantified target compounds & qualitative unknowns © 2006 IARC 26

GC/MS Analysis of Results U-cte: run a minimum if 3 chambers, check flow at beginning and end of sampling. Quantitative results: those compounds run in the standard can be quantified with respect to their response in the standard. All others are determined with respect to toluene response in the standard using the relative areas; semi-quant results. © 2006 IARC 27

Analytical process conditions Unity-Ultra Desorption Parameters: GC-MS Parameters: Parameter Value Column 60 m, 0. 25 μm GC oven (start) 40 o. C GC oven Ramp 1 110 o. C @ 6 degs/min GC oven Ramp 2 315 o. C @ 15 degs/min GC oven hold 315 o. C for 10 mins Total time 35. 33 mins Column flow control Constant velocity mode, 24 cm/sec Ion source 200 o. C Interface 315 o. C m/z range 35 to 350 © 2006 IARC 28