4 Material und Umwelt
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Emission testing of volatile organic compounds (VOC) from materials and products is commonly based on emission test chamber measurements. To ensure the comparability of results from different testing laboratories, their measurement performance must be verified. For this purpose, Bundesanstalt für Materialforschung und -prüfung (BAM) organizes an international proficiency test (round robin test, RRT) every two years using well-characterized test materials (one sealant, one furniture board, and four times a lacquer) with defined VOC emissions. The materials fulfilled the requirements of homogeneity, reproducibility, and stability. Altogether, 36 VOCs were included of which 33 gave test chamber air concentrations between 13 and 83 µg/m3. This is the typical concentration range to be expected and to be quantified when performing chamber tests. Three compounds had higher concentrations between 326 and 1105 µg/m3. In this paper, the relative standard deviations (RSD) of BAM round robin tests since 2008 are compared and the improvement of the comparability of the emission chamber testing is shown by the decrease of the mean RSD down to 28 % in 2018. In contrast, the first large European interlaboratory comparison in 1999 showed a mean RSD of 51 %.
The reliable measurement of very volatile organic compounds (VVOC) in indoor air by use of thermal desorption gas chromatography (TD-GC) in order to include them into evaluation schemes for building products even nowadays is a great challenge. For capturing these small molecules with carbon numbers ranging from C 1 –C 6 , strong adsorbents are needed. In the present study, recovery rates of nine suitable adsorbents of the groups of porous polymers, graphitised carbon blacks (GCB) and carbon molecular sieves (CMS) are tested against a complex test gas standard containing 29 VVOC. By consideration of the recovery and the relative humidity (50% RH), combinations of the GCB Carbograph 5TD, the two CMS Carboxen 1003 and Carbosieve SII as well as the porous polymer Tenax® GR were identified to be potentially suitable for sampling the majority of the VVOC out of the gas mix. The results reveal a better performance of the adsorbents in combination than being used alone, particularly under humid sampling conditions. The recovery rates of the chosen compounds on each adsorbent should be in the range of 80–120%.
Natural building materials for interior fitting and refurbishment - What about indoor emissions?
(2021)
Indoor air quality can be adversely affected by emissions from building materials, consequently having a negative impact on human health and well-being. In this study, more than 30 natural building materials (earth dry boards and plasters, bio-based insulation materials, and boards made of wood, flax, reed, straw, etc.) used for interior works were investigated as to their emissions of (semi-) volatile organic compounds ((S)VOC), formaldehyde, and radon. The study focused on the emissions from complete wall build-ups as they can be used for internal Partition walls and the internal insulation of external walls. Test chambers were designed, allowing the compounds to release only from the surface of the material facing indoors under testing Parameters that were chosen to simulate model room conditions. The emission test results were evaluated using the AgBB evaluation scheme, a procedure for the health-related evaluation of construction products and currently applied for the approval of specific groups of building materials in Germany.
Seventeen out of 19 sample build-ups tested in this study would have passed this scheme since they generally proved to be low-emitting and although the combined emissions of multiple materials were tested, 50% of the measurements could be terminated before half of the total testing time.
This study investigated the adaptation of the state-of-the-art test procedure for the determination of emissions of volatile organic compounds (VOC) from materials into indoor air to test for the radon exhalation from stony construction products. A complete robustness validation including all relevant parameters showed that the procedure can be well applied by testing institutes already holding available the required VOC testing infrastructure that solely needs to be complemented by calibrated commercial radon measurement instrumentation. When measurements of the radon exhalation from construction materials become mandatory by law, test capacity can easily be applied. This work can serve as a recommendation for the European standardisation that still is on hold in this point.
The ISO 16000-6 standard describes a method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air by sorbent-based active sampling, thermal desorption and gas chromatography coupled with mass spectrometry (GC/MS). It also gives directions to adapt this methodology to very volatile organic compounds (VVOCs). Indeed, toxicologically based guideline values are being implemented for these compounds and it becomes necessary to measure them. But a comprehensive and robust measurement method is lacking. This work highlights the points that still need to be explored towards the standardisation of a suitable procedure: investigations on sorbent combinations, the suitability of chromatography columns and the use of gaseous standards are required. The biggest challenge remains in the fact that strong sorbents adsorb water together with VVOCs. Water may impair the analysis and the optimal approach to eliminate it is still to be found and integrated into the sampling strategy.
The ISO 16000-6 standard gives directions to adapt the analysis of volatile organic compounds (VOCs) in indoor and test chamber air to very volatile organic compounds (VVOCs). The same techniques with sorbent-based active sampling, thermal desorption and gas chromatography coupled with mass spectrometry (TD-GC/MS) should be used. However, VVOCs require gaseous standards, an adapted GC column and a reliable sampling adsorbent. This work presents experimental results to tackle those three experimental gaps. A stable standard gas mixture containing 47 VVOCs, 13 VOCs and an internal standard was successfully generated. It was employed to study the suitability of seven types of chromatography columns. The use of PLOT (Porous Layer Open Tubular) columns such as PoraBOND Q is well suitable for VVOC analysis. The recoveries of the 60 analytes on a total of 16 adsorbents and their combinations were determined: A combination of the graphitized carbon black Carbograph 5TD 40/60 and the carbon molecular sieve CarbosieveTM SII showed great recoveries for all analytes. Carbon molecular sieves adsorb water which can impair the analysis. A dry purge of the multi-sorbent in the sampling direction led to a complete water removal and promising recoveries of the analytes.
On the use of Carbograph 5TD as an adsorbent for sampling VVOCs: validation of an analytical method
(2023)
A standardised method for the analysis of very volatile organic compounds (VVOCs) in indoor air is still missing. This study evaluates the use of Carbograph 5TD as an adsorbent for 60 compounds (47 VVOCs + 13 VOCs) by comparing their recoveries with different spiking modes. The influence of the spiking of the tubes in dry nitrogen, humidified air or along the whole flushing duration mimicking real sampling was investigated. 49 substances (36 VVOCs from C1 to C6) had recoveries over 70% on the adsorbent in humidified air and were validated. The linearity of the calibration curves was verified for every spiking mode and the limits of detection (LOD) and quantification (LOQ) were determined. The LOQs were lower than the existing indoor air guideline values. The robustness of the method was considered by studying the influence of the sampling volume, the sampling flow rate, the humidity level and the storage of the tubes. In general, the most volatile or polar substances were the less robust ones. The combined measurement uncertainty was calculated and lies below 35% for a vast majority of the substances. An example of an emission chamber test using polyurethane foam is shown: Carbograph 5TD performs much better than Tenax® TA for VVOCs and emissions from n-butane were quantified with combined measurement uncertainty.
EN 16516 sets specifications for the determination of emissions into indoor air from construction products. Reliable, accurate and International System of Unit (SI)-traceable measurement results of the emissions are the key to consumer protection. Such measurement results can be obtained by using metrologically traceable reference materials. Gas-phase standards of volatile organic compounds (VOCs) in air can be prepared by a variety of dynamic methods according to the ISO 6145 series. However, these methods are not always applicable for semi-VOCs (SVOCs) due to their high boiling point and low vapour pressure. Therefore, a novel dynamic gas mixture generation system has been developed. With this system gas-phase standards with trace level VOCs and SVOCs in air can be prepared between 10 nmol mol−1 and 1000 nmol mol−1. The VOCs and SVOCs in this study have normal boiling points ranging from 146 °C to 343 °C. Metrologically traceable reference materials of the gas-phase standard were obtained by sampling of the VOC gas-phase standard into Tenax TA® sorbent material in SilcoNert® coated stainless steel tubes. Accurately known masses between 10 ng and 1000 ng per VOC were sampled. These reference materials were used to validate the dynamic system. Furthermore, the storage and stability periods of the VOCs in the reference materials were determined as these are crucial characteristics to obtain accurate and SI-traceable reference materials. In a round robin test (RRT), the reference materials were used with the aim of demonstrating the feasibility of providing SI-traceable standard reference values for SVOCs for interlaboratory comparison purposes. Based on the results from the validation, the storage and stability studies and the RRT, gas-phase standards and reference materials of VOCs and SVOCs with relative expanded uncertainties between 5% and 12% (k = 2) have been developed. These reference standards can be used as calibrants, reference materials or quality control materials for the analysis of VOC emissions.
In this work, we use a gas sensor system consisting of a commercially available gas sensor in temperature cycled operation. It is trained with an extensive gas profile for detection and quantification of hazardous volatile organic compounds (VOC) in the ppb range independent of a varying background of other, less harmful VOCs and inorganic interfering gases like humidity or hydrogen. This training was then validated using a different gas mixture generation apparatus at an independent lab providing analytical methods as reference. While the varying background impedes selective detection of benzene and naphthalene at the low concentrations supplied, both formaldehyde and total VOC can well be quantified, after calibration transfer, by models trained with data from one system and evaluated with data from the other system. The lowest achievable root mean squared errors of prediction were 49 ppb for formaldehyde (in a concentration range of 20–200 ppb) and 150 μg/m³ (in a concentration range of 25–450 μg/m³) for total VOC. The latter uncertainty improves to 13 μg/m³ with a more confined model range of 220–320 μg/m³. The data from the second lab indicate an interfering gas which cannot be detected analytically but strongly influences the sensor signal. This demonstrates the need to take into account all sensor relevant gases, like, e.g., hydrogen and carbon monoxide, in analytical reference measurements.