On the use of ASTM closed vessel tests in accelerated ageing research

The ASTM D6819-02e3 standard for testing the accelerated ageing of paper, published in 2002, recommends using closed glass vials in order to keep the degradation products in contact with the paper and thus permitting a better simulation of the natural ageing conditions inside closed books. In the present study, the actual conditions and their stability inside closed vessels have been evaluated. The necessity of assuring a very high sealing performance (tightness) of the systems in order to avoid leakage of water vapour is the main drawback of this ageing method. Systematic studies presented in this publication tried to monitor this tightness and have provided data that helped to answer the question of what circumstances could lead to achieving its improvement. Both gravimetric monitoring of water content in vials and in situ IR measurements of the aged paper humidity have been applied for this purpose. As a result, better sealing materials (gaskets and caps) than those recommended by the ASTM standard, have been found. Additionally, application of a dynamometric spanner for closing the vials is recommended, as this is a guarantee of reasonably high and recurring tightness of the systems used in tests. Nevertheless, the systematic, linear with time, loss of moisture for all used vials was observed. A 9% loss of the initial moisture content in samples of the aged paper was observed for the tested conditions (14 days at 90 degrees C). Therefore, it seems that including some kind of gravimetric control for ageing tests performed in closed vessels is of essential importance. Kinetic studies of accelerated ageing in both closed and open systems, as monitored by DP and breaking length measurements, unexpectedly show that no statistically meaningful difference of degradation rates can be observed. On the other hand, the pH and whiteness index values reveal a meaningful difference between the rates of ageing in these systems, thus confirming the basic assumption of the ASTM test concerning the interaction of paper degradation products with the paper itself. (C) 2009 Elsevier Masson SAS. All rights reserved.