Active Standard: D7309 - 13
The relationship between the sample mass and heating rate in 10.1.2.1 is based on a limited set of empirical data obtained on an early version of the Microscale combustion calorimeter as described in Ref. (1). This apparatus had different construction from D7309 and required mathematical deconvolution (unsmearing) of the oxygen consumption signal to obtain the specific heat release rate, which introduced significant error in the maximum specific heat release rate and the relationship between heating rate and sample mass. A revision of the Test Parameters section 10.1.2.1 Heating Rate is proposed to incorporate a more accurate relationship between the heating rate in the test and the sample mass that includes the expected error of the measurement as described in the added Ref. (14): R.E. Lyon, N. Safronava, J. Senese and S.I. Stoliarov, Thermokinetic Model of Sample Response in Nonisothermal Analysis, Thermochimica Acta, 545, 82-89 (2012). The recommended specimen mass of 5 mg at a heating rate of 1 K/s in 10.1.2.1 assumes a relative error of 9% based on the average coefficient of variation of the Qmax reproducibility in Table 2.
Keywordscalorimetry; carbon dioxide; combustion; controlled heating; heat release; heat release rate; heat release capacity; oxidative thermal decomposition; oxygen consumption calorimetry; pyrolysis; thermal analysis; thermal decomposition: Calorimetry; Combustion; Flammability; Plastics;
Ballot Item Approved as D7309-2013 and Pending Publication