In the recent years, there are a lot of hazardous contaminated compounds emitted from the indoor building materials. Therefore, we usually sample the concentration of volatile organic compounds by the small-scale environmental chamber in our country in order to manage these building materials emission station. However, consider the property and adsorption of the VOC as well as the air tightness of the chamber, it is necessary to estimate the pros and cons of the sampling method. Therefore, this study uses the ISO 16000-25 and the ASTM D5116 as the test methods, trying to compare the difference of them by sampling the paints and the PVC tiles from the market. The result shows that the concentration and the emission rates calculated by micro-glass method are easy to be influenced by both the paints property and the emission area of the paint, which will decide whether the surface is wet or not. Causing the changing of emission rates. Furthermore, although the remains of VOCs compared to the 48 hours sampling are small, the heating phase of micro-glass method indeed can increase the trap concentration. And due to its high load factor and ventilation, it can both gather more compounds and the air concentration, proper to precise controls. For the small-scale environmental chamber method, it is appropriate to present the situation in indoor environments and easy to control the process. The properties of building materials make the emission condition different. Moreover, by raising the testing temperature or the thickness, the trapped quantity of the VOC from building materials are increasing.