D-14 Drying TABLE D-3 Observations during Freeze-Drying Sugar Solutions (10% w/w) Freezing Pattern Sucrose alone Sucrose + 5% TBA Sucrose + 10% TBA Lactose alone Lactose + 5% TBA Lactose + 10% TBA Collapse Shelf Product Drying Temperature, °C Temperature, °C Temperature, °C Rate, g/hr Spontaneous Slow, needles Slow, needles Spontaneous Slow, needles Slow, needles -28 -21 -20 -23 -22 -21 -30 +30 +30 -15 +30 +30 -31 -28 -30 -27 -26 -27 0.21 0.60 0.67 0.19 0.70 0.79 Taken from DeLuca, P P., Kamat, M S., Koida, Y Congr Int Technol Pharm., 5th, 1989, 1, 439, permitted by the publisher, Rue J.-B Clement TABLE D-4 Effects of TBA on Properties of Dried Sucrose Without TBA With TBA Initial drying Texture Particle shape SEM Polarized light Crystallinity Residual moisture Surface area Slow Coarse Irregular Plate-like Non-birefringent Amorphous 1–2% 0.9 m2/g Residual TBA Total drying time 40 hr Fast Smooth, soft Irregular Plates but porous Partial birefringence Partial crystallinity 1–2% 1% TBA = 1.13 m2/g 5% TBA = 2.25 m2/g 10% TBA = 2.80 m2/g