LANOLIN DERIVATIVES FOR PRESSURIZED FORMULATIONS 335 Table i ß • - '3 '• • •'~ • Ash (%) ........ o'oz 0'05 0'04 O'Ol O'Ol O'Ol o'oz o'o4 o'I3 0'2 Volattics (1 hr. at lO5 ø C) (%) O.lO 0.35 0.40 o.17 2.00 1.2o 3.oo 0.20 0.20 0. 3 Free cholesterol (%) .... 1'5 34'0 25'9 3'3 I'2 1.2 o.8 o.8 trace trace Total cholesterol (%) .... 20-0 34'6 27'6 I3'8 5'6 5'6 3'5 25'0 0'3 1.1 Unsaponifiables (%) .... 52'0 96'3 93'0 54'0 31'8 41'3 23'6 84'8 -- -- Acid value ........ 0'4 1. 4 2. 9 i-o 0. 4 0.6 o'7 I'4 0.2 2.0 Saponification value .... 95'0 6.0 14-o lOO.O 14o-o 114'o 146'o 155'o i6.o 9'0 Iodine value (Wij) ...... 27'0 35 '0 35'3 27'5 23'0 77'0 35'1 48'4 23'0 22.0 Acetyl value ........ 29.0 14o'o 16o.o 38'2 46'0 64'9 79-6 8.0 34'4 60.0 Melting point (øC) ...... 40'0 60.0 43'0 18'3 -- -- -- 15'o 49'2 47'5 Flash point (open) (øF) .... 400 34 ø 290 400 305 335 306 425 530 50o Cloud point (øF) ...... -- -- -- 55 48 36 30 56 -- -- Pour point (øF) ...... -- -- -- 55 35 25 25 50 -- -- Specific gravity at 20 ø C .... 0'94 0-96 0'98 0'95 0'89 0'89 0'90 0'98 1.14 x.1 Viscosity (Redwood No. 1) at 6o ø C (sees) ........ 73 ø -- 977 738 5I 57 64 392 3453 60 Solubility in water ...... nil nil nil nil nil nil nil nil corn- com- plete plete Emulsifying tendency .... w/o w/o nil w/o w/o w/o w/o w/o o/w o/w EXPERIMENTAL The following systems were tested: A -- propellant 12 B -- propel]ant 11 C -- propellant 114 D -- propellant 12/IMS, DM7 grade, 74 o.p. (2:1 w/w) E -- propel]ant 11/IMS, DM7 grade, 74 o.p. (2:1 w/w) F -- propellant 114/IMS, DM7 grade, 74 o.p. (2:1 w/•v) G -- propellants 11/12 (1:1 w/w) H -- propellants 11/12/IMS, DM7 grade, 74 o.p. (1:1:1 w/w) I -- propellants 11/12/isopropanol 99% (1:1:1 w/w) 5% by weight of each product was mixed with the propellant, or pre- dissolved in the alcohol prior to the addition of the propellants. With anhydrous lanolin B.P. (i) and liquid lanolin "50 Super" (v) it was, however, necessary to introduce the product directly into the test bottle, and each material was warmed therein together with the requisite amount of alcohol in order to achieve maximum solution prior to the addition of the propellant. Whenever a particular material was found to be insoluble in a system

336 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS containing either propellant 11 or 114, the dispenser was warmed and kept at 50 ø C for 15 minutes, amidst constant shaking, to obtain maximum solution. No warming took place with System A (propel!ant 12), but where necessary, the dispensers were shaken intermittently tor 1 hour. All filled dispensers were allowed to stand for 1 hour at 20 ø C before being examined for solubility. The results obtained are detailed in Table 2. Dispensers filled with each variable were re-examined after 6 weeks' storage at both 20 ø C and 0 ø C, in the following manner. Dispensers stored at 20 ø C (1) Visible assessment of solubility (2) Assessment of sprayability, and observation of valve blockage, if any. Dispensers stored at 0 ø C (1) Visible assessment of solubility at 0 ø C, and after being allowed to stand for 24 hours at 20 ø C. (2) Assessment of sprayability, and observation of possible valve block- age, at 0 ø C, and after being allowed to stand for 24 hours at 20 ø C. Containers and valves Plastic.coated glass containers were utilised for all tests. For systems A-H, Aerosol Research valves AR74 with SF64 (0.02") actuators were employed, and for system I, Precision valves [J18 stem, standard housing (0.08#)] with reverse taper break-up spray actuators. There was no definite preference for the Aerosol Research valve, but Precision valves suitable for glass containers were not available to us at the time when these experiments were started. RESULTS Table 2. Solubility of 10 lanolin products after 1 hour at 20 ø C Lanolin Propellant systems products A B C D E F G H I Total i ii iii iv v vi vii viii ix x 4 3 6 4 3 4 3 3 4 5 3 6 3 3 3 3 2 2 4 1 6 I 1 3 2 1 3 5 2 6 2 1 2 4 2 2 4 I 6 2 1 3 2 1 2 2 2 6 1 2 2 2 1 1 6 2 6 2 1 1 2 1 1 1 2 6 1 2 2 1 1 1 4 4 6 2 2 4 4 2 4 6 4 6 2 2 3 4 4 4 Total 41 24 60 20 19 27 27 18 24 34 30 22 26 22 19 22 17 32 35 Key 1 = soluble--no precipitate 2 = soluble, with negligible precipitate (visible only on close scrutiny) 3 = soluble, with slight precipitate (readily seen on inverting bottle) 4 = partially soluble, with either a dense precipitate or an insoluble liquid layer floating on the surface 5 = partially soluble with dense precipitate and insoluble waxes 6 = totally insoluble a = agglomeration of precipitate