November 1954 INDUSTRIAL AND ENGINEERING CHEMISTRY
to 172' C. The combined material boiling over 172' C. was
treated with a solution of sodium ethoxide in alcohol until alkaline
to remove residual chlorine. After the chlorine-free material
had been stripped under reduced pressure, careful fractionation
a t atmospheric pressure gave 556 grams (2.73 moles) of p-methyl-
vinyltriethoxysilane (boiling point 177-9" C., d25 0.90), a yield
of 80 mole %.
CROTYLTRICHLOROSILAXE. 111 a 1-liter three-necked flask
equipped with reflux condenser, mechanical stirrer, and dropping
funnel there was placed 379 grams (2.0 moles) of crotyltrichloro-
silane. Through the dropping funnel there was added 184 grams
(4.0 moles) of anhydrous ethyl alcohol at room temperature over
the course of 1 hour. Hydrogen chloride evolved was allowed to
escape into a fume hood. -4t this point the reaction mixture was
heated to reflux and 92 grams (2.0 moles) of ethyl alcohol were
added during a period of 2 hours. After unreacted material
had been removed and residual chlorine neutralized with sodium
ethoxide, the crude product was stripped under reduced pressure.
Fractionation of the stripped material a t atmospheric pressure
gave 328.5 grams (1.51 moles) of crotyltriethoxysilane (boiling
point 193-195' C., d26 0.89, a yield of 75.5 mole %).
Analysis. Calculated for CloHzzSiOa;C, 55.1; H, 9.9, Si,
12.9; unsaturation, 0.735 gram of bromine per gram. Found:
C, 54.9; H, 10.2; Si, 12 65. unsaturation, 0.96 gram of bromine
per gram.
CHLORINATION
ALLYLTRICHLOROSILANE. I n a glass reaction vessel equipped
with a gas inlet tube and side arm there was placed 229 grams
(1.3 moles) of allyltrichlorosilane. The vessel was placed in an
ice bath and chlorine was slowly bubbled into the chlorosilane
for 5 hours. During this time a total of 110 grams of chlorine
xas added. Distillation of the reaction product gave 186 grams
of impure material [boiling point 53" C. (0.3 mm.)], uThich upon
careful fractionation yielded p,r-dichloropropyltrichlorosilane
[boiling point 36" C. (0.15 mm.), d261.471, Analysis. Calculated
for CaH5CljSi: Si, 11.3; C1, 72.0; C, 14.6; H, 2.04. Found:
Si, 11.2; C1, 73.0; C, 14.4; H, 2.2.
p-METHYLVINYLTRICHLOROSILANE. I n a glass reaction vessel
equipped with a gas inlet tube and side arm there was placed 253
grams (1.44 moles) of 0-methylvinyltrichlorosilane. Chlorine
was passed into the compound for 3 hours, during which time the
reaction mixture became hot and 109 grams of chlorine was ab-
barbed by the sample. Some substitution of chlorine also took
place, as indicated by evolution of hydrogen chloride during the
reaction. Distillation of the reaction mixture (362 grams) gave
242.5 grams of material [boiling point 87-91' C. (20 mm.), d25
1.46, per cent hydrolyzable chlorine 57.7 (theory for four chlorine
atoms 57.6)], which upon careful fractionation gave 139 grams
(0.56 mole) of reasonably good c&dichloropropyltrichlorosilane
[boiling point 84.5-86.5' C. (17 mm.), d251.453.
CROTYLTRICHLOROSILANE. I n a glass reaction vessel of 500-
mi. capacity equipped n i t h a side arm and gas inlet tube there
was placed 189.5 grams (1 0 mole) of crotyltrichlorosilane. A
cold trap mas connected to the side arm to protect the reaction
vessel from moisture. After the vessel had been immersed in a
mixture of dry ice and acetono to prevent substitution, chlorine
was passed in for 46 minutes. during which time chlorine addition
no longer occurred. The gain in weight of the reaction mixture
a-as 72 grams. Fractionation of the 259.5 grams of material
Vapor Pressures of Silicon Compounds
ARTHUR C. JENKINS AND GEORGE F. CHAMBERS
Linde Air Products Co., Division of LTnion Carbide and Carbon Corp., Tonawcenda, V. Y .
V APOR pressures of 20 silicon compounds were measured
for use in plant design calculations. The range of pressure
varies within 20 and 760 mm. of mercury. The constants of
the Antoine equation logic Pmm. = A - B/(t +C) are given for
each compound. Vapor pressures of eome of these compounds
have been reported by other workers, and in most cases the agree-
ment with their data is satisfactory.
The compounds used in this work were fractionated a t least
twice in a column with 20 theoretical plates, and the center cut
with a sharply defined boiling point was retained for the vapor
2367
collected gave 122 grams (0.47 mole) of 2,3-dichlorobutyltri-
chlorosilane [boiling point 76-77' C. ( 5 mm.), d2* 1.41, per cent
hydrolyzable chlorine 57.3 (theory for four chlorine atoms 54.5)],
and 127 grams of other unidentified products.
DISPROPORTIONATION
ALLYLTRIETHOXYSILANE. I n a 250-ml. flask connected to a
fractionating column there were placed 137 grams (0.67 mole) of
allyltriethoxysilane and 1.2 grams of sodium ethoxide. The
mixture was heated a t the reflux temperature for 5 hours, during
which time 52 grams of material distilling below 165" C. was
removed from the head of the column. Fractionation of this
low-boiling material and the residual material separately gave 63
grams (0.20 mole) of ethyl silicate (boiling point 162-164' C., d25
0.92), and a complex mixture of products believed to be allyl-
ethoxysilanes. Formation of ethyl silicate in the reaction indi-
cated that disproportionation of allyl and ethoxy groups had
taken place.
CROTYLTRIETHOXYSILANE. I n a 250-ml. flask connected to a
fractionating column there were placed 134.5 grams (0.62 mole)
of crotyltriethoxysilane and 2.0 grams of sodium ethoxide. The
mixture was heated a t the reflux temperature for 20 hours, during
which time 46.0 grams of material distilling below 175" C. \$as
removed from the head of the column. At this point the residual
material was stripped under reduced pressure. A total of 126
grams of volatile product was obtained. Fractionation of this
material gave 42 grams (0.20 mole) of ethyl silicate (boiling
point 162-165' C., d26 0.92), 45 grams (0.21 mole) of recovered
crotyltriethoxysilane and 21 grams (0.092 mole) of dicrotyldi-
ethoxysilane (boiling point 217-221" C., dZ60.87).
Analysis. Calculated for CIZH2&3i02: C, 63.25; H, 10.5; Si.
12.3; unsaturation, 1.40 grams of bromine per gram. Found:
C, 63.2; H, 10.8; Si, 11.4; unsaturation, 1.81 grams of bromine
per gram.
ACKNOWLEDGMENT
The authors wish to thank W. N. Moore, C. M. Birdsall, and
others of this laboratory for many of the analyses and infrared
data reported here.
LITERATURE CITED
(1) Bailey, D. L., Ph.D. thesis, Pennsylvania State College, 1949
(2) Hurd, D. T., and Roedel, G. F., IKD.ENG.CHEM.,40, 2078
(1948).
(3) Sommer, L. H., and associates, J . Am. Chem. SOC.,
68, 1083 (1946).
(4) Sommer, L. H., Tyler, L. J., and Whitmore, F. C. Ibid., 70,
2872 (1948).
( 5 ) Sommer, L. H , Van Strien, R. E., and Whitmore, F C., Ibtd.,
.~ 3056
71
I ~~-~ (1949).
~~ ~ I
(6) Swiss, J., and Amtzen, C. E. (to Westinghouse Electric Corp.),
U. S. Patent 2,595,728 (Xay 6, 1952).
(7) Wagner, G. H., and associates, ISD. EKG.CHEY.,45, 367 (L953).
RECEIVED for review March 24, 1954. ACCEPTED August 3, 1954.
Presented before the Division of Organic Chemistry, Symposium on Carbon-
Functional Silicones, at the 125th hfeeting of the AMERICANCHEMICAL
SOCIETY, Kansas City, hlo.
pressure measurements. An additional indiestion that the
samples were of high purity was provided by the isoteniscope
method, which involves repeated boiling of the sample a t con-
stant temperature until constant pressure is attained. X o diffi-
culty was encountered in obtaining a constant pressure within
0.05 and 0.10 mm.
APPhR4TUS AXD METHOD
The vapor pressure apparatus was based on the Smith-Xenzies
isoteniscope ( 6 , 8).
2368 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 46, No , I 1

~ T A L01 SILICOS~ o v r ~ o v r u s
I. E X P E R I J I J ~ Da~a
TABLE
.- l'mm.
i, C. Obsd. Calcd.
:lllyltric lilorosilanc
43.7 53 0 j3.0 I i 160 7 160 (1
57 9 93 5
76.3 199.5 199.4
92 0 3 4 8 . 9 331 3
63 6
2:
2s 0
; 483
225
223.5
3 9 3 74
3P29
0
489 G
6 603!10
7 82031
1116
--
9922
183
251
116 8
202 0
115 0
..
1 0 4 . 9 5 2 0 . 2 534 0 :I4 16'10 1 630 1
1 1 3 . 1 7 2 4 . 3 724.8 40.7 7 5 5 5 735.0 cliloi oailane 7 932302227 260 180 6
I)icthyldiclilorosilane 7 07712148? 223 130. 4 13ij 4
Diethyldic!ilorosilaiie Tetraclilorosilane UiirietliS-ldiclilorosilanc 714351 1328 24 1 70.5 70 3
I~ir~lien~ldiclilo:.osilan~6 95480 1884 158 301 4 304 0
48.1 40 4 40.4 2 2 863 861 Ethylilichlorosiiane 761420 1664 276 7,j i
G5 3 83.9 85.7 23 1 230 0 218 2 658174 1102 I 9 9 98 8 00' 3
83 7 176 2 174.5 .34.2 340 7 340.2 7 18148 1.j3 0 1(Iq 160 9 ..
100 0 305 9 306 0 40 G 481 7 431 0 7 lllcici 118!1 228 191.7
116.5 511.7 511.6 !G 5 531 0 531 0
127.7 706 2 705.4 .iG 9 752 2 731 .j
Ilexaetliylcyclotri-
",-Chloro~lrogyl- silosane 6 , 3 8 31 7 1.276 11P %XI.3
6.0 50 0 51.7 triclilorosiianc ~Ie~iiyldichloiosilarie 7 04812 I179 2.42 '40 9 4'1' 9
21 3 1 0 3 . 9 114 0 l\ietliyltrichlorosiianc 6 87213 1167 '26 66 4 66.4 6.l 7
87.1 32 5 32 .i Phenyltric!iiorosiianc F 98140 1641 100 201 0 201 0
31.1 I 5 5 4 137 0 121 8 126 4 126 8 Tetrachlorosihne 6 97287 u n o 286 .57 3 .iO, 8
35.5 167 5 187 2 14cj.3 308 0 3 0 7 . 6 Trichlorosilane 7.09110 1170 216 31 0 31.8
43.6 274 3 27.5 5 139 1 4 0 0 . 2 4 0 9 . 1 Trimet tiylcnlorosilane 6 95054 11!11 235 57 6 37 3
?$I :i 315 6 315 J 1 7 1 . 6 j 7 5 . 8 576 2
33 2 363 1 362 7 \'iny!tl.ic;iloio4ilane 7.32284 151.3 230 $10 6
1 7 9 . 4 70G 4 7 0 5 . 7 \-inyltrierhoxy-silane 7 . A4075 1733 220 160 ,5
51 4 482 .i 481 3
13 1 703 2 704 2
~Ieth~ltriclilo~~silane
Histricliloro- 13 7 101 0 100 8
silylethane 23 5 157 3 157 3
30 0 261 6 261 8
htalitly evacuated 011one side. This manometer as inadc O i
91 2 18 5 I8 6 12-mni. tubing; since t,he pressure was equal to the differeiiw
I14 i 48 2 48.9 49 8 433 8 $37 3
147 1 134 2 I54 4 57 3 562 3 566 0 between the two sides of the manometer, meniscus correctioii,*
159 9 2 8 1 . 0 2R1 2 61 3 710 8 711 5 were negligible. Pressure readings xvere made with a Gaert,i~c,r
Diiiiethyl- Trichloroailnnc (sathetometer with two telescopes which were compared at a
diclilorosilane fiducial point for consistency. Pressure readings were reduced
2.1 236.8 237 3 io 0" C. The correction to st,andard gravity was not matic sincc
27 8 l:Q 5 l39.G 10 1 333 4 333 2
38.0 211 5 211.0 18.7 466 0 468 6 it was lees than 1 part in 2500.
48 0 353 5 3 5 3 . 5 22 5 342 R 541.6
38 0 504 4 593 6 27 0 638.9 649.0 Temperature control was obtained Iiy immersion of the iso-
66 1 658 8 63G 5 31.6 750 7 75'2 ,5
72.1 7 9 8 . 0 708 1 tcmiscope in a wcll-st,irred silicone oil bath contained in a SOrip
Hcxaetliyloyclo- silvered Dewar flask of 4-liter capacity. Two immersion hcaters
trisiloxene
28 5 ,53 3 54 7 161 3 55.6 56 1 hlc transformers werc used. Oiic hcatcr p ~ ~ ~ i d ( - : l
3s 7 88 2 88 2 186 6 138 6 138 8 ree of heat; the other supplied heat when called f w
. i 8 . 7 167 1 1 6 6 . 2 213 0 302.3 3 0 2 . 7
70 2 ci07.9 307
no 0 ,183.4 ,586 0
, 223.9
232 3
4 0 4 . 9 404 5
500 0 4 9 9 . 5
thermoregulator. When required, a cooling coil
93 6 694 7 6 9 3 . 6 242 8 6 4 1 . 4 641 1 Temperat,ures w r e rneasurcd with a ca1ihr:itc~tI
four junction Lceds and Sorthrup copper constantan thcrmo-
1.2-DichloroetiiyI-
triclilososilane couple ~ i t tvio
h junctions in the constant temperature bath and
101 7 33 8 33 6
102 2 61 2 61.2 108 8 44 4 44 9 t ~ inoan ice bath. The e.m.E. of this thermocouple was nicasurc(I
128 0 1 3 8 . 1 157 0 153 8 214 7 214 8 with a Kcnner pot,entiometcr. In some of the measurcnioiits . I
147 3 245 3 203 7 175 6 400 3 400 6
1 4 8 . 4 303 4 303 8 194 8 657 0 655 1 Bureau of Standards calibrated iiiercury-in-glass thermometer W:LP
1 6 4 . 0 480 4 182 2 197 4 692 9 697 7
180.5 738.0 7 3 8 . 5 also used as a check on the thermocouples. Indications ii-ci't:
Trimethyl- that, t,he temperature measurements \Yere accurate within 0.1 ' ('.
Dii~lienyl- chlorosilane
' diclilorosilane
2.6 8G 7 86 7
The ieoteniecope ivas opcratcd according to the standaixt,
1!'2 1 37 4 37 5 2 7 . 0 252 3 253.9 method.-that is, the sitmple was boiled repeatedljr a t constajit,
210 7 60 8 70 0 38 7 397 8 397 2
235.6 147 1 147 3 43.0 464.1 463.8 temperature until the change in pressure between two succcssivc
260 2 281.8 281 7 4 8 . 5 561.2 561.7 Ijoilings did not' exceed 0.05 mm.a t the loner pressures or 0.10
281.2 462 6 4G2.6 55.6 7 1 1 . 9 711.4
nini. a t the higher pressures. The levels of the isotcniscolic IT-
tube n-ere adjusted by eye. Because of the low density or ~ J K
64.3 21.2 21 1 17.7 46.3 46 9
81.0 46 2 46.5 28.6 78 0 78 0 s:tmple a2 compared with mcrcury, this adjustincnt could i)o iii:iclo
90.5 70.2 70.2 4 4 . 8 154 9 1 5 5 . 1 n-ithin t,he limits of error in reading tho mercury manonidci~.
121.7 231.4 229.4 6 8 . 5 374.3 373.6
1 5 3 . 4 616.6 61G.3 8 2 . 9 590.4 599 7 Observation of the U-tube also gave a good indication of the it-ni-
Ethylvinyl- pcrature control, since any fluctuations in the bath tempcrat ur(>
diclilorosilane resulted in fluctuat,ions of the liquid Icvcls in t h e U-tube.
01.1 18 4 18.5
44.9 15.5 43.5 70.0 28 7 28.7 A%sa preliminary check on the experimental method, :i fen.
7 3 . 5 140.0 130.0 81.0 4 7 . 0 47.5
93.4 3 0 6 . 1 3 0 3 . 2 Q5.5 87.4 87.4 nieasurements m r e made on miter betmecn 50" and 100" C.
10G 7 465 8 463 3 1 0 5 . 0 1 3 2 . 5 131 0
1 1 7 . 0 628.4 629 1 128 0 270 0 285 2 T h e results agreed n-ith the d a h of Osborne and Mycrs (4)witlr
121.7 7 1 9 . 9 7 1 9 . 0 1 4 8 . 1 535 2 533.8 i3.n average deviation of 0.12% in pressure.

I n this devicel the bulb containing the liquid sample w a s joined
to a U-tube also filled halfrag with the sample. The liquid
levels in the U-tube Tyere balanced by thc vapor pressure of the
liquid on one side and drv nitrogen pressure on the other. By
reducing the nitrogen pressure, air and low boiling impuritics
mere removed from the sample and bubbled through the U-tube
liquid. Nitrogen was then admitted until the liquid level in
each side of the U-tube was equal. The nitrogen side of the U-
tube was connected t o a pressuie reservoir immersed in a water
bath and to an absolute mercury manometer, which nas con-
RESULTS
The experimental data are given in Table I. The constaiits
of the hntoine equation m r e determined for each compound by
first plott>ingthe experimental data on a log,^ P versus l / ( t 230) +
scale and t,hen selecting three consistent points for the calculri-
tion of C, B, and A follovr-ing the directions given by Thomsoii
( 7 ) . The remaining points \yere then checked against the cqua-
tion. The average deviation betmen the calculsted and 01)-
served pressures for all t,he data is 1 0 . 8 mm; most of the v d i m
November 1954 INDUSTRIAL AND ENGINEERING CHEMISTRY 2369

TABLE 111. VAPOR PRESSURES O F SILICON COMPOUSDS

Temperature, _ C _ ~ ~-
~~ ___~___
Compound Formula 10 mm. 2~nim. 40 mm. 60 mm. 100 inm. 200 inm. 400 mni. 760 in1ii.
.illyltrichlorosilane CHz=CHCHzSiCla (16.1) (27.5) (40. 1) 48.3 59.4 76.4 95.9 (116.8)
l3istrichlorosilylethane ClaSiCzHaSiCla (77 7 92,Y 109.6 120.1 134 2 I55 2 (178 6) (202.9)
(180.6)
1,2-Dichloroethyltrichlorosilane
llietliyldichlorosilane
l~imethyldichlorosilane
ClCHzCHClSiCla
(CZH5)zSiClz
(CH3)zSlClz
(21.0)
( -24,8)
(75.7)
(33 7)
(-13.7)
(:;,E?
(-1.4)
101.7
56.9
(6 5 )
115.2
69.1
(17 2 )
135.2
87 5
33.2
157 6
108 I
51.4
(130.4)
70.5
Dio henyldic hlorosilane (CeHs zSiClz (158.4) ( 1 7 5 . 2 ) 194 0 205 9 222 2 246.8 274 8 (304.4)
Etbyldichlorosilane C2HadiHClz (-24.4) (-12 0) (0.8) 9 1 20.4 37.8 56.0 (75.5)
Ethyltrichlorosilane CZH~S~C~J (-I.!) (9.7) (22.3) 30 4 41.5 58.4 77.9 (98.9)
Etliyltrietlioxysiiane CzHaSi(OCzH5) a (50.9) 63.4 77 7 86 8 99 2 117.7 138 8 (160 9)
Ethylvinyldichlorosilane (CeH5) (CHz=CH SICIS (15.5) (28.1) (42.1) 51 . o 63.1 81.3 102.0 (123.7)
-,-Chloropropyltrichlorosilane C H ~ C ~ C K ~ C H X S I ~ ~ ~( ’6 2 . 3 ) 91.9 101.8 115 3 135.4 158.3 (182.3)
Hexaethylcyclotrisiioxane
LIethyldichlorosilane
&$&El: la (123.0)
(-47.1)
(76 4)
(137.1)
(-36 9)
(152.9)
( - 25 . 5 )
163.1
-18.7) (
177.1
- 8 . g )
198,6
6 . 3
228.5
2 3 . 2
(250.3)
(10 9)
1Iethyltriohlorosilane CHaSlCla (-27.3) (-16 5) (-4.6) (3.1) 13.5 29.3 47.3 (66.4)
Phenyltrichlorosilane CoHsSiCls (75.3) (89.8) 105.9 116 3 130 3 151.5 175.5 (201 . O )
Tctrachloroeilane Sic14 (-36.1) (-24.4) (-12.6) ( - a 0) 5.3 20.9 38.6 (57.3)
Triclilorosilane SiHCla (-53,9) (-43.9) (-32.9) -25.8) ( - 1 6 . 2 ) (-1.8) 14.6 (31.9)
Trimethylchlorosilane (CH43SiC1 (-34.9) ( -21.2) (- 12,3) (-4.7) 5.6 21.2 38.9 (57 6)
Vinyltric hlorosilane CFII=CHSi Cla -
( 10.7) (1.3) 14.5 22.9 34.2 51.3 70.5 (90. B)
1160.5)
Vinyltriethoxysilane CHs=CHSi(OCzHs)a (49.4) (62 E) 77 2 86.4 98.9 117.6 138.6
0 Temperatiires in parentheses arc, abo\ e or below range of experiincntal value.

are within 1 1 . 0 mm., and a few deviations are as large as 8.8
niin. The ilntoine constants are given in Table 11, together
with the normal boiling points derived from t,hese constants,
and the boiling points of those compounds reported by others.
The average deviation between our boiling points and those re-
ported by S h l l (6) is 0.4” C., and for three of the compounds
there is exact agreement. The boiling points a t pressures of
10, 20, 40, 60, 100, 200, 400, and 760 mm. of mercury are given
in Table 111. All these boiling points were derived from the
equations; those in parentheses are above or below the range of
the experimental data.
ACKNOU IXDGVlhUT
Tiw author? wish to aclrnoirledgr the work of H. C. Givens
and E. R. York in the purification of the samples used in these
measurements.
LITER4TURE CITED
(1) Booth, H. S., and Carnell, P. H., J . Am. Chem. Soc., 68, 2G50
(1946).
(2) Booth, H. S., and Slartin, TV. F.. Ibid., 68, 2655 (1946).
(3) Booth, H. S., and Suttle, J. F.,Ihld.. 68, 2658 (1948).
(4) Osborne, K.S., and Myers, C . IS., J . Research Natl. Bur. Staizd-
ards, 13 (1934) (Research Paper 891).
( 5 ) Smith, A., and IUenzies, A. W.C., J . Am. Chem. Soc., 32, 1412
(1910).
(6) Stull, D. R., IND.ENG.CHEW,39, 517 (1947).
(7) Thomson, G. TV., Chem. Revs.. 38, 1 (1946).
(8) Thomson, G. W., “Physical Methods of Organic Cheniistry.”
A. Weissberger, ed., 1-01. 1, Interscience, New York. 1949.
RECEIVED
for review March 22, 19.54. ACCEPTEDJ u l y 27, 1964.

Flow Properties of Vinyl Chloride

Resin Plastisols
E. T. SEVERS AND J. $1. AUSTIN
Mellon Institute of Industrial Research, Pittsburgh 13, Pa.

0 XE of the best examples of the application of rheology to

industrial problems is found in the development of organic
dispersions of vinyl chloride resins. Previous investigators
(7-9, 15) have stressed the importance of flow properties in the
formulation, manufacture, and application of these dispersions.
Plastisols are fluid dispersions of vinyl chloride resin in plas-
ticizer to which desired quantities of pigments, filler, and stabil-
izers have been added. Plastisols are converted to elastonleric
compounds by heating to the point where the resin is solvated
by the plasticizer and fused to a homogeneous product. The
successful use of vinyl chloride resin plastisols demands a knowl-
rdge of the flow properties a t the rates of shear encountered during
application. High speed roll and knife coating of cloth or paper
and die coating of wire or tape subject plastisols to high rates
of shear. Even processes such as slush molding and dip coating,
ordinarily involving low ratcs of shear, may require pumping of
plastisols a t relatively high rates of shear to replenish dip tanks
and provide circulation. Mixing operations using roller mills
or high energy input mixers will subject the plastisols to high
shear stresses.
Flow properties have been measured by rotational viscometers
and viscosity cups. Rotational viscometers, however, become
quite elaborate when designed for high rates of shear, arid fric-
tional heat buildup becomes serious. Viscosity cups, where the
material flows through an orifice under its own head, are limited
to measurements a t relatively low rates of shear. Furthermore,
irregularly shaped or short orifices make difficult a fundainental
analysis of flow data so obtained.
An extrusion rheometer is Rssentially a pressurized viscosity
cup with a cylindrical orifice. but it is capable of measuring vis-
cosities a t high as well as low rates of shear. The instrument is
rugged enough for production control, yet capable of yielding fun-
damental data. This instrument was used extensively in the
present investigation to determine the effect of plasticizer com-
position and concentration and aging conditions on the flow prop-
erties of plastisols.
One of the earliest extrusion rheometers put to practical use
was the “grease gun” type which Barus ( 2 ) used for investigating
marine pitches. Bingham (3) devised a gas-actuated capillary
viscometer for measuring the viscosity of a variety of substances