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OCR for page 189
Appendix F
EXCERPTS FROM TITANIUM TETRACHLORIDE SPECIFICATIONS
du Pont de Nemours & Co. ~ Inc. Specifications (Extracted from E. I.
ium Tetrachloride)
This description was originally prepared to assist users of du Pont
titanium tetrachloride in planning sat e storage and handling procedure s.
The excerpts presented below are based on du Pont experience.
In planning sate storage and handling
Titanium tetrachloride ~ TiC14) is manufactured by the chlorination
o f t it anium-bearing ore s in the pre sence of coke as a reducing
agent. Titanium tetrachloride is a colorless to light-yellow liquid
with a pungent odor. Ti tanium tetrachloride is very susceptible to
hydrolysis, and the liquid fumes strongly when exposed to moist air.
The fumes are dense and persistent and consist of hydrochloric acid,
f inely divided particles of titanium oxychloride and hydrated oxides
of titanium. (Tables below give typical analysis and properties of
TiC14 ~
Typical Analysis (percent )
TiC14
Tin
Silicon
Iron
Vanadium
Aluminum
Chromium
Copper
Lead
Ni ckel
99.5
0.05
0.02
O .0006
0.003
0.003
O .0003
O.0007
O .002
0.008
Chemical Properties
Physical Properties
Molecular weight
Boiling point ~ 760 mm Hg ), °C
°F
Freezing point ~ °C
°F
Specific gravity @ 20°C (68°F)
Weight per gallon, lb
Vapor pressure, mm Hg @ 20°C
Viscosity, cP (mPa) ~ 20°C
Specific Heat ~ liquid), cal/g/ °C
J/kg/K
189.71
136.4
277.5
-25
-13
1.73
14.4
10
().85
0.19
795
Ti tanium tetrachloride breaks down almost completely on solution in
water converting into colloidally dispersed titanium oxyhydrates. The
reaction of liquid TiC14 with water is extremely violent, almost
explosive. The products in strong HC1 solution are clear at room
temperature .
189
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190
TiCl4 dissolves in various alcohols (methanol ~ ethanol) forming
salt-like solvates having good electrical conductivity. With the organic
halides ~ TiC14 generally forms weakly conducting salt-like complexes.
Health Hazard s
Titanium tetrachloride is a powerful desiccant and contact with the
liquid product will cause burns from both chemical and thermal effects.
The vapor is also hazardous and is extremely irritating to the skin, eyes,
nose and throat . Overexposure deco the vapor may cause burns to the eye s and
lungs .
Oregon Metallurgical Corporation Ticks Specification (Nov. 30, 1976)
Scope:
This specification covers titanium tetrachloride used in the production
of titanium sponge .
Color:
yellow.
The acceptable color of TiCl4 will be water white to light straw
Chemical Compo sit ion:
Chlorine
TiCl4
Iro n
Vanadium
Ca rbon
Silicon
Ch romium
Nickel
Aluminum
Tin
Copper
Manganese
Sn, Cu. Mn:
Quality:
None
9 9.8 Percent
25 PPM
25 PPM
40 PPM
lo PPM
25 PPM
25 PPM
25 PPM
50 PPM
50 PpH
50 PPM
Total 100 PPM
Vendor shall be responsible f or establishing and usi ng sampling
procedures and methods for chemical analysis to afford reliable assurance
of the acceptable quality levels.
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191
Timet Divison, TCMA TiC14 Specif ication
The following tables are a tabulation of specifications for TIMET
titanium te trachloride:
Ca talyt ic Or ade
Chemi stry
Re port editMaximum Typical Physical Charac teri stic s
Tin 10 ppm 6 ppmAPHA Color: 40 max.
Aluminum 20 ppm 6 ppmClarity: no sign of turbidity
Iron 10 ppm 5 ppm
Vanadium 10 ppm 7 ppm
Silicon 10 ppm 5 ppm
Copper 5 ppm 2.5 ppm
Chromium 5 ppm 3 pp~n
Re sidue 160 ppm 90 ppm
bother elements by special request .
-
Physical Properties of Titani~ Tetrachloride
Reference
Color ' Colorless
Odor Sharp, fumes in air
Molecular weight 18 9. 71 ( 1)
Melting point -25 °C (1)
Boiling point 136 .4 °C ~ 1 )
Specific gravity 20/20°C 1.726 (1)
Refractive index n25 1.61 (1)
D
Heat capacity, liquid 35~7 cal/deg mole, 25°C (2)
Heat capacity, gas 25e45 + Oe23 X 10-3T - 2~36 X 10-5T2
cal/deg mole (3)
Heat of fusion 2e24 kcal/mole' - 25°C (21~3 BTU/lb) (4)
Heat of vaporization 8e346 kcal/mole, 136e4°C (79~2 BTU/lb) (4)
Heat of formation, liquid -192.1 kcal/mole, 25°C (-1822.7 BTU/lb) (4)
Free energy of formation, -175.9 kcalimole, 25°C (-1669.0 BTU/lb) (4)
liquid
Ref. (1) Handbook of Chemistry and Physics, 48th Edition, 1967-1968.
Ref . (2) Chemical Engineers' Handbook, John H. Perry, Third Edition.
Ref. (3) Ke lley, K. K., "U. S. Bureau of Mines Bulletin 476. " (1949) .
Ref . (4) Thermodynamic Properties of 65 Elements--Their Oxides, Halides,
Carbides, and Nitrides, C. E. Wicks and F. E. Block, USBM Bulletin
605, 1963.
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Cabo t Corporation TiC14~
192
ecif ications
Grade I Grade II
TiC14 9 9 . 8 % Min
Co lor 5 0 APHA 200 APHA
Turbidity Clear Clear
.
Chemical Analysis:
Al 5 PPM Max. 5 PPM Max.
Sb 5 .' 8' 5 8' t.
As 10 " " 10 " "
Bi 5 08 t. 5 88 88
Bo 5 88 ·8 5 8. ''
C 40 8. 85 40
Or 5 ,. ..
Co 5 " " 5 " "
Cu
Fe 10 8' '' 10 '. t'
Pb 5 " " 5 " "
Mg 5 se ~ 5 '' t'
Mo
'; 5 " "
Ni 5 08 '. 5 08 ..
Si 10 ~10 8' 8.
Sn 10 8' 88 25 " "
V 5 8' .' 10 " ''
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193
Data Sheet from Soviet TiC14 Specifications
Impurity Content, Percent by Weight
Impurity In technical Specifications In purified
TiC14 for pure TiC14 TiC14
Grade 1,
according to
TU--39--69
VOC13 0.33 0.0034 0.0034
AlC13 a 0.02 0.005 0.005
SiC14 a 0.4 0.006 0.006
Si2OC16 a 0.04 - 0.003
FeC13 a 0.012 0.0029 0.0029
CC14 0.06 0.005 ~
CC13COC1 0.005 0.0005 0.0002
CS2 0.01 0.00002 0.00002
COS 0.009 - 0.00002
Oxygen
(oxychlorides) 0.03 0.001 0.001
Si3O2Clg 0.007 - 0.002
C6C16 0.015 - -
CO2 0.01 - -
COC12 0.5 0.0005 0.00002
C12 0.05 -
Arbitrarily, the amounts of Al, Fe, and total Si are limited.
The allowable content of impurities in titanium tetrachloride going
for the production of sponge titanium is no more than the following
percent by weight:
Impuri ty
A1
at
Fe
V 0.004
COC12
C1 (free)
O2 (oxychlorides)
Grade O
Grade 1
Grade 2
Grade 3
.
( percent by weight )
0.0015
0.005
0.004
Trace
0.003
0.0005
0.001
0.003
0.007
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Representative terms from entire chapter:
molecular weight
