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二氧化钛(钛白粉)
二氧化钛(钛白粉)$ |. d" s# Q1 B3 _0 E! ~
W- d2 P( G2 E" @& b# MJECFA关于二氧化钛(钛白粉)的结论) M+ g4 o& E$ N2 s: T" P: [
- ?$ ~7 A- J/ |# l, p摘要: 2006年JECFA关于二氧化钛的结论8 g$ I) _7 A: b! ?6 Q9 V$ {+ C
ADI值:不作限制。
1 g2 o. X9 F4 y3 ~2 s; b功能:着色剂7 x* M$ ?& P. I$ r' D. v% u
( t/ c4 }# H$ Q3 kTITANIUM DIOXIDE2 S8 p1 U# q" f4 f9 O/ ]
Prepared at the 67th JECFA (2006) and published in FAO JECFA
6 v N+ B0 d5 \4 hMonographs 3 (2006), superseding specifications prepared at the 63rd
- E% E9 i: Z$ O N5 h) W: L; g( uJECFA (2004) and published in FNP 52 Add 12 (2004) and in the
) n; a2 u7 B A$ g$ l; k5 i- ]' i. yCombined Compendium of Food Additive Specifications, FAO JECFA
4 m5 v2 A# u7 d4 R1 qMonographs 1 (2005). An ADI “not limited” was established at the 13th5 k+ k9 _& ^) b" e% f, B1 l
JECFA (1969).
+ g& c4 W- e+ j5 `( e2 bSYNONYMS* B9 E% ^( d/ b# Q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171. |9 X6 U3 Y2 h' F( s, R
DEFINITION
$ q. ~. e w/ `3 \' dTitanium dioxide is produced by either the sulfate or the chloride
4 x3 ]7 E- D/ pprocess. Processing conditions determine the form (anatase or rutile( U; r% m# F |5 h, l) C
structure) of the final product.% k8 e! m' X- T- D" m. |
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
2 L6 F6 s# G& ^7 i* Xor ilmenite and titanium slag. After a series of purification steps, the
: g+ g, r" ~) E& q+ |6 k; Risolated titanium dioxide is finally washed with water, calcined, and* r' H; [9 k% T: ?6 n8 ]: \/ E
micronized.
% b0 m1 f' H5 H4 k# T; `) ZIn the chloride process, chlorine gas is reacted with a titaniumcontaining2 }; I+ w$ q5 m, W+ P2 v) J
mineral under reducing conditions to form anhydrous
* H' H$ e# s8 ~- x! l% u- T6 q1 ~titanium tetrachloride, which is subsequently purified and converted to5 M& \1 t: p7 N- ]* L
titanium dioxide either by direct thermal oxidation or by reaction with% @9 P0 d4 v. }2 i& O1 s( h
steam in the vapour phase. Alternatively, concentrated hydrochloric
7 t7 w/ k: I$ A' F/ t+ Yacid can be reacted with the titanium-containing mineral to form a
1 A% h7 p; g7 Dsolution of titanium tetrachloride, which is then further purified and
8 G% F; u1 L1 a; ^" tconverted to titanium dioxide by hydrolysis. The titanium dioxide is& b" W& U4 u) b# N* M
filtered, washed, and calcined.
p, U i6 y& kCommercial titanium dioxide may be coated with small amounts of
; T0 E1 m' ^% C: X' `# [/ u: K- b# Valumina and/or silica to improve the technological properties of the% S# f, A& U1 Q, o! y
product.
; [; T: W/ J8 z A9 |C.A.S. number 13463-67-7
+ j+ ~- `: q0 g% ~6 j3 }3 pChemical formula TiO2
8 m/ }* U' g& w- Q0 BFormula weight6 M) ^9 } d! `; [ Y7 F
79.88 K- A- S9 x' {0 d
Assay
' K$ z. G4 b5 P; \- k' Y( jNot less than 99.0% on the dried basis (on an aluminium oxide and
+ g. t+ i4 N4 t5 r( g+ V! Ysilicon dioxide-free basis). C5 \9 N, O/ }. s( j& f
DESCRIPTION) G& o* Y5 n& U* N: n; T/ o
White to slightly coloured powder# h) s8 P" C; E" q2 X2 L
FUNCTIONAL USES
7 Q/ r0 O9 o7 }Colour
0 T/ A' M5 t& e2 E/ W1 y- eCHARACTERISTICS
2 I9 w! L9 M2 i& R. gIDENTIFICATION5 l$ ]6 ~- Y; c, U+ Q, y
Solubility (Vol. 4)
& m+ c0 c+ ?6 T2 uInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic3 R S/ y- ^8 Y) }( J6 m* w
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
+ j" j' q3 |9 ~" L: p- Wsulfuric acid.( W$ ~& l" W `0 p/ m
Colour reaction* h3 Y+ w* o# ~) I* V
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of. _, e7 L' i. m- f
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
( Y, T2 D+ j; t4 Wwater and filter. To 5 ml of this clear filtrate, add a few drops of
& B2 p: a' }$ Vhydrogen peroxide; an orange-red colour appears immediately.
; K7 g. t& E5 G; b" J+ a5 ePURITY2 ^3 U( k& J' C/ ~& g* [4 n/ J( V
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)! i% K m7 | G$ V ~8 R
Loss on ignition (Vol. 4)8 `% N- |, l$ `7 r3 u% Y
Not more than 1.0% (800o) on the dried basis
7 b6 S% h! [' ^0 e5 p4 i' t: `Aluminium oxide and/or
% G# X5 e' z( r; e; qsilicon dioxide
2 |' D. ?5 M* [) b0 r, tNot more than 2%, either singly or combined( _! s6 N, {" [3 @
See descriptions under TESTS" I9 ?0 r3 a; H: M" n4 b* G- k) I+ L
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing. A9 ]+ I5 b* x+ g/ W- c3 A
alumina or silica.
% t/ T/ e& A7 A" HSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
$ q' r( Z* i- \, @& E( aplace on a steam bath for 30 min with occasional stirring. Filter/ ^$ k9 i7 i. l# P
through a Gooch crucible fitted with a glass fibre filter paper. Wash
: E8 Z7 h$ x! S) F1 `/ x2 Z" k; Dwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
6 t% _/ ]8 I( p, z/ ycombined filtrate and washings to dryness, and ignite at a dull red
. D6 _3 t- w: {. W4 s( ?+ oheat to constant weight.$ f+ @; u, `" ?3 L
Water-soluble matter
$ {* t. w5 d, q7 f(Vol. 4)
* g* t: D# ?" u `Not more than 0.5%
2 X1 m* q$ d( @! N6 C! eProceed as directed under acid-soluble substances (above), using- A% i$ Y) ] r* s: h) B' g: r& w
water in place of 0.5 N hydrochloric acid.
# Y. m. j/ ~8 N- Y3 mImpurities soluble in 0.5 N
+ w8 P2 ]# I5 c* q b7 Yhydrochloric acid* N9 N# @9 f# s+ Y! {
Antimony Not more than 2 mg/kg
! j+ P5 z7 R2 J$ [See description under TESTS
) O- u. b5 J: ?. D& @Arsenic Not more than 1 mg/kg
% Z3 z5 B c1 Z [See description under TESTS
& A( E' O( G- DCadmium Not more than 1 mg/kg6 t I# j' j) t% n( d
See description under TESTS/ G( _3 q8 H; l' m3 h1 T2 U; C
Lead) C+ d. M1 r) b. n0 \' b3 F7 v0 l
Not more than 10 mg/kg# c0 R9 E7 S5 ^( o. I
See description under TESTS
# ]! ?0 }% k- [Mercury (Vol. 4) Not more than 1 mg/kg' b% r) c. J2 S: ` d
Determine using the cold vapour atomic absorption technique. Select a
: y2 [; t9 ^/ Gsample size appropriate to the specified level8 m' h9 F0 l& p7 D# @
TESTS
$ W2 E2 R6 O. p9 c. y6 u' bPURITY TESTS0 _% T* q8 x9 ~( i; U5 \2 p
Impurities soluble in 0.5 N
% o/ ^6 `9 S! P1 P. ?( Y: M, Fhydrochloric acid3 G0 e9 Q% ^* B0 I) C/ G0 s
Antimony, arsenic,
: \$ `, X/ ~* C7 _+ zcadmium and lead$ ~+ q! r% p5 ~: n* |
(Vol.4)% k! w: t' t5 Y# g
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
+ c" l& i; I5 c' R/ I8 [hydrochloric acid, cover with a watch glass, and heat to boiling on a
- V; i* N# U: L9 R7 k yhot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml6 `2 D4 @/ ~2 ]! R' J7 S; f
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved: M& t; W+ B; t' m4 i2 j. J# V, e
material settles. Decant the supernatant extract through a Whatman
2 i4 F9 f; k- jNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
+ v2 s% k6 r" U: u8 avolumetric flask and retaining as much as possible of the undissolved
, N& G- j6 e7 {: Ematerial in the centrifuge bottle. Add 10 ml of hot water to the original# {0 i6 i3 Q$ Y; O" M% Z1 d
beaker, washing off the watch glass with the water, and pour the
9 @7 N& h0 T1 P! K& d7 s9 Ycontents into the centrifuge bottle. Form a slurry, using a glass stirring( D3 n% L, f% i4 n
rod, and centrifuge. Decant through the same filter paper, and collect; M @8 T8 x. b
the washings in the volumetric flask containing the initial extract.+ N2 `2 Y1 N; l) v# t# x3 N) M
Repeat the entire washing process two more times. Finally, wash the
) N( Q- {0 V) m7 afilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
! d1 Z; U' @1 o9 dto room temperature, dilute to volume with water, and mix.
% E1 n- p; V- E5 u& QDetermine antimony, cadmium, and lead using an AAS/ICP-AES
/ W' H; G5 i$ _5 b3 Q4 Qtechnique appropriate to the specified level. Determine arsenic using the
5 C" Z' \9 n1 S, X0 Y5 e, _ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using; F9 j8 k$ x; D9 m' _/ L
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than% z% d" \0 ?% { ]# I
1 g. The selection of sample size and method of sample preparation; n! N, c# F& d0 ]9 ]1 L( L
may be based on the principles of the methods described in Volume 4.
) R6 R# Q! k; c1 DAluminium oxide Reagents and sample solutions
! {! S9 n% V; G2 x* r& K$ C. H0.01 N Zinc Sulfate6 l% ]! o4 Z# P" y2 ]: I' Y
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
% Z0 B4 W5 H4 Z6 C+ W% r& wmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
7 U) x4 F" r' E, D d4 \of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
! E5 Z. a3 c3 A( r! M- iconcentrated hydrochloric acid, heating gently to effect solution, then* L( s9 I# }$ c) P8 n+ j
transfer the solution into a 1000-ml volumetric flask, dilute to volume' v7 r- H) X3 K; }& b, S9 M# R
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
; m6 p2 J: u2 H) X% m0 [ml Erlenmeyer flask containing 90 ml of water and 3 ml of
7 Q7 U" g; ^# \& P* Q' Aconcentrated hydrochloric acid, add 1 drop of methyl orange TS and- l0 Y* A6 \) ]! Q, g/ J8 ?
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,8 _$ E0 q0 u! O2 Z: Y/ s1 P ~
dropwise, ammonia solution (1 in 5) until the colour is just completely
9 k5 L- j2 q; g3 \) S# u/ F/ z7 Wchanged from red to orange-yellow. Then, add:3 h% y( J7 a# W' y( A( p- L, Q0 H9 D
(a): 10 ml of ammonium acetate buffer solution (77 g of/ h6 W' }7 M) G9 t) Y% X$ o0 K
ammonium acetate plus 10 ml of glacial acetic acid, dilute to
6 X8 l H" ?9 v/ G8 U' U* t3 u1000 ml with water) and
3 I3 I& k e- b L(b): 10 ml of diammonium hydrogen phosphate solution (150 g$ J0 c# L: k$ E. m( @( O! q2 s/ x( P) ]
of diammonium hydrogen phosphate in 700 ml of water,
6 g: A% O/ y3 o/ `adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
, i0 }% i3 K% ^; r. ]2 [then dilute to 1000 ml with water).: w6 _! m# p, b% h
Boil the solution for 5 min, cool it quickly to room temperature in a/ I' |) P& l# W5 n! _& Z
stream of running water, add 3 drops of xylenol orange TS, and mix.
7 H3 F5 ^: e" z$ Z7 g/ {5 FUsing the zinc sulfate solution as titrant, titrate the solution to the first) A9 A. b% t4 ?. a( I1 x% ]! b3 ~7 z
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:5 l8 M- j4 h }
This titration should be performed quickly near the end-point by
o* u: M* T) Jadding rapidly 0.2 ml increments of the titrant until the first colour1 O. \' I% t$ j' t) f
change occurs; although the colour will fade in 5-10 sec, it is the true
) @4 U0 C/ B( X+ _end-point. Failure to observe the first colour change will result in an. ~, I! X& _$ [$ X! E% x% v: k
incorrect titration. The fading end-point does not occur at the second, a5 z7 W' q/ E. z3 g
end-point.)$ {$ z5 m. x& m# Z0 _
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a! m/ d. O' {, h& g- a E5 }8 F
stream of running water. Titrate this solution, using the zinc sulfate' v6 V4 s0 w& H( d! |2 y" W& i
solution as titrant, to the same fugitive yellow-brown or pink end-point+ z3 Z* a9 P( `& w7 q8 u3 A# u' f
as described above.
. n6 |, `0 s/ x1 q( a f; x* iCalculate the titre T of zinc sulfate solution by the formula:* v$ R. v3 G1 n: r
T = 18.896 W / V
* ^0 m$ o# S. `' Z- iwhere
1 F9 S2 P9 a7 c! BT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
- b) R( q" w G2 a5 Q% fW is the mass (g) of aluminium wire9 W, F, c! A* m* E/ O
V is the ml of the zinc sulfate solution consumed in the" l/ i: G8 h4 j0 t/ E
second titration# B' }8 R' Q* p0 Q
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and( a3 o- n0 C: ]) z1 H
R is the ratio of the formula weight of aluminium oxide to1 `" V& _! ^0 c1 w
that of elemental aluminium.
( ^+ L) H8 }0 f& I, d0 H: F7 \Sample Solution A9 b8 e1 Q" I. d& X% `4 a1 h
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica( R; r x+ m/ F0 G- a K* F% y
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
; l- C9 ^- N. a2 g" H(Note: Do not use more sodium bisulfate than specified, as an excess
. ], y; Q. E9 c* Z& g! s2 M+ o- sconcentration of salt will interfere with the EDTA titration later on in the' t, v& L* J. s8 | R9 k1 h
procedure.) Begin heating the flask at low heat on a hot plate, and
0 U3 z& p( A: Y% a( lthen gradually raise the temperature until full heat is reached.
6 O z) l7 `. V/ g9 I7 |% _(Caution: perform this procedure in a well ventilated area. ) When" L; H5 z# @, k8 ?9 g) X
spattering has stopped and light fumes of SO3 appear, heat in the full
6 s0 C4 y/ x* f. L5 hflame of a Meeker burner, with the flask tilted so that the fusion of the; n1 @2 i* a. _& _
sample and sodium bisulfate is concentrated at one end of the flask." L& h# z# m, r0 n- @+ A
Swirl constantly until the melt is clear (except for silica content), but
# x# d$ e& v# iguard against prolonged heating to avoid precipitation of titanium
8 ~2 j! q, u4 p, v' G! q) ~8 zdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
4 G' i M& C8 J7 `: Kthe mass has dissolved and a clear solution results. Cool, and dilute to6 _1 s @4 h( t3 f; _# Z
120 ml with water. Introduce a magnetic stir bar into the flask.6 s# M5 L# B+ V; y3 S
Sample Solution B0 F% \+ I- `% o2 W3 t
Prepare 200 ml of an approximately 6.25 M solution of sodium
- e* t! C% {* G: Nhydroxide. Add 65 ml of this solution to Sample Solution A, while1 E1 W" Y% G. q
stirring with the magnetic stirrer; pour the remaining 135 ml of the; \1 c q: y2 `2 M! H8 ~
alkali solution into a 500-ml volumetric flask.' B9 B: ^. t, J( t2 s
Slowly, with constant stirring, add the sample mixture to the alkali7 X8 D' d# b0 H5 F
solution in the 500-ml volumetric flask; dilute to volume with water,
! j3 x% W1 D2 s; Yand mix. (Note: If the procedure is delayed at this point for more than2 ]% K8 {8 V# g
2 hours, store the contents of the volumetric flask in a polyethylene7 J# k5 x/ }3 {, J, [6 J
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),5 M: H/ I3 T9 U# k
then filter the supernatant liquid through a very fine filter paper. Label
6 u) l- H" h- N* _, G3 S d5 D' _the filtrate Sample Solution B.- f+ n& n! r8 \: V1 R" c* z
Sample Solution C3 ~5 o- v" A2 b
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer- g2 H- W; X7 P7 C" {+ x9 H
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
: a: x; O4 B, t* d& T5 ysolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
7 V, t" m, d, m0 ~M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is1 W3 Z: }( c9 X% @1 }7 w0 w
known, calculate the optimum volume of EDTA solution to be added. v) r( C1 [# {7 l
by the formula: (4 x % Al2O3) + 5.]# c& J4 {5 ]+ \) R
Add, dropwise, ammonia solution (1 in 5) until the colour is just; p" N1 s: W$ Y6 F0 f4 W7 N
completely changed from red to orange-yellow. Then add10 ml each3 F5 r& D) B, {; Z
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to2 G/ l( |# S) I- K9 z& k X6 [
room temperature in a stream of running water, add 3 drops of xylenol! e- C$ B0 C, F. @2 o3 j
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
* ~5 |; b# i0 Q* l: abring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired4 l8 ~ k& N; {% c5 g# c" k7 a U# G
pH, a pink colour indicates that not enough of the EDTA solution has
1 }( @9 j* P8 [, [ [been added, in which case, discard the solution and repeat this
# d' t/ M1 _, X, r& i7 f1 b( c! bprocedure with another 100 ml of Sample Solution B, using 50 ml,/ K8 r# }. C; }' R _& Z
rather than 25 ml, of 0.02 M disodium EDTA.
9 n$ G0 v8 o- L' x& v( HProcedure" L8 ^/ O) F0 X3 g
Using the standardized zinc sulfate solution as titrant, titrate Sample# _- x {. q) R4 a' p. j$ ~, N
Solution C to the first yellow-brown or pink end-point that persists for; G1 f$ o/ n3 |
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first( `- {6 L8 u5 T4 r' {# ]8 Y w& z
titration should require more than 8 ml of titrant, but for more accurate3 p' f7 |6 M. u) c5 ]& A1 [
work a titration of 10-15 ml is desirable.; K- H+ s, ^4 w6 ?& h
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5+ C1 E l, ?' J; Y3 L9 w" H
min, and cool in a stream of running water. Titrate this solution, using m4 ]4 N* Z6 P6 X( X0 G
the standardized zinc sulfate solution as titrant, to the same fugitive
# V) ], q( U; w. Z! Kyellow-brown or pink end-point as described above.
% C! q I7 P/ ~# OCalculation:: K: }9 a1 x1 o7 _
Calculate the percentage of aluminium oxide (Al2O3) in the sample
4 C' \4 s3 ~: x* btaken by the formula:$ l# i: I, N7 |( N' E, c4 W
% Al2O3 = 100 × (0.005VT)/S
# X% c5 {+ h- S+ j) d$ G: Swhere; l& a8 P0 i1 R6 e7 w7 P
V is the number of ml of 0.01 N zinc sulfate consumed in
- t* P* P9 o3 _( t: z$ q. n6 }the second titration,
# C) L, t) l' f( fT is the titre of the zinc sulfate solution,3 w O$ H: ]7 k0 T6 y6 C: T
S is the mass (g) of the sample taken, and" r/ J/ F0 E4 M$ v
0.005 = 500 ml / (1000mg/g × 100 ml).
2 f3 X" f w% l% ]( e) G& lSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica" r! R( F8 n' _
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O). D7 g; V( d* R' b/ `
Heat gently over a Meeker burner, while swirling the flask, until* d3 S- u3 v- }& z
decomposition and fusion are complete and the melt is clear, except$ r6 k7 g8 A$ D- H
for the silica content, and then cool. (Caution: Do not overheat the' E, u5 ?) C! u
contents of the flask at the beginning, and heat cautiously during6 `/ O# h$ b# K$ n2 f; p
fusion to avoid spattering.)# | G% p5 H, _4 L" u; s6 l
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat, N: Q' p( D; q: p- c, \6 `9 g t
carefully and slowly until the melt is dissolved. Cool, and carefully add9 w( W6 E) f' Z7 g: i& r1 |% g
150 ml of water by pouring very small portions down the sides of the; [: W4 P) Z7 Z* h0 M
flask, with frequent swirling to avoid over-heating and spattering. Allow8 m8 C. g1 }( L+ z( z
the contents of the flask to cool, and filter through fine ashless filter4 C6 [! X2 v' ^. d
paper, using a 60 degree gravity funnel. Rinse out all the silica from
+ U( j' ~! e+ P. ?2 t+ c( uthe flask onto the filter paper with sulfuric acid solution (1 in 10).
: \4 a/ w6 _8 d/ y1 T" X4 u, JTransfer the filter paper and its contents into a platinum crucible, dry in
) y1 q) N+ g1 \an oven at 1200, and heat the partly covered crucible over a Bunsen
6 j9 y7 x+ q5 `% Mburner. To prevent flaming of the filter paper, first heat the cover from
( X/ j, ~% y* h1 M8 g5 pabove, and then the crucible from below.+ {( J+ \3 J! b: ? e' {- b
When the filter paper is consumed, transfer the crucible to a muffle
. E/ y/ b% A3 Ufurnace and ignite at 1000o for 30 min. Cool in a desiccator, and+ a7 `. [( W- R/ N+ t' r F* r
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated1 K* I* E; |& r6 a& D& R1 R p
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
6 N. d7 ~ |6 r( C$ f1 D4 K/ Uon a low-heat hot plate (to remove the HF) and then over a Bunsen
! s( Y. e) L) Q9 _/ tburner (to remove the H2SO4). Take precautions to avoid spattering,2 [0 M' y' a& k0 U6 k) j
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a! A, o* @3 ]; ?8 C* p$ |
desiccator, and weigh again. Record the difference between the two
$ s* D5 H7 M$ p5 g2 Kweights as the content of SiO2 in the sample.
/ r% c2 r! F; u1 E+ ~: `METHOD OF ASSAY4 _9 \! A4 I1 w8 ?2 E% F
Accurately weigh about 150 mg of the sample, previously dried at 105o) A. n$ A; t) M
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water% J B; @/ t) M; L% t- Z
and shake until a homogeneous, milky suspension is obtained. Add 30- o; E& E1 g- Y8 G
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
/ A: ?+ w8 W, ` m8 y# yheat gently, then heat strongly until a clear solution is obtained. Cool,: v# C: e, r2 s* J/ V5 W' v
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
9 M; c* Q* d, ~( {) Q0 u6 O) iacid, and stir. Add 3 g of aluminium metal, and immediately insert a
( }* y, G1 H0 |' Z) |rubber stopper fitted with a U-shaped glass tube while immersing the
6 U9 A3 X4 b; U# \; f6 oother end of the U-tube into a saturated solution of sodium: ]" c! m2 G2 t: q! }' D# g: |, r
bicarbonate contained in a 500-ml wide-mouth bottle, and generate3 b( l5 G% V+ ?9 g4 S
hydrogen. Allow to stand for a few minutes after the aluminium metal
! Y: D5 K; \8 k0 H+ ?has dissolved completely to produce a transparent purple solution.% v, @$ @ P! @: f# W7 l4 e9 t+ E
Cool to below 50o in running water, and remove the rubber stopper+ f" \9 m& v! M) p2 l% g7 V
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate$ a' F4 V0 l* q5 R3 @; i- |
solution as an indicator, and immediately titrate with 0.2 N ferric7 K' t7 r# o& D! Y ?
ammonium sulfate until a faint brown colour that persists for 302 m6 x: m7 n) d! I5 r
seconds is obtained. Perform a blank determination and make any
9 P( h% [$ h* u6 Onecessary correction. Each ml of 0.2 N ferric ammonium sulfate is0 b# K2 S w/ G) E
equivalent to 7.990 mg of TiO2.
6 | p" P% a( [2 _ |
|