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发表于 2008-5-23 12:10:00
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二氧化钛(钛白粉)
二氧化钛(钛白粉)
% q X( ], c% X: R( K) Q' x6 z% t/ G
JECFA关于二氧化钛(钛白粉)的结论
& d" S! x2 h m5 h9 Y* q% A6 m% A$ t* } r0 \' o: I
摘要: 2006年JECFA关于二氧化钛的结论
2 `0 K4 m( m3 a2 X e1 Q3 K: A6 wADI值:不作限制。
6 R. l% R9 S+ W5 ~8 o- P功能:着色剂
1 o% G; r+ m8 m8 t/ I0 A! x+ Y, Q5 V" J- E
TITANIUM DIOXIDE
6 L0 e$ }0 O4 r$ c7 e5 c& wPrepared at the 67th JECFA (2006) and published in FAO JECFA$ S: k) v. c* ^* r0 {
Monographs 3 (2006), superseding specifications prepared at the 63rd% B: e- {) h0 f- f
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
& L5 a N# `+ ~+ S( D7 }$ _; vCombined Compendium of Food Additive Specifications, FAO JECFA
5 H* S+ w! K: I9 @Monographs 1 (2005). An ADI “not limited” was established at the 13th3 x' M8 z' z" X; E. Z6 f
JECFA (1969).! Q! {' K" D" p# S) W1 V9 M
SYNONYMS
2 \2 l' v W2 p. @$ P. R4 {Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
1 O8 G; U: [1 a# \DEFINITION9 D. V1 a9 F' r: {
Titanium dioxide is produced by either the sulfate or the chloride- W: R+ |2 T$ b( J
process. Processing conditions determine the form (anatase or rutile5 f1 W) y0 n0 z6 N+ T; q
structure) of the final product.+ f2 I6 u# _& }. L! N
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)4 ] w& _# L, |' f8 h: k* U( ~4 V' T
or ilmenite and titanium slag. After a series of purification steps, the+ o) B0 X+ c5 B% f( B
isolated titanium dioxide is finally washed with water, calcined, and# ~4 h9 k- J1 y, |+ C T0 b
micronized.
6 R; k7 F O$ A7 S1 c" BIn the chloride process, chlorine gas is reacted with a titaniumcontaining
1 P/ [3 @0 D# mmineral under reducing conditions to form anhydrous
. @2 c( ~8 b L- x7 s7 o/ ktitanium tetrachloride, which is subsequently purified and converted to5 g& Q- N' z! L9 D5 | I; }
titanium dioxide either by direct thermal oxidation or by reaction with
6 Z' y& _: L* T6 C; ~6 l2 Lsteam in the vapour phase. Alternatively, concentrated hydrochloric
) B0 e" U: t3 e4 Aacid can be reacted with the titanium-containing mineral to form a
* x9 I- B/ U. F, ^# A/ {9 ^solution of titanium tetrachloride, which is then further purified and" G- ?$ i4 B& G- Q
converted to titanium dioxide by hydrolysis. The titanium dioxide is, p1 p& } }9 }0 n% R
filtered, washed, and calcined.
+ J3 a6 H8 Q. i( w N0 @, GCommercial titanium dioxide may be coated with small amounts of
2 l; _2 B% W2 [3 U' ^alumina and/or silica to improve the technological properties of the
4 l3 I9 ~! T& x- sproduct.& X+ D5 R2 f5 i) w- w: g
C.A.S. number 13463-67-7
$ v* T; o' h5 Z( p# _. D' RChemical formula TiO22 t( L! X( Z, K D; @
Formula weight
& p o5 q6 z. m5 V: T1 _2 X$ I" U6 H79.88% y$ a; y, @6 M' L
Assay0 `+ q# `% `2 e5 A
Not less than 99.0% on the dried basis (on an aluminium oxide and- M0 h8 n$ x k0 W
silicon dioxide-free basis); \7 \" F" c+ P' f; R$ t: e4 S
DESCRIPTION& k$ N4 ^, }; X3 z
White to slightly coloured powder- T% _ g# S6 X" K, Q5 m5 n8 l
FUNCTIONAL USES T2 J- [3 F' J! \) X2 U
Colour
8 N- C6 N+ L& a! w2 c' Z$ {1 KCHARACTERISTICS
% Y0 Q: ?* t# C% E0 s* hIDENTIFICATION
; O5 E E. ^" d/ xSolubility (Vol. 4)- T- B: R E8 o
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic; g- L- c6 Q+ O/ _
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
) G$ D( X4 |% \, y+ r, [. o4 z/ t2 ~sulfuric acid.
! {$ {/ ?: B+ P, k3 Z" vColour reaction x+ d1 R1 I X4 i8 ]( k
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
8 h3 |) W! c6 E$ u- w' J5 Hsulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
0 l& j8 w6 F" z3 zwater and filter. To 5 ml of this clear filtrate, add a few drops of
7 Q2 P* [6 }5 Q9 W* ~1 ]3 nhydrogen peroxide; an orange-red colour appears immediately.
& ?; U, h G) K2 b/ UPURITY. |& z. R1 Q) h2 q7 f2 _* n
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
! d7 m4 W8 L% P: lLoss on ignition (Vol. 4): H1 X) W' s0 h! _, c; X- [& u5 ]' u$ f$ G
Not more than 1.0% (800o) on the dried basis$ j: a! |0 p0 Z% K E
Aluminium oxide and/or9 E6 Z* [- U( k: O5 I% e9 |
silicon dioxide
- D9 k* S1 w3 o+ B- g! \8 r6 wNot more than 2%, either singly or combined5 v- m- {0 p4 k
See descriptions under TESTS
- z) l) p; G6 j1 n2 eAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
. |4 m8 s/ I1 w4 v, ]; T: z# Qalumina or silica.* U- b& L* x, e1 H( Y
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
4 g8 G( H3 _: t6 Y2 W6 q7 ]place on a steam bath for 30 min with occasional stirring. Filter( `' O" H7 Q$ v* y; Y
through a Gooch crucible fitted with a glass fibre filter paper. Wash, G; G& k( E" V( K
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
) G2 _2 }2 ^/ A7 {5 W/ jcombined filtrate and washings to dryness, and ignite at a dull red& l6 a( j9 c2 k- t( `4 o/ K
heat to constant weight.7 c( [$ p+ s5 t0 B. |
Water-soluble matter
4 q9 Y4 n9 {! z( M" h(Vol. 4)6 E& _/ g$ ]/ A0 U( T8 |5 o x
Not more than 0.5%
$ Q8 C& K; T8 U& i3 PProceed as directed under acid-soluble substances (above), using" J+ D* ~1 C, F8 o
water in place of 0.5 N hydrochloric acid.
) T1 V0 t* F7 b, GImpurities soluble in 0.5 N9 M# W% k5 Y# T9 t. h% v
hydrochloric acid2 J! Q" M- I3 t
Antimony Not more than 2 mg/kg
6 e+ [( i* g+ \' Q. r- J2 DSee description under TESTS
* Q% _/ `0 f& ~. Z1 c) g1 YArsenic Not more than 1 mg/kg4 c( u! _' `) K6 _
See description under TESTS
/ g V, V/ U5 _+ |/ C2 kCadmium Not more than 1 mg/kg3 B& {" E& } V: g
See description under TESTS
1 ]* q8 l6 |; B1 C% x% [Lead9 X7 k" _1 ` }1 Y
Not more than 10 mg/kg @5 [2 p7 f, j' S( ^
See description under TESTS
5 X: N$ E* G4 t+ k* ~8 X' zMercury (Vol. 4) Not more than 1 mg/kg
) d) ]# u. o1 D# {& w* }4 kDetermine using the cold vapour atomic absorption technique. Select a4 n \7 k( S, ]7 s
sample size appropriate to the specified level
: P/ ?( X! `, `0 m) D9 s9 DTESTS
# t9 u3 P0 U6 _+ `9 g" m3 s0 L4 yPURITY TESTS
8 _; X; j' L4 ~$ pImpurities soluble in 0.5 N
; i% B. i. p) G) l7 D+ `' O3 J, ahydrochloric acid. k$ m/ ]2 o$ @' A
Antimony, arsenic,
$ z9 N ^, \7 u) Scadmium and lead
. F+ a/ ?; _# l1 B; K! I(Vol.4)
* D/ f, k. ` {" PTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N7 ^% H g* P0 o/ u
hydrochloric acid, cover with a watch glass, and heat to boiling on a/ o2 D4 c8 s: h& k
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml9 d# x% j- g( T. `9 C
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
$ I, `4 o; ~% \# o' Vmaterial settles. Decant the supernatant extract through a Whatman
( R' \4 B( c- ?; o+ K' x2 G! _No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml/ l& }" N) r: j! [% ?1 u- F: O
volumetric flask and retaining as much as possible of the undissolved' S% E! y1 M9 q" ]5 d7 j
material in the centrifuge bottle. Add 10 ml of hot water to the original
& E0 ~( V5 [8 H* V1 Zbeaker, washing off the watch glass with the water, and pour the8 D/ q2 f: z" B6 D3 E5 B5 ?
contents into the centrifuge bottle. Form a slurry, using a glass stirring- ~0 G. Z6 h2 ~: D% i3 U. f
rod, and centrifuge. Decant through the same filter paper, and collect8 V( C$ Z) l+ T; j' I5 N) K* X1 j% f& p
the washings in the volumetric flask containing the initial extract.
! G3 j% C. d* m) f9 Y( lRepeat the entire washing process two more times. Finally, wash the( ~8 E6 R( u V& w) F# o0 g
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask/ F; P1 |! [4 O! j/ S
to room temperature, dilute to volume with water, and mix.
( m* h" b% X5 K! QDetermine antimony, cadmium, and lead using an AAS/ICP-AES
/ m5 W Y0 q( y L4 Ntechnique appropriate to the specified level. Determine arsenic using the0 H- s/ F, M: `6 u: o; {' v
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using# Z9 b* R7 k( c3 X2 \: q. a
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
$ P& R4 g) G" o. k$ O D1 g. The selection of sample size and method of sample preparation
, V0 Q0 n5 p7 R. e2 p7 g5 imay be based on the principles of the methods described in Volume 4.
k4 ~1 ^% [. f4 W5 K* R @Aluminium oxide Reagents and sample solutions7 L5 e0 S: a0 W# q% \
0.01 N Zinc Sulfate i- P$ E$ I4 I {7 ?' r. H! R
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to3 O# b% m+ D) |) H3 M5 F% W: w3 G
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg) x, a7 z' n1 ]" H' k
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of5 q: F0 [8 J& k2 ~+ n1 i) _8 M
concentrated hydrochloric acid, heating gently to effect solution, then; {1 d. v' V" x& v$ m
transfer the solution into a 1000-ml volumetric flask, dilute to volume
6 o- z! R* [1 p2 Ewith water, and mix. Transfer a 10 ml aliquot of this solution into a 5005 g* i% A' w' V' r
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
! l6 {. ~- t. h; D/ Bconcentrated hydrochloric acid, add 1 drop of methyl orange TS and0 `. d' v: d' B9 ?9 K2 q- P3 t
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,$ Q% j8 _& x8 D! ~0 M
dropwise, ammonia solution (1 in 5) until the colour is just completely* m; ?! j! G, `6 f @9 q
changed from red to orange-yellow. Then, add:
, e) R+ N0 H( S6 M- \! k(a): 10 ml of ammonium acetate buffer solution (77 g of3 Q! q" W* A& y+ ?9 W5 q
ammonium acetate plus 10 ml of glacial acetic acid, dilute to/ @" _3 U1 B: r& s E6 T- h! S
1000 ml with water) and2 w. s6 l* v7 G3 Z
(b): 10 ml of diammonium hydrogen phosphate solution (150 g4 U% w! A4 P8 W) _% q0 |: _
of diammonium hydrogen phosphate in 700 ml of water,
4 @; ^3 R3 i0 W0 W6 m" w& xadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,. R8 Q4 q" ^* l8 |
then dilute to 1000 ml with water).
+ N3 G: Z+ v0 oBoil the solution for 5 min, cool it quickly to room temperature in a
8 T( X8 A# O p9 W7 @# rstream of running water, add 3 drops of xylenol orange TS, and mix.. p* c6 h6 ^* S8 d$ e! i
Using the zinc sulfate solution as titrant, titrate the solution to the first" l: \- `' y/ z6 ~0 ]% f0 H
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
s( |# h s% M0 V; gThis titration should be performed quickly near the end-point by0 I. z) G8 I/ f" U) l6 {( S: T, U
adding rapidly 0.2 ml increments of the titrant until the first colour! x! s. s5 L' L1 z; @
change occurs; although the colour will fade in 5-10 sec, it is the true$ U: ]. f9 S' i E
end-point. Failure to observe the first colour change will result in an/ _; R+ B( Z. e8 l4 J. r6 F
incorrect titration. The fading end-point does not occur at the second
9 a3 x9 ~* _' ]8 ^3 uend-point.)9 H2 T5 Q) u5 J! W
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
h: X) x# `: P1 Tstream of running water. Titrate this solution, using the zinc sulfate
* [4 @ F" G/ v, V$ W: q- [solution as titrant, to the same fugitive yellow-brown or pink end-point, ^ C2 i( [. J; S+ E# }
as described above.
/ ~( j+ H# I. H% {: RCalculate the titre T of zinc sulfate solution by the formula:
' f# a; u1 P( A( }: D# V( n2 Y1 _T = 18.896 W / V& C ?! `8 M! T3 d0 p. \
where
" q. ^( y7 _3 U* [$ g4 U; s9 U: }) NT is the mass (mg) of Al2O3 per ml of zinc sulfate solution! V1 \+ F5 v* k$ i i( q! h' J* _
W is the mass (g) of aluminium wire
! a; u4 p- j/ r2 JV is the ml of the zinc sulfate solution consumed in the
) u9 P! a% W9 j. C& I4 \- Y. asecond titration
6 S) K6 Z8 y, {: R1 z# O; \18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and3 ]$ o, t4 R% o9 `
R is the ratio of the formula weight of aluminium oxide to `% R, N1 x* \
that of elemental aluminium.
) ]3 z+ C4 j* x% Y! ISample Solution A# J2 i9 m7 U6 M
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica c% B+ \2 F, j
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
, p; L# h% \! a2 a+ a2 B' L(Note: Do not use more sodium bisulfate than specified, as an excess
! b+ ?2 K9 u( v6 a% g: Mconcentration of salt will interfere with the EDTA titration later on in the
/ y) ]8 Z# s: ^$ I+ Cprocedure.) Begin heating the flask at low heat on a hot plate, and$ b4 B8 a( B2 c5 h- @( d
then gradually raise the temperature until full heat is reached.
" N0 L- A. I( ~0 V) P(Caution: perform this procedure in a well ventilated area. ) When- ]6 R7 j( t4 _1 n) w# C
spattering has stopped and light fumes of SO3 appear, heat in the full
+ q2 t9 w' y2 ]/ _1 _0 cflame of a Meeker burner, with the flask tilted so that the fusion of the5 h0 b/ [, c, ?+ r
sample and sodium bisulfate is concentrated at one end of the flask.
4 v3 D8 C. z; n1 @8 m: B- @ F" Z/ wSwirl constantly until the melt is clear (except for silica content), but# T8 G6 @3 i" g3 J, n: H' |. G
guard against prolonged heating to avoid precipitation of titanium$ v" b! A( o7 N: j, ~+ T0 ?* F
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
! `' C5 M; P# t0 D8 X. x% q8 Ythe mass has dissolved and a clear solution results. Cool, and dilute to
3 N1 B6 G9 w3 i0 a* k120 ml with water. Introduce a magnetic stir bar into the flask.
" K/ }+ }9 r5 c) X: l. t3 M7 c" wSample Solution B4 m0 Q5 u. F9 j6 z0 Q! Z% x
Prepare 200 ml of an approximately 6.25 M solution of sodium2 |; V, N5 w3 |& u$ z. [
hydroxide. Add 65 ml of this solution to Sample Solution A, while
. F4 q+ y' q, `+ X) {) [stirring with the magnetic stirrer; pour the remaining 135 ml of the
, L N: s. H% ~+ `8 ]4 S5 l4 [alkali solution into a 500-ml volumetric flask.1 k% P% Q; x g
Slowly, with constant stirring, add the sample mixture to the alkali+ m3 _) Z) U# M% s/ p$ L/ D
solution in the 500-ml volumetric flask; dilute to volume with water,
" s0 A4 i$ Q, J- t5 [& q: sand mix. (Note: If the procedure is delayed at this point for more than" W i# y2 m2 n: Z' Z
2 hours, store the contents of the volumetric flask in a polyethylene! h1 r& q n3 S& M# m [ K7 B
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
1 }& C9 {1 ^- R9 ?7 r* Vthen filter the supernatant liquid through a very fine filter paper. Label& `. ?. E2 `; Z( B, U! [" Y# n
the filtrate Sample Solution B.
% w6 h0 \$ q8 j2 f' uSample Solution C/ C: s7 m% ~ J7 P. H, S: N
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
9 \2 I3 n+ T( x$ aflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
) p( D* }- ?/ Usolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
0 Q4 `3 e- z: w$ UM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is4 P1 z. ~2 {& f; [
known, calculate the optimum volume of EDTA solution to be added( B, v: [& `4 p4 `
by the formula: (4 x % Al2O3) + 5.]' J% K% i: t+ [, @
Add, dropwise, ammonia solution (1 in 5) until the colour is just- z0 S( [0 W) Q8 I Z4 N+ k8 C0 |
completely changed from red to orange-yellow. Then add10 ml each0 ~. J+ p2 L, F) j* N
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
6 f; f+ T6 b. p% Droom temperature in a stream of running water, add 3 drops of xylenol' Z6 p% y) V0 a/ H
orange TS, and mix. If the solution is purple, yellow-brown, or pink,! N1 X- z A2 r& z% S9 j
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired. R0 T7 t {0 p! N" N& p0 n1 R! V
pH, a pink colour indicates that not enough of the EDTA solution has9 h8 R' S4 J6 B) d, Q s3 C1 g
been added, in which case, discard the solution and repeat this
' `2 j" j8 q' G" O: uprocedure with another 100 ml of Sample Solution B, using 50 ml,* S) e2 C) w K5 Z) e9 S
rather than 25 ml, of 0.02 M disodium EDTA.
( P4 H# _8 T# [" r2 b3 cProcedure- x- o- c8 L3 @% b7 ~- g' y; Z
Using the standardized zinc sulfate solution as titrant, titrate Sample
5 |7 P& \9 e1 O& z& [Solution C to the first yellow-brown or pink end-point that persists for
4 N: k# T2 P& n! N( I8 S5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first3 B5 t( h# f' G4 N. L
titration should require more than 8 ml of titrant, but for more accurate
8 R( A$ c# ?% J1 ~3 E( cwork a titration of 10-15 ml is desirable.( `0 e' }* l e2 v% g5 L
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-58 X8 B( V+ g( k1 U& a
min, and cool in a stream of running water. Titrate this solution, using4 [$ L" w2 b5 {( `" j* D3 h) e
the standardized zinc sulfate solution as titrant, to the same fugitive
8 O7 Q5 b$ q$ E' Z. V ~yellow-brown or pink end-point as described above.
: y7 r- z1 B# o; ] {! eCalculation:
% q. w# }7 {. v! R p- yCalculate the percentage of aluminium oxide (Al2O3) in the sample
/ W( _1 M4 x: ?! g( ?taken by the formula:
4 J% l. r. |* I3 C5 _7 t% Al2O3 = 100 × (0.005VT)/S9 F% Z9 w6 I8 d* F
where& t9 i2 v; V; i$ c2 ~% R: M
V is the number of ml of 0.01 N zinc sulfate consumed in
# u: p) O8 U* A7 q! _the second titration,
5 s8 @+ r# t# G- b6 ]! WT is the titre of the zinc sulfate solution,
& V$ d/ Y; ]' B! p1 C6 J4 ^5 C- ^S is the mass (g) of the sample taken, and
; w; c a* y) _& a* R0.005 = 500 ml / (1000mg/g × 100 ml).! q1 ] l0 T( p1 v; [( G
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
1 E( F& I6 Z8 j Yglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).. Q2 r; ~2 v" j3 e2 C! Z6 j* `
Heat gently over a Meeker burner, while swirling the flask, until
6 @& E- d$ M- j; q# odecomposition and fusion are complete and the melt is clear, except
( F( ~' E+ k- L0 K4 d/ F$ p% _- R6 Gfor the silica content, and then cool. (Caution: Do not overheat the, k+ ? I% R/ t" W {7 j: f9 x' N4 @8 `
contents of the flask at the beginning, and heat cautiously during
7 \) ?. L8 G1 D0 \* m1 U* g6 a/ ofusion to avoid spattering.)# B! o! ]0 Y! g# U& G" ~2 X; n& x
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat! F0 b6 Z- d. _3 s+ I% M
carefully and slowly until the melt is dissolved. Cool, and carefully add
& [# E6 B4 q/ @) Z3 R" a) Y150 ml of water by pouring very small portions down the sides of the
9 C/ e* g7 b) Gflask, with frequent swirling to avoid over-heating and spattering. Allow x6 ^3 I4 j) D; L$ E' a3 z% {
the contents of the flask to cool, and filter through fine ashless filter4 Q# H B1 @2 o$ R7 G$ {% j. [% ~
paper, using a 60 degree gravity funnel. Rinse out all the silica from1 D5 m; R- M6 P$ t( W
the flask onto the filter paper with sulfuric acid solution (1 in 10).
4 c3 `9 c6 O7 g. \- BTransfer the filter paper and its contents into a platinum crucible, dry in& m$ @. E& E' o
an oven at 1200, and heat the partly covered crucible over a Bunsen' [* e$ R* ^, f4 T" [
burner. To prevent flaming of the filter paper, first heat the cover from( B: |! O; f) A) Y4 s5 ?1 P5 n, G5 D) C
above, and then the crucible from below., j! i# h) z: Q7 J
When the filter paper is consumed, transfer the crucible to a muffle
4 J6 U5 t8 L8 o2 sfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and& F4 O! M4 M8 K: Z& ~' O
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated; o: W6 q& c$ P2 U0 {7 ]0 N' Z# n3 n
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
5 R/ Q0 L' O! T3 x9 ^4 oon a low-heat hot plate (to remove the HF) and then over a Bunsen- p( w- ]; `, z1 S/ @/ m5 p8 l5 Q+ D
burner (to remove the H2SO4). Take precautions to avoid spattering,( p, M! L, t$ P& J: j* {% }
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
% }5 \& M/ E! G9 Xdesiccator, and weigh again. Record the difference between the two( Y% M$ E( I5 P3 ~
weights as the content of SiO2 in the sample.6 M9 Q. `! J6 d& P/ f6 N
METHOD OF ASSAY
* Y% _" X8 {; H- VAccurately weigh about 150 mg of the sample, previously dried at 105o/ d3 }/ \+ l! ~8 J; i( K
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water; R( q0 N- X2 K5 m% ?6 l1 Q) B
and shake until a homogeneous, milky suspension is obtained. Add 30# y& t8 ?* U9 |8 Z* _
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
8 c1 d' S6 R( C( d6 A; M) Zheat gently, then heat strongly until a clear solution is obtained. Cool,
+ W& E2 w* `) I4 E* Hthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
f# ~' N! \! q8 r1 _$ Pacid, and stir. Add 3 g of aluminium metal, and immediately insert a
2 K4 l: Y; t3 {, X7 B$ p9 P+ d* qrubber stopper fitted with a U-shaped glass tube while immersing the
1 x& D- w" r5 ?other end of the U-tube into a saturated solution of sodium3 H! y/ q, i" h) b S1 q- M
bicarbonate contained in a 500-ml wide-mouth bottle, and generate8 ]& ^; w l7 f/ f/ R
hydrogen. Allow to stand for a few minutes after the aluminium metal' S2 V- L4 W# M% }6 T- q
has dissolved completely to produce a transparent purple solution.
; H, `% a5 F' D" }0 @' m/ ^Cool to below 50o in running water, and remove the rubber stopper [8 n! F8 t8 ?* j% e2 r
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
7 T8 a2 Y! @2 [solution as an indicator, and immediately titrate with 0.2 N ferric. F) y; u6 z$ S- c
ammonium sulfate until a faint brown colour that persists for 30- n" B7 ], e2 e
seconds is obtained. Perform a blank determination and make any) X0 w. z1 t" s' }6 M& ?9 C5 {) M
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is& l3 ~, \ K- H0 b# h8 O
equivalent to 7.990 mg of TiO2.
: L- V4 l5 w/ v7 X I$ z |
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