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二氧化钛(钛白粉)
二氧化钛(钛白粉)+ I) D2 _* L1 N: W
, H5 c( s( p! N1 \5 Z |0 z
JECFA关于二氧化钛(钛白粉)的结论
|+ c8 X" J$ e* r- K' b8 H k+ q% a0 m H! ?8 s, {
摘要: 2006年JECFA关于二氧化钛的结论+ N. S" ?7 |" W. k1 C
ADI值:不作限制。
, s' W7 j8 E3 M% Z0 Q7 ]7 J功能:着色剂
3 n$ r4 R8 @5 Y1 e, `0 g5 W& L0 F! @& r% ~1 |
TITANIUM DIOXIDE3 q$ L+ Z. p9 [. T. j0 V+ g
Prepared at the 67th JECFA (2006) and published in FAO JECFA9 ?8 @5 d9 H+ x# g
Monographs 3 (2006), superseding specifications prepared at the 63rd
" \ ~! V. y* s qJECFA (2004) and published in FNP 52 Add 12 (2004) and in the- @+ c1 b6 r9 t1 H0 }
Combined Compendium of Food Additive Specifications, FAO JECFA
3 W1 G4 k' Q3 J4 e dMonographs 1 (2005). An ADI “not limited” was established at the 13th
+ r* I3 N; `3 E8 j# ZJECFA (1969).
! W, A& z- F9 p; ySYNONYMS
( s9 W2 E/ d/ ~6 F: [' F* v" tTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 1719 K# e( _* _/ [0 u
DEFINITION
" y1 ~/ q7 m( J3 V0 bTitanium dioxide is produced by either the sulfate or the chloride
+ z; w, s, ?0 y+ {- qprocess. Processing conditions determine the form (anatase or rutile
& q, x9 E7 l# g* M- k2 Xstructure) of the final product.
9 \" U% S: w, [. I5 x8 k0 _9 X3 pIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
% a( ~# L4 @: A K/ Ior ilmenite and titanium slag. After a series of purification steps, the0 V% J1 n \. R& c4 f' P: a
isolated titanium dioxide is finally washed with water, calcined, and6 D; o- e" {% ^! u3 A
micronized.; s$ \: F. t: q3 Y c, k2 q% D
In the chloride process, chlorine gas is reacted with a titaniumcontaining/ `- \) Q: n' A! p# e' N/ H
mineral under reducing conditions to form anhydrous
% X8 J* ?2 a9 o$ o6 c$ d5 ^( ktitanium tetrachloride, which is subsequently purified and converted to4 [# {. @% h/ _ x0 x0 ~% I+ a
titanium dioxide either by direct thermal oxidation or by reaction with
4 n6 a" | `. c3 W( m8 j' d2 bsteam in the vapour phase. Alternatively, concentrated hydrochloric
) {2 H$ a Y& t9 B* racid can be reacted with the titanium-containing mineral to form a
( k* B6 ?+ ~% c/ d A' v2 B N" T$ wsolution of titanium tetrachloride, which is then further purified and) V* k- j* q2 Z9 H5 [
converted to titanium dioxide by hydrolysis. The titanium dioxide is9 @: V/ E9 ]5 F6 l! m
filtered, washed, and calcined./ ?( p: W: @* P) w* Y. {& R4 X \5 E
Commercial titanium dioxide may be coated with small amounts of( N1 y% z% j+ a4 `- N
alumina and/or silica to improve the technological properties of the
& r) W5 {. U! z" a8 y' M( |) Bproduct.
# _5 f+ r( H# \2 s3 a# t3 E6 m0 h2 ^C.A.S. number 13463-67-7) y( I4 } r4 q
Chemical formula TiO2
! z2 B7 p1 S6 v' _0 V4 M; S! oFormula weight! }: d* n! b. K& m1 ` C
79.882 a; n0 a/ S! W7 t+ Q
Assay. w& J( D9 W5 F$ m7 Y1 r# {
Not less than 99.0% on the dried basis (on an aluminium oxide and
0 o; @+ G2 V. l3 j) {9 csilicon dioxide-free basis)! ^6 w$ \) ]" e2 a
DESCRIPTION
4 `1 x# e- J" o7 U, LWhite to slightly coloured powder! D% M; E" Z% W" B8 f
FUNCTIONAL USES# y! D v2 ?1 K1 d1 E
Colour, k# P( s& L, o S9 \% @. m1 c
CHARACTERISTICS' ^* N+ |# R9 B" W& b
IDENTIFICATION! f, T* J9 J' o. g7 \
Solubility (Vol. 4)
; Z: {+ B, v: t; d, e% l6 ?Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
% _/ j; A- x. w! B3 M4 ?4 vsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated3 A4 l5 k+ x; v4 P7 w
sulfuric acid.
. q6 S; q4 J1 c( x$ VColour reaction
7 z& A; M" {" \7 r- W% C3 {( MAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of" A7 v6 w! d, s* [2 W8 v
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with: \9 ^! a$ o& N2 G7 [; o4 N! y* j
water and filter. To 5 ml of this clear filtrate, add a few drops of
4 W) P& ^8 c/ f4 O6 D, d" H) Vhydrogen peroxide; an orange-red colour appears immediately.
5 H8 H& [& J% y8 G! HPURITY
8 l4 d S: F6 [/ F5 vLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
5 N, `. x: h: V r. i, x0 RLoss on ignition (Vol. 4)
, g8 L! @! m* W$ {! N8 M3 Y9 dNot more than 1.0% (800o) on the dried basis2 B2 G0 a z) Q5 x# Y
Aluminium oxide and/or$ M; m1 f) C- J# r0 E: k5 B
silicon dioxide
/ j. ?0 W" V7 J& x" G" C6 DNot more than 2%, either singly or combined
Q5 s6 j) J7 vSee descriptions under TESTS
* }0 y0 z* u% IAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing2 F# \ w# O3 r6 H( ]. ?+ n
alumina or silica.( W" i9 N- x/ v; I a% q6 o
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
% `2 k$ h) _/ j3 x$ }place on a steam bath for 30 min with occasional stirring. Filter3 J/ h$ L7 Q$ |. t0 a
through a Gooch crucible fitted with a glass fibre filter paper. Wash
: K6 j# l H7 }with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the! C3 `- p# R& `! D. {6 v* }$ S
combined filtrate and washings to dryness, and ignite at a dull red$ P R/ W+ n9 _7 c
heat to constant weight.% V7 J7 K3 K: l" N( W7 K* U. i# s
Water-soluble matter
3 l: A; T3 F/ l7 L$ n5 `% c, q(Vol. 4)9 n; D+ X0 o8 o" X# `
Not more than 0.5%
4 j. e# M# S% u. s4 i" k/ lProceed as directed under acid-soluble substances (above), using3 A& ]6 ^& c0 q4 z( B
water in place of 0.5 N hydrochloric acid., g" y8 R$ g' f, \; p) b4 }2 Y
Impurities soluble in 0.5 N
( K% a, \1 J6 nhydrochloric acid; k# _5 K, U3 H$ s$ n' K0 q
Antimony Not more than 2 mg/kg/ C5 |! x6 u' @0 L2 j
See description under TESTS
: d+ s$ ^ u5 q2 zArsenic Not more than 1 mg/kg0 f1 r' @3 w5 k9 g& V+ w+ H
See description under TESTS* @5 T6 K4 N0 Z5 {
Cadmium Not more than 1 mg/kg
- T1 k9 u' v9 `+ Y5 L% TSee description under TESTS A, K7 t4 }, f3 z R5 o
Lead5 i0 B$ |1 @7 f5 P' _1 X& p) ]
Not more than 10 mg/kg
5 z8 ?$ [7 h. U/ QSee description under TESTS. f( j9 W, d& e
Mercury (Vol. 4) Not more than 1 mg/kg
# L$ K- p, l* F% E3 D9 y0 e1 vDetermine using the cold vapour atomic absorption technique. Select a
9 U3 M7 U; ]2 {% @sample size appropriate to the specified level" j" @8 [- p9 ?0 D6 C) s7 I3 ^
TESTS
4 m& F- M+ k9 ?8 S9 i8 C8 H5 }PURITY TESTS
; X$ U0 @% ^+ o ]0 u! lImpurities soluble in 0.5 N0 H* _+ J4 t( l/ [0 `: i1 w
hydrochloric acid# s) S7 j# I! K9 `
Antimony, arsenic,
8 O- d" j2 v A- i9 wcadmium and lead
, ^$ o, ` ^: Y+ b+ n3 t(Vol.4)
' C4 ^8 ?1 S" g5 ~Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N/ e1 W( b) E1 r9 o0 Q3 B" W+ J' P
hydrochloric acid, cover with a watch glass, and heat to boiling on a7 ^# i( q) G: {8 G. l, `( d
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
4 D7 }" h' t4 d* Y4 Ucentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved/ U& F6 b* c6 z/ d3 @+ ~( A Y. W
material settles. Decant the supernatant extract through a Whatman$ d+ d- x0 q W
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
# P- x: }) p% z6 E+ s4 Qvolumetric flask and retaining as much as possible of the undissolved
, ?* {0 i& e1 z4 C! {9 W4 R R4 r9 j& Nmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
, S" B6 R" `) E Q7 ]! w8 ]beaker, washing off the watch glass with the water, and pour the4 X! Q/ Y+ X+ v9 M
contents into the centrifuge bottle. Form a slurry, using a glass stirring
' |8 Q& k+ C- o* l% ?rod, and centrifuge. Decant through the same filter paper, and collect# Z+ m( X3 P0 U2 o+ ?1 S) R
the washings in the volumetric flask containing the initial extract.
. K/ I+ d; v* J3 @0 b# aRepeat the entire washing process two more times. Finally, wash the
% J0 a6 f F5 N- { lfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask
4 X R% ]$ s! `' ~. V6 m+ Wto room temperature, dilute to volume with water, and mix.& y2 |( \, }5 s5 P4 v4 m# h7 H w1 M
Determine antimony, cadmium, and lead using an AAS/ICP-AES& ]0 X* M% n9 P+ {! L0 Z
technique appropriate to the specified level. Determine arsenic using the
' j5 P% s, o, R/ B# a- w) aICP-AES/AAS-hydride technique. Alternatively, determine arsenic using @% W6 G; b3 |: @3 d
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than( L1 k" O- i5 { A, [" F! |
1 g. The selection of sample size and method of sample preparation
; g1 c: l/ L, U6 Lmay be based on the principles of the methods described in Volume 4.
1 R- p g& I$ t. eAluminium oxide Reagents and sample solutions
$ ?- r- W( X9 D) ?3 P6 ]4 v0.01 N Zinc Sulfate# v7 [, f! q* L4 m
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to7 w; s. N7 E4 T$ U
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg1 d1 [3 ~" O; F
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
; l8 z8 A7 E% } z; aconcentrated hydrochloric acid, heating gently to effect solution, then
' b8 x9 _/ H' X6 B8 _transfer the solution into a 1000-ml volumetric flask, dilute to volume
( [( P T. k0 j" z d2 y: Y: ~with water, and mix. Transfer a 10 ml aliquot of this solution into a 500
6 X! `, {3 [+ v6 `5 Sml Erlenmeyer flask containing 90 ml of water and 3 ml of$ J) ^- k( z, o8 g
concentrated hydrochloric acid, add 1 drop of methyl orange TS and% a+ r- s# W( G! `2 y' |) n
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
6 |( b8 P/ k K/ ~8 U" ldropwise, ammonia solution (1 in 5) until the colour is just completely
9 Q8 `6 \2 w* ^2 xchanged from red to orange-yellow. Then, add:8 y- \/ o3 O. v# C. c9 K |
(a): 10 ml of ammonium acetate buffer solution (77 g of
1 ?) v$ Y6 Q: @) Iammonium acetate plus 10 ml of glacial acetic acid, dilute to! }8 b" h6 F* P
1000 ml with water) and
8 v$ j8 ~. \; p& J' ^& M/ J(b): 10 ml of diammonium hydrogen phosphate solution (150 g
6 Z! ]2 |8 y0 ], O- i/ bof diammonium hydrogen phosphate in 700 ml of water,* V! f j3 h8 y/ m* C$ E$ k* R
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,8 A2 b3 X% [( r" a9 ?; _! c$ w
then dilute to 1000 ml with water).
: Z& b @1 M5 _% P; E. |% KBoil the solution for 5 min, cool it quickly to room temperature in a& H9 I) k5 g: C
stream of running water, add 3 drops of xylenol orange TS, and mix.
2 Y% o7 o& `4 R* K: SUsing the zinc sulfate solution as titrant, titrate the solution to the first V) G2 f% r, I" c
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
6 `7 }/ k4 i7 P) }9 uThis titration should be performed quickly near the end-point by
0 C8 G- }, g$ A K% N8 |adding rapidly 0.2 ml increments of the titrant until the first colour& z5 P9 y" n1 k! P1 f& d
change occurs; although the colour will fade in 5-10 sec, it is the true S5 H8 U T: u* I- v
end-point. Failure to observe the first colour change will result in an
& v0 Y/ H6 f% j# H2 sincorrect titration. The fading end-point does not occur at the second4 z' Q. B( y, y( P+ ^
end-point.)
7 ?) ?0 h5 H1 p4 BAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
" p2 @3 P/ b/ p1 x5 I+ R4 dstream of running water. Titrate this solution, using the zinc sulfate0 p+ H) i1 Y8 v2 A3 V! ]
solution as titrant, to the same fugitive yellow-brown or pink end-point
; `5 V' |. A' d7 ias described above.
q+ W* \9 K5 m2 W8 A/ uCalculate the titre T of zinc sulfate solution by the formula:: _6 `3 j! P. u- t) W( j
T = 18.896 W / V, v- M/ r" ~; ]/ z
where
8 v/ ~' @4 Y/ xT is the mass (mg) of Al2O3 per ml of zinc sulfate solution) b7 V0 a4 X" S* V9 I; |; h
W is the mass (g) of aluminium wire4 q- J1 g% O6 D! `
V is the ml of the zinc sulfate solution consumed in the
$ V' J0 N; n, H! E- ?' |4 ?* {second titration
: B4 w! K, I! D18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
+ F; t5 p3 j1 m4 s: CR is the ratio of the formula weight of aluminium oxide to- t% q/ ~! F" d
that of elemental aluminium.
9 X; ^7 ?8 p4 V; Y! RSample Solution A
# T' R7 e6 } {% M- _& eAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica8 j7 k( C2 h, e
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)." j# p' k! k+ Z2 V3 z
(Note: Do not use more sodium bisulfate than specified, as an excess
+ j7 [+ C: p2 l2 jconcentration of salt will interfere with the EDTA titration later on in the
. X o, h8 l; G5 Iprocedure.) Begin heating the flask at low heat on a hot plate, and
0 G, e7 [. Y0 N/ `1 M- e. |( X% O" Lthen gradually raise the temperature until full heat is reached.. c6 S( }2 @2 d
(Caution: perform this procedure in a well ventilated area. ) When' i9 q8 t- J0 E. Z; I0 n' r
spattering has stopped and light fumes of SO3 appear, heat in the full
* e# m$ q4 \: w6 I, }4 N6 L' Jflame of a Meeker burner, with the flask tilted so that the fusion of the
, U5 s& ]( j9 }sample and sodium bisulfate is concentrated at one end of the flask.
$ u4 K8 y7 h0 i7 P" `3 ~2 q7 b9 f) XSwirl constantly until the melt is clear (except for silica content), but! S2 R% L; |9 d; L1 C( {3 t
guard against prolonged heating to avoid precipitation of titanium6 z9 m, v9 l/ L
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
% b, J4 L/ ]; F! W- J+ U! Lthe mass has dissolved and a clear solution results. Cool, and dilute to
( f1 Q& h+ ^4 ^# ~; t) I( v7 Z120 ml with water. Introduce a magnetic stir bar into the flask.
& J$ ?, N( j, T' ySample Solution B# |$ x* e. h) Q0 T: S$ K7 N C
Prepare 200 ml of an approximately 6.25 M solution of sodium
% M6 s! T3 J7 A" Rhydroxide. Add 65 ml of this solution to Sample Solution A, while
+ l/ A! Z! x" Y# `6 U' R. a0 ^" Istirring with the magnetic stirrer; pour the remaining 135 ml of the2 ^3 V! p, f3 Z' x+ q! e$ ]1 r! y
alkali solution into a 500-ml volumetric flask.
' B2 d' _4 f+ u; B4 T! OSlowly, with constant stirring, add the sample mixture to the alkali
4 e0 ^, [1 B+ N$ bsolution in the 500-ml volumetric flask; dilute to volume with water,5 ^- F' C6 F& V" F+ q5 Z
and mix. (Note: If the procedure is delayed at this point for more than3 ~* j) Z. \, h/ d X, A, x
2 hours, store the contents of the volumetric flask in a polyethylene- Z- ]$ e# i# ]* x' X
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),7 T2 R4 A$ N! g0 P+ y0 D
then filter the supernatant liquid through a very fine filter paper. Label3 X( T8 {; M8 {& `- r
the filtrate Sample Solution B.
2 Y0 R) \: G8 e( x k) wSample Solution C
4 J( J- `, B5 ^Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer- y) U: m4 n4 z! U
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
! e6 _* C3 M( C3 D( Hsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
' ]+ G9 W' D- s( p, UM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is- ~. O+ r: Y6 d4 k k* R
known, calculate the optimum volume of EDTA solution to be added
- Q& g! T9 F+ \; Z0 w; eby the formula: (4 x % Al2O3) + 5.]0 e" Q0 ~; A# O
Add, dropwise, ammonia solution (1 in 5) until the colour is just+ M$ G6 Y J" o: n
completely changed from red to orange-yellow. Then add10 ml each
. _8 D# q2 M" m, b* k1 C, q% fof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to9 y7 G) C0 Q$ ]
room temperature in a stream of running water, add 3 drops of xylenol6 {& x4 `; [4 u" C
orange TS, and mix. If the solution is purple, yellow-brown, or pink,3 ]* k1 C" Q+ V9 s- w" X; c) L. A
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
. U$ X# I& Q" I, h! XpH, a pink colour indicates that not enough of the EDTA solution has
: T0 x) ^! ^. r8 G! V5 i/ Y2 T- c2 {been added, in which case, discard the solution and repeat this: y$ _1 G9 m+ w( q
procedure with another 100 ml of Sample Solution B, using 50 ml,
% l/ ^# L- b2 Wrather than 25 ml, of 0.02 M disodium EDTA.* q! a, k+ a7 |1 ]2 {
Procedure
2 c: E% x# f( Y0 Y2 K! i9 KUsing the standardized zinc sulfate solution as titrant, titrate Sample q8 p4 c; K: u5 D1 _
Solution C to the first yellow-brown or pink end-point that persists for
# Y. i3 W6 P r9 u4 s( \' B5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
$ N6 s ~3 ?& c0 S& T# utitration should require more than 8 ml of titrant, but for more accurate! l; H% G3 L( j, [
work a titration of 10-15 ml is desirable.
4 e! c V" t7 Z7 g6 |. M3 BAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
1 q8 T, m: _+ Y3 ~/ h- |min, and cool in a stream of running water. Titrate this solution, using
2 h* L2 s- x% u! Cthe standardized zinc sulfate solution as titrant, to the same fugitive/ Q" K+ y3 F( T9 _9 D# N
yellow-brown or pink end-point as described above.
2 L- S4 f# T: D \7 VCalculation:
6 |! Y: j% Z$ s" N [' OCalculate the percentage of aluminium oxide (Al2O3) in the sample
& l: z2 b& y4 j3 U7 Xtaken by the formula:
6 q& [1 T/ \9 H% Al2O3 = 100 × (0.005VT)/S/ Q( A; [ E2 s1 \0 |5 @1 ?: `
where
8 y( J/ ~$ P( WV is the number of ml of 0.01 N zinc sulfate consumed in: p5 A: r& o4 @$ N+ ?3 Q. [
the second titration,
( [, U3 O$ ]1 y3 a- K; t( }8 S! wT is the titre of the zinc sulfate solution,/ l k5 o; M6 z. M
S is the mass (g) of the sample taken, and# s3 G; u" P* a% W+ [/ ]
0.005 = 500 ml / (1000mg/g × 100 ml)., k) f& M" S* i' E
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
- _* l) |- c+ w, z; f+ Dglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).1 U' t8 T- V8 `4 {/ Z
Heat gently over a Meeker burner, while swirling the flask, until. x; m9 M% L3 o `9 }7 E5 O8 [
decomposition and fusion are complete and the melt is clear, except
2 _0 L7 I- }4 k9 B0 E" kfor the silica content, and then cool. (Caution: Do not overheat the
( I! C' S" g2 L, z0 I Gcontents of the flask at the beginning, and heat cautiously during0 H% a( w8 p& J* \/ K% j2 h
fusion to avoid spattering.)3 u4 D% K: `' R- U) m; P r
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
% O6 K1 |8 S2 |$ d/ D5 Vcarefully and slowly until the melt is dissolved. Cool, and carefully add
2 x4 r2 n7 I- i) d2 o150 ml of water by pouring very small portions down the sides of the m2 j: B# a' P* B* l3 B4 F
flask, with frequent swirling to avoid over-heating and spattering. Allow# b* Q+ O4 q1 J. o& j
the contents of the flask to cool, and filter through fine ashless filter
4 a: @5 B4 ?5 x9 W* F3 ppaper, using a 60 degree gravity funnel. Rinse out all the silica from2 P' M: t0 {* C( Q# i# K7 f
the flask onto the filter paper with sulfuric acid solution (1 in 10).9 u+ e5 O. m2 ?
Transfer the filter paper and its contents into a platinum crucible, dry in/ D; L9 R3 ~3 Z c
an oven at 1200, and heat the partly covered crucible over a Bunsen
e- t! j! S! R; V7 e8 cburner. To prevent flaming of the filter paper, first heat the cover from
8 X8 j; P. j- [/ Z: V! p3 zabove, and then the crucible from below.9 R$ B) P; r/ \# W [. |
When the filter paper is consumed, transfer the crucible to a muffle
: I( T/ F8 Z, E- \8 ofurnace and ignite at 1000o for 30 min. Cool in a desiccator, and! s9 V/ [( j, f8 O6 P
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated
$ T% c% l% P) f3 W7 V/ Q( ehydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
! O2 q' W ^( u9 z/ L# m+ u' a4 g- b. T. yon a low-heat hot plate (to remove the HF) and then over a Bunsen+ P( o; Y1 s) B% t6 n X$ K& g$ g
burner (to remove the H2SO4). Take precautions to avoid spattering,
$ n) k: p5 B* C0 c" e7 T2 F3 c8 l5 Zespecially after removal of the HF. Ignite at 1000o for 10 min, cool in a5 ^3 _. a( d$ L* i8 l4 U
desiccator, and weigh again. Record the difference between the two
7 W: T3 C' A1 g) @, P& ^, \weights as the content of SiO2 in the sample.
, r$ R4 C8 h. z! QMETHOD OF ASSAY2 _ h7 }( r" k' r! |1 i9 b
Accurately weigh about 150 mg of the sample, previously dried at 105o% M( w; Z4 Y3 w
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water* D, Y5 j9 y- e5 A* G
and shake until a homogeneous, milky suspension is obtained. Add 30
2 a/ v: U6 D: Rml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
`* h8 T# v3 O# i5 I5 bheat gently, then heat strongly until a clear solution is obtained. Cool,
8 n/ }% P" ^3 z7 p' Nthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric- v( s, c* A2 U! f/ w% b
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
! u! M1 {! @# s, Xrubber stopper fitted with a U-shaped glass tube while immersing the' F& v' L- U* X# S
other end of the U-tube into a saturated solution of sodium y. }8 R8 O, z) M, ^7 ?
bicarbonate contained in a 500-ml wide-mouth bottle, and generate+ i( H) O; R. b( q
hydrogen. Allow to stand for a few minutes after the aluminium metal
6 m# C2 S8 R7 ahas dissolved completely to produce a transparent purple solution.
$ T! q+ B2 l% |, ?Cool to below 50o in running water, and remove the rubber stopper0 r/ Z; H- P- p" G& _( n5 L% k
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate5 @5 s# I. M: c6 Q
solution as an indicator, and immediately titrate with 0.2 N ferric( \, r: [( H3 V4 C) d( b6 x" k
ammonium sulfate until a faint brown colour that persists for 300 O5 C* q% A6 M, T) H# ?( j
seconds is obtained. Perform a blank determination and make any
5 j/ w6 K! X% A: w5 k" Dnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is% {* w0 N2 e$ e* S: B
equivalent to 7.990 mg of TiO2.; u+ d0 _# Z6 n5 Y# Y0 @
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