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二氧化钛(钛白粉)
二氧化钛(钛白粉)
6 X% P8 K7 d J3 ~8 a
( M$ r2 }2 P/ i9 |JECFA关于二氧化钛(钛白粉)的结论4 N! Z3 j9 U7 }' c6 j. I
% ~- v' J" A5 h8 r+ z) z
摘要: 2006年JECFA关于二氧化钛的结论
1 p( _, W9 U& b' {ADI值:不作限制。
5 E; { L- O- ~功能:着色剂
6 Q! n2 p0 \0 V" X @
: `: k6 n% q. I+ Q0 Q/ s m. h7 lTITANIUM DIOXIDE' `3 x: a- J* o7 M2 {
Prepared at the 67th JECFA (2006) and published in FAO JECFA( g0 @4 H$ `% s% w+ f* x
Monographs 3 (2006), superseding specifications prepared at the 63rd# _ ?- ]9 n& C
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
5 G( E1 l7 d- ]' a6 W7 P4 Q/ q4 ICombined Compendium of Food Additive Specifications, FAO JECFA
/ L% D: V& z( }! j" S9 S4 rMonographs 1 (2005). An ADI “not limited” was established at the 13th+ t. t2 w& }) f$ r2 Q7 i T
JECFA (1969).
) U2 K, O7 a. mSYNONYMS
/ x) v( \& f/ B6 fTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
' n3 j, d1 g* CDEFINITION
# h1 o0 E; n% R2 q! \Titanium dioxide is produced by either the sulfate or the chloride+ {! {7 O7 U1 P6 S, Y: P. L7 r
process. Processing conditions determine the form (anatase or rutile
# e' K2 e% @! [, d4 a. dstructure) of the final product.
% u8 ? ^) x% Z# t( FIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
0 I0 v3 `6 G/ G, v4 z' eor ilmenite and titanium slag. After a series of purification steps, the0 ^6 M3 ?0 d* m1 i3 \3 H# I
isolated titanium dioxide is finally washed with water, calcined, and
" u# j0 ]5 h2 X4 ~) ~micronized.
. g% W6 N: J/ |$ Z# N! U+ m$ FIn the chloride process, chlorine gas is reacted with a titaniumcontaining$ N+ w8 l7 T1 e! ]8 Q
mineral under reducing conditions to form anhydrous
" |% _7 C: G% m2 ]% x( e" Ptitanium tetrachloride, which is subsequently purified and converted to' w6 w. O$ n ]. ]* L
titanium dioxide either by direct thermal oxidation or by reaction with
7 b2 L$ R0 h [" b) Csteam in the vapour phase. Alternatively, concentrated hydrochloric
2 ?* v# Z6 c7 u. hacid can be reacted with the titanium-containing mineral to form a# {4 j4 k! L! A1 B! `! o% y6 }, q, t
solution of titanium tetrachloride, which is then further purified and
& N3 \% h; R/ \converted to titanium dioxide by hydrolysis. The titanium dioxide is5 F+ I) f: g/ b( E" d9 W- e& v
filtered, washed, and calcined.# `5 ]6 o v) Z+ v& p+ z
Commercial titanium dioxide may be coated with small amounts of
# A7 u0 }1 u9 z: [; _1 Yalumina and/or silica to improve the technological properties of the
H9 x" X- f# A" p4 z8 Lproduct.
' J, C [& J( f+ ?( S/ N: mC.A.S. number 13463-67-7
+ C6 c" f Y w. Q, F7 E8 D: sChemical formula TiO2
/ w: ]. Q& }* c! {( yFormula weight) O8 S" t( V# H( l, P
79.88& Z$ ?& l* s$ }; K6 X- x) y j
Assay5 p7 D3 {9 k2 r# H6 W, C) P% o
Not less than 99.0% on the dried basis (on an aluminium oxide and
5 R, d" S8 ^ V. `silicon dioxide-free basis)
' H- n% R& b+ n) ?DESCRIPTION3 K" i# _# B- A r$ y9 r" w& p5 w
White to slightly coloured powder
& f1 x' z0 B8 K5 m7 `3 s6 t2 uFUNCTIONAL USES' ^" H9 n3 r8 M
Colour1 C0 }. X5 z" C
CHARACTERISTICS
3 I4 p. H A# m% {# e5 `6 F- a& RIDENTIFICATION
3 j( v0 u1 Z, w5 D& o! pSolubility (Vol. 4)! J. P C' n7 U9 @: z, x
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic) F! c3 T& W: d+ g! v- F
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated
" f& X* O+ u; A7 P2 gsulfuric acid.! J7 Y3 T2 K2 @4 M) Q( l
Colour reaction
1 E7 O8 f( f/ l) s# H: B3 B5 OAdd 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
! c% L# |# F* w: \ d: L9 a( ~sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
. r& }/ i# o s& z Iwater and filter. To 5 ml of this clear filtrate, add a few drops of
" c2 W0 t0 }$ T. J4 }+ X! mhydrogen peroxide; an orange-red colour appears immediately.
9 x1 j& I) g! f) ~* ~ L. ]PURITY
6 w: X- S5 L2 uLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h), } U; j$ V2 a
Loss on ignition (Vol. 4)
# p* U( n% z1 x+ ]" w4 B6 K' u2 JNot more than 1.0% (800o) on the dried basis
, G; Y% {2 D4 G8 U" }1 A9 y* C1 RAluminium oxide and/or
# i, a+ g# d, A/ \$ Asilicon dioxide
8 L7 x: v+ ~$ v" U1 i$ V# G; MNot more than 2%, either singly or combined3 F' c; x% `9 p+ U9 ]! E, [
See descriptions under TESTS) L, v3 \ {% `/ d3 X) d( m O* b
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing' T5 T6 C; y+ ?5 J1 Y# I
alumina or silica.( U [2 L0 j" Z; g7 d+ ?' L/ n
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
% m3 K& E0 T ?$ [4 [place on a steam bath for 30 min with occasional stirring. Filter
! I9 |/ h" o+ g4 [7 _7 Bthrough a Gooch crucible fitted with a glass fibre filter paper. Wash- e% N) p9 Q" `- Q: K. \& U y3 R
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
! |( b/ H" [6 A/ n6 Q( @combined filtrate and washings to dryness, and ignite at a dull red
* m% i$ h. p' K- B( N& Uheat to constant weight.3 J" a9 j( M2 e0 {/ Z5 B6 Q+ i
Water-soluble matter, X+ H& {$ ]9 Y9 R( b! o
(Vol. 4)5 m. D9 X) x/ `6 ?6 f, m- Z
Not more than 0.5%
, A# G5 d+ p4 i( Z/ IProceed as directed under acid-soluble substances (above), using- Y+ J, L% k6 n/ U/ W
water in place of 0.5 N hydrochloric acid.: l5 G7 p# i. g: x' {& p
Impurities soluble in 0.5 N" p2 E/ I. L( R. f% u
hydrochloric acid/ V. F" R+ l, O
Antimony Not more than 2 mg/kg
. q. w: o" ^* m4 N+ N" VSee description under TESTS
, z5 N4 |# u% r) HArsenic Not more than 1 mg/kg
$ ?1 {: `# k; T2 A2 i; d* xSee description under TESTS
1 X3 D1 R) [5 c$ sCadmium Not more than 1 mg/kg
5 L e% [6 F( R4 ` NSee description under TESTS. A4 v% A+ b, s* j
Lead
% ~" i3 i( _* I; LNot more than 10 mg/kg
; j: {' u( @2 D5 G! J/ a" v2 gSee description under TESTS; {. N1 G' b& M% D& M8 y" ?* }( G
Mercury (Vol. 4) Not more than 1 mg/kg! i3 [5 J6 k) `% V
Determine using the cold vapour atomic absorption technique. Select a
% N/ V# `" ^/ l" O* {sample size appropriate to the specified level
* w# I* S3 g' S) x. BTESTS
, B( l0 C/ ~% b3 bPURITY TESTS9 l4 B, {, g9 f7 y
Impurities soluble in 0.5 N
$ s, d5 {# ^+ y$ Y8 e: H/ W+ Zhydrochloric acid! Z2 C, Y9 x, W& g. @6 y; E
Antimony, arsenic,, R, p( v% \6 |$ ~9 K8 d5 X& X
cadmium and lead. C% o/ F& w# H1 ^( I& N2 V' V
(Vol.4)9 {: ^$ Y2 i6 N3 g$ h; F/ l5 Z
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
1 X' r# h; N. x7 ihydrochloric acid, cover with a watch glass, and heat to boiling on a% e2 b' u9 o" y% `
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
; X% C6 {: {! O' @ }centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
3 o" x* F8 |* I: A. B( hmaterial settles. Decant the supernatant extract through a Whatman2 Z1 g( l! Y" o! Z4 o R7 G4 F
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
' L" W& x7 d" {! F7 [ k; Tvolumetric flask and retaining as much as possible of the undissolved
8 w7 E' q! f" c+ Z) nmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
/ S+ ^+ d9 Q" H& D8 ebeaker, washing off the watch glass with the water, and pour the
. ?) ?; {7 M+ H0 y7 Ncontents into the centrifuge bottle. Form a slurry, using a glass stirring
' G3 c9 Q n2 s( ]5 S. m, Jrod, and centrifuge. Decant through the same filter paper, and collect$ |* D% ~) S, O- D& b
the washings in the volumetric flask containing the initial extract.
, E' h" P+ T7 cRepeat the entire washing process two more times. Finally, wash the& @9 f4 {' q3 U8 @
filter paper with 10 to 15 ml of hot water. Cool the contents of the flask
1 }9 V! Q |; g5 i Yto room temperature, dilute to volume with water, and mix.
6 G/ D) k& k* W- g/ Q7 A3 h1 R! cDetermine antimony, cadmium, and lead using an AAS/ICP-AES
! S3 M" ?/ U2 P9 ?/ u4 G9 U( t# Wtechnique appropriate to the specified level. Determine arsenic using the
: X+ _" z, V5 D# I; N0 T, YICP-AES/AAS-hydride technique. Alternatively, determine arsenic using G1 H$ g- ]$ M% P$ L6 Q" h% o8 {
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
. g' U C8 x6 m2 m, ^) Z1 g. The selection of sample size and method of sample preparation$ U9 n. f" b5 Z
may be based on the principles of the methods described in Volume 4. F$ J! Q. J& R9 ?$ A( @
Aluminium oxide Reagents and sample solutions
& ~4 u- E1 I" @' y3 h$ I; F& u0.01 N Zinc Sulfate
( g6 C, f+ P( F: K. aDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
0 T0 R* s$ w O# n6 L2 r6 Ymake 1000 ml. Standardize the solution as follows: Dissolve 500 mg; J4 X; O0 `8 |* K" n
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of% _! j, @" Z1 H. M6 S
concentrated hydrochloric acid, heating gently to effect solution, then8 X9 Y2 }! ?) Z! g6 e
transfer the solution into a 1000-ml volumetric flask, dilute to volume
. _! Z" C9 F( M* O- E9 ~: awith water, and mix. Transfer a 10 ml aliquot of this solution into a 5009 R C* W( r- h4 U
ml Erlenmeyer flask containing 90 ml of water and 3 ml of( \+ s1 n8 t' O
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
, k4 b# D: b* S5 f) d25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,+ H, \$ C% Z9 S% |/ _- G4 @, o" x
dropwise, ammonia solution (1 in 5) until the colour is just completely) K* y" k! Z- Z; C* D
changed from red to orange-yellow. Then, add:
) g" i/ c( L. i9 f3 z! u(a): 10 ml of ammonium acetate buffer solution (77 g of! r$ z0 { |+ L* M! e( d
ammonium acetate plus 10 ml of glacial acetic acid, dilute to1 I+ ^0 H; R8 Y4 X
1000 ml with water) and
% n9 i a g6 L" \- U8 M! l, d(b): 10 ml of diammonium hydrogen phosphate solution (150 g/ g, o4 f- N) t/ ^
of diammonium hydrogen phosphate in 700 ml of water,
2 V8 |2 z9 U% m o' jadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid," K9 P7 {3 s$ Y, L
then dilute to 1000 ml with water).
0 o. Q+ C& r5 {7 uBoil the solution for 5 min, cool it quickly to room temperature in a
& N) Y5 Y3 T/ {" y5 n. qstream of running water, add 3 drops of xylenol orange TS, and mix.
0 T& @ y) t6 A1 i/ _- G: LUsing the zinc sulfate solution as titrant, titrate the solution to the first
+ i2 b: z. S2 n6 K* A$ k4 Jyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
9 I- O7 {4 ?/ W8 gThis titration should be performed quickly near the end-point by
- ]' h6 T, N3 ^! Sadding rapidly 0.2 ml increments of the titrant until the first colour
3 l/ ~! [% ]' M0 E1 Q5 i# }change occurs; although the colour will fade in 5-10 sec, it is the true8 z7 Z5 h) {+ w( X
end-point. Failure to observe the first colour change will result in an
2 D- O7 p# s5 O4 I4 _incorrect titration. The fading end-point does not occur at the second: \$ G0 d. D: W/ {
end-point.)8 i* B2 K& q; V/ L
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
0 W) O4 ^2 u2 O/ B% D8 E9 ystream of running water. Titrate this solution, using the zinc sulfate
3 P$ s2 N0 Q" f$ B7 hsolution as titrant, to the same fugitive yellow-brown or pink end-point7 y h3 D7 R7 @/ T s- ?5 B
as described above.3 w: m& H" H9 ~9 w
Calculate the titre T of zinc sulfate solution by the formula:5 W6 d* ?3 Q4 b- T
T = 18.896 W / V: E! o- R& W9 A6 c
where
0 q$ R/ n/ g |( t7 o/ K4 p+ K1 aT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
W t: x* A# L* F+ kW is the mass (g) of aluminium wire
' E( R7 |: Y4 eV is the ml of the zinc sulfate solution consumed in the& I8 _2 M! [; _
second titration
. D7 k& X, ]* | \7 O18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and8 E2 `( ]4 N8 R4 `* N# l
R is the ratio of the formula weight of aluminium oxide to
/ @4 b1 s/ P& Pthat of elemental aluminium.+ A, u) H& y" T. ~* n, K
Sample Solution A
7 z [8 D0 \3 W; [8 O) u1 X* M6 yAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica9 ~0 z) M! P1 u5 p- j" o% t
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
) G; N( p m0 P, l. M$ _# G(Note: Do not use more sodium bisulfate than specified, as an excess
/ j. w4 {8 l4 p+ \5 Q; Dconcentration of salt will interfere with the EDTA titration later on in the6 z E) i$ ~/ O& i/ T
procedure.) Begin heating the flask at low heat on a hot plate, and
( j) D3 f( U4 ythen gradually raise the temperature until full heat is reached., z+ F. x5 D4 f4 _* t* s! r# n, F" X
(Caution: perform this procedure in a well ventilated area. ) When
; e; E2 ?. e4 I& [4 G) U4 L( lspattering has stopped and light fumes of SO3 appear, heat in the full0 e) `" J" k" d" W* m
flame of a Meeker burner, with the flask tilted so that the fusion of the A3 S5 j5 a( K l- Q" i, S, ^
sample and sodium bisulfate is concentrated at one end of the flask.. Q/ S# P1 f5 k u2 A: b4 A
Swirl constantly until the melt is clear (except for silica content), but
' [% i9 N! _' d9 ~- N( y. Aguard against prolonged heating to avoid precipitation of titanium5 { C/ y! }7 @" ]) I3 p+ M0 B
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
: o- \" _$ H7 G0 u A, Gthe mass has dissolved and a clear solution results. Cool, and dilute to
Y7 W$ P3 g$ S% e' c# Y9 l1 G120 ml with water. Introduce a magnetic stir bar into the flask.' @" \& G8 ?" i" d
Sample Solution B
8 |1 s( u; i# r& c( RPrepare 200 ml of an approximately 6.25 M solution of sodium4 s% n& T6 \: x5 X" k
hydroxide. Add 65 ml of this solution to Sample Solution A, while
' T8 p+ X0 {% P& F& _stirring with the magnetic stirrer; pour the remaining 135 ml of the7 [$ w) V% H7 y# p; Z
alkali solution into a 500-ml volumetric flask.
% @9 Q( d5 K" Y+ [2 V8 x! M& F( l5 X; YSlowly, with constant stirring, add the sample mixture to the alkali
( n4 F @* p$ u, q) Ksolution in the 500-ml volumetric flask; dilute to volume with water,
9 W, K# a" u3 m& r" Vand mix. (Note: If the procedure is delayed at this point for more than# M2 i2 K* k# V! J3 t, u* F
2 hours, store the contents of the volumetric flask in a polyethylene. G/ I4 _ K% T! W3 o) _& s5 d
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),* ]; ?7 u/ G- ~1 p: B0 F5 [6 ^
then filter the supernatant liquid through a very fine filter paper. Label
) N9 x! T! l: G6 uthe filtrate Sample Solution B.$ N. z7 j7 Y. v5 Z, \) {) E
Sample Solution C
. |3 d* b. `! R. C, ATransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer9 v6 l/ B/ d1 f, w( B O# ?
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
; R% Q) N: {9 m: q1 {; H( Ssolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
& M3 x, X6 m7 i; m+ `3 M* R( |- nM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is+ D. Y6 W) r2 ~. L% E# O- Q6 p- o
known, calculate the optimum volume of EDTA solution to be added! l: E! m% r; l# l) [7 ?) |2 Q2 [- F
by the formula: (4 x % Al2O3) + 5.]
! [- H4 g( H# cAdd, dropwise, ammonia solution (1 in 5) until the colour is just9 F8 a9 ~+ Y- d$ x P1 t
completely changed from red to orange-yellow. Then add10 ml each. z& B3 `$ A$ \+ _4 w' D+ D
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
2 h" q: B8 C, S3 N0 _) f6 d) ]+ _/ Sroom temperature in a stream of running water, add 3 drops of xylenol2 p# I! N, b4 F; I( c- O0 k2 ?
orange TS, and mix. If the solution is purple, yellow-brown, or pink,( H. p" D! M2 e
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
j8 y4 _" Z r; {# ~pH, a pink colour indicates that not enough of the EDTA solution has" C; [, Y& { D" E$ k4 K
been added, in which case, discard the solution and repeat this
; J! }% d0 a# K4 z/ Wprocedure with another 100 ml of Sample Solution B, using 50 ml,
$ i3 I, i3 f# Z( J9 D+ z8 N2 @rather than 25 ml, of 0.02 M disodium EDTA.; {. J, X' ~; l- M0 C& N9 B9 H
Procedure. n n, j; A$ s5 N) o5 N
Using the standardized zinc sulfate solution as titrant, titrate Sample) G2 C! x& n6 ]5 e* z
Solution C to the first yellow-brown or pink end-point that persists for
; u/ \0 k6 V% P O: U+ h4 N/ A5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
: Q E2 u8 J0 a8 Atitration should require more than 8 ml of titrant, but for more accurate2 ?. ]; F" @' S9 |
work a titration of 10-15 ml is desirable.
& g; K. p) ^) C. l3 EAdd 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
, I" d. T$ Z, U; kmin, and cool in a stream of running water. Titrate this solution, using# q7 w) Q1 J* D/ t& y
the standardized zinc sulfate solution as titrant, to the same fugitive/ h1 a3 U2 b" J5 r9 I
yellow-brown or pink end-point as described above.0 {/ t7 f1 B# W+ w& b
Calculation:
1 [7 a, ]! f" J pCalculate the percentage of aluminium oxide (Al2O3) in the sample
4 k3 t* @4 J' ]) K; ` Xtaken by the formula:2 F( a% a7 I" j1 w2 v R7 G$ O
% Al2O3 = 100 × (0.005VT)/S# E) g$ _ x; z& m: L- c
where7 X, A/ C: m. b7 u; y! |
V is the number of ml of 0.01 N zinc sulfate consumed in
; D" r0 s9 V N7 f" r) E$ w6 g# s) Mthe second titration,$ s" p: c0 ^, e4 d0 x' M
T is the titre of the zinc sulfate solution,
0 X( e4 S- \0 b1 n5 r1 jS is the mass (g) of the sample taken, and
: c" x5 M. |9 H; L0.005 = 500 ml / (1000mg/g × 100 ml).
) ? h w, K- Q8 h" u! a" CSilicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
! ~+ }) r( u' w" bglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).7 p6 c+ ~' P* a9 i, E `9 o
Heat gently over a Meeker burner, while swirling the flask, until
; p2 R9 {2 F6 K% A0 }decomposition and fusion are complete and the melt is clear, except
1 K2 S: m& B, q3 R% F* Cfor the silica content, and then cool. (Caution: Do not overheat the
2 @! }9 Z7 O& b. f: R( D$ dcontents of the flask at the beginning, and heat cautiously during. \: t& Z1 O* B
fusion to avoid spattering.)) _! i" ~2 J; }' \/ S; \. G
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat0 ^4 k7 l9 C5 K
carefully and slowly until the melt is dissolved. Cool, and carefully add
J, n) a! a; w3 a150 ml of water by pouring very small portions down the sides of the) u( {8 { T+ Z3 p! _1 }
flask, with frequent swirling to avoid over-heating and spattering. Allow) |3 J9 x( g' b5 a3 t9 W$ V5 m1 I
the contents of the flask to cool, and filter through fine ashless filter
( X: z6 P, V- W5 O* opaper, using a 60 degree gravity funnel. Rinse out all the silica from
( w) U$ s$ @9 Q( Vthe flask onto the filter paper with sulfuric acid solution (1 in 10).
" {1 p! H. F/ d4 z7 h" dTransfer the filter paper and its contents into a platinum crucible, dry in2 ]* t4 @2 w7 S9 r* w% @8 p' `2 k$ U
an oven at 1200, and heat the partly covered crucible over a Bunsen
6 ^7 Y, y9 p5 I; @- iburner. To prevent flaming of the filter paper, first heat the cover from: h! I P6 B; M9 ~% {# h1 G9 ^
above, and then the crucible from below.
7 Z$ u: u. S, Z+ ]% L6 f4 tWhen the filter paper is consumed, transfer the crucible to a muffle
8 m5 h7 N0 V- y" J4 A2 bfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and7 K8 T% v! t; W4 |" O# }
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated0 ~7 g) L0 T$ O ?9 E d) b i
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first- m- g6 C9 F" k* [" e
on a low-heat hot plate (to remove the HF) and then over a Bunsen
6 D S& M: z, x" b) O; \burner (to remove the H2SO4). Take precautions to avoid spattering,0 W5 l% A/ `1 z0 C+ G
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
% l- E7 Y1 Y2 N. U3 y6 }* x) ^desiccator, and weigh again. Record the difference between the two. E/ N3 C p$ O% k4 `! U' P4 X
weights as the content of SiO2 in the sample.
( C& o# @" x) B& W% h2 }$ FMETHOD OF ASSAY" K2 s! p+ m) T
Accurately weigh about 150 mg of the sample, previously dried at 105o
: `& g/ O7 T9 I8 w _5 \for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water) H7 l& x. F6 Z* q; d2 {
and shake until a homogeneous, milky suspension is obtained. Add 30
. a e' @) T# A0 Uml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially, L l4 e3 \- i- T+ @7 v
heat gently, then heat strongly until a clear solution is obtained. Cool,
! j5 e& C% l2 f" Y# y5 n. A( E, bthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
( u8 h W, q: s% {9 ]; W7 uacid, and stir. Add 3 g of aluminium metal, and immediately insert a4 o( P3 w! W- V' Y" h1 F
rubber stopper fitted with a U-shaped glass tube while immersing the- r& x3 _ B% H, w
other end of the U-tube into a saturated solution of sodium
$ p m7 A$ R2 F# l1 _' Fbicarbonate contained in a 500-ml wide-mouth bottle, and generate
) u- ?7 J. E z6 Thydrogen. Allow to stand for a few minutes after the aluminium metal& O7 ]6 k" f3 W# @6 \
has dissolved completely to produce a transparent purple solution.
" Q/ }6 G+ } p, N# S2 F, K- TCool to below 50o in running water, and remove the rubber stopper
" x1 y V2 ?* m$ `" S0 U* `2 i/ gcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
e1 B3 t/ f6 esolution as an indicator, and immediately titrate with 0.2 N ferric1 X. |9 w- \' d
ammonium sulfate until a faint brown colour that persists for 30
" t6 @ q- H0 p. m0 Lseconds is obtained. Perform a blank determination and make any
& ]4 O g, f, Y, `) A0 t( m* g3 E3 Onecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
7 ~- E8 Y! ?- h) M: S. Z" Wequivalent to 7.990 mg of TiO2., e, z0 T& i8 X, F9 e3 {
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