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二氧化钛(钛白粉)
二氧化钛(钛白粉)
3 f7 `2 D: t* f& T& R
( C# x+ l% N" B. o5 FJECFA关于二氧化钛(钛白粉)的结论4 i$ N: t+ ~2 y7 U- @9 d* p3 ~+ l
# x# ?: T" L" A T摘要: 2006年JECFA关于二氧化钛的结论, U" X q2 C! q# t( A
ADI值:不作限制。
" w, C- I5 C/ E3 f" p功能:着色剂
. ? s0 }1 z1 z# A! D x
! N9 G, g* Q5 Z; D+ z+ m# c, ITITANIUM DIOXIDE
9 o0 e O" l, B( bPrepared at the 67th JECFA (2006) and published in FAO JECFA+ ?! e, O! a" r6 S- \/ D v
Monographs 3 (2006), superseding specifications prepared at the 63rd9 E( Y6 h$ N* S. M
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
. B4 Q0 N+ Z3 E0 w' tCombined Compendium of Food Additive Specifications, FAO JECFA
+ v |: j2 R, l/ O* ^6 c0 rMonographs 1 (2005). An ADI “not limited” was established at the 13th
# w& Y- ^+ i8 x9 X6 D3 UJECFA (1969).- v9 r Q! ?" L: A- Q* M2 D a
SYNONYMS
! w" ~8 r" y5 a- v) XTitania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
n4 y" x1 a' n- @8 G" ODEFINITION# @6 C( t( L6 c8 F) p% h B+ I/ W
Titanium dioxide is produced by either the sulfate or the chloride! \. P3 c% ?/ T A$ {4 I1 u
process. Processing conditions determine the form (anatase or rutile/ O( o6 j; N2 {, i9 u- n. B
structure) of the final product.: q8 p* G6 S6 E
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)( j# c- R n6 w9 P" |
or ilmenite and titanium slag. After a series of purification steps, the$ t4 F# \$ p4 [1 T0 w
isolated titanium dioxide is finally washed with water, calcined, and! K$ |! c7 d/ K
micronized.
% t% @( }5 P9 B& p; g8 `: i- `In the chloride process, chlorine gas is reacted with a titaniumcontaining
4 |3 o+ n2 q6 N& u- jmineral under reducing conditions to form anhydrous/ p, I e1 q( u) v$ W$ N! r
titanium tetrachloride, which is subsequently purified and converted to, n3 y3 c, O% E9 k/ p
titanium dioxide either by direct thermal oxidation or by reaction with% M1 k! f9 h3 _; Y/ f$ y
steam in the vapour phase. Alternatively, concentrated hydrochloric
t& w# i9 O7 {) k& oacid can be reacted with the titanium-containing mineral to form a Y5 \" @: m' Y: D2 x, w
solution of titanium tetrachloride, which is then further purified and
) ~. m2 v: Z% w* sconverted to titanium dioxide by hydrolysis. The titanium dioxide is
8 `$ T9 a& W# X+ z- }; F2 [filtered, washed, and calcined.
' b: F r8 L/ v; c3 V' CCommercial titanium dioxide may be coated with small amounts of
0 K0 A$ e* L2 u! f( Halumina and/or silica to improve the technological properties of the
1 x. l0 j# o! A0 u, j0 |product. v0 R2 y- j! e3 ~
C.A.S. number 13463-67-7
0 J4 B, B/ O s! x" ^Chemical formula TiO2# ^5 ]' a: ^5 A0 L/ r% W6 S
Formula weight. {, I- @1 S P& p H
79.88
v7 c9 E1 V9 D' C' U q: e) S* ZAssay
P; j4 E2 K- mNot less than 99.0% on the dried basis (on an aluminium oxide and
' k: H6 f4 ?, o) }& K1 vsilicon dioxide-free basis)" H! \7 j2 Y) P# P1 j; A
DESCRIPTION2 }5 V' D T2 Z' [7 }
White to slightly coloured powder
& h" [ ` y; F2 d2 u9 q& [FUNCTIONAL USES
7 w+ h7 k4 c5 g$ E& N+ v5 J9 X+ C/ oColour7 ?5 t: A# f! [! c3 x
CHARACTERISTICS& G: [# \3 u6 `& F
IDENTIFICATION
8 k; I9 ]% I1 i0 C% L6 a' iSolubility (Vol. 4)% E9 q* g! |- f/ Q; Z1 R
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic7 y5 O l- B3 x- {0 Y* C
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated0 Y b1 R4 ]9 @& r5 A& g7 T: |
sulfuric acid.
1 B/ e. z3 P1 T: v' a% x" Q' aColour reaction: g5 g7 ~# @+ I) I8 p
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of* p, Q( R* m! s+ u9 r* l2 p1 ]
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
|: X8 M$ g: \7 ^( Zwater and filter. To 5 ml of this clear filtrate, add a few drops of* ^7 f4 w+ [# }+ E$ M4 Z/ W7 G
hydrogen peroxide; an orange-red colour appears immediately.6 L) F5 S7 s4 B: d
PURITY) }$ f& `% z O' W% v# l
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h); d k: R z. T7 }$ K$ y4 C0 V
Loss on ignition (Vol. 4)8 U( @' u {) a! O. O$ B
Not more than 1.0% (800o) on the dried basis
$ F7 T! `; h& I, @# H4 B5 h. F( i7 ^Aluminium oxide and/or& Y3 {$ d/ u/ }/ }0 m& M0 U
silicon dioxide. c3 f$ m* o; a0 i1 ?; g+ V
Not more than 2%, either singly or combined
6 X `3 x- i$ O2 o! kSee descriptions under TESTS+ ~2 J6 J3 |: s1 v: `) s. _
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing) Y/ r9 i, K% H4 p: W0 l
alumina or silica.
# a0 ]" v: {( l4 h7 R2 U! b0 PSuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
( z7 N5 L- H6 r+ M! ~1 a( l/ X) Rplace on a steam bath for 30 min with occasional stirring. Filter1 ^! \5 j7 s9 g+ P" F5 _
through a Gooch crucible fitted with a glass fibre filter paper. Wash* Z! q9 u, ?9 f6 |6 i, B7 D% G
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
* E* d& |& q% f; _3 y5 \, Y! q# w, H/ ]combined filtrate and washings to dryness, and ignite at a dull red3 y- C# v9 Q5 E4 h
heat to constant weight.' C' z3 C! A/ b8 Y+ V
Water-soluble matter, m* `+ @$ @5 a: j4 w
(Vol. 4)! _- d3 v: Y7 b! ~2 m- q
Not more than 0.5%; W$ p( b$ L0 E, v7 E {
Proceed as directed under acid-soluble substances (above), using
* K2 e3 e1 Z# a2 e& awater in place of 0.5 N hydrochloric acid.* \! e0 t& K; d
Impurities soluble in 0.5 N' W% N9 b& K- J' m
hydrochloric acid
8 l- \( \, o" U1 _5 v3 zAntimony Not more than 2 mg/kg8 X6 t# M; s4 s9 {' P4 b* Z
See description under TESTS: u9 ~$ g7 ]) V T
Arsenic Not more than 1 mg/kg5 w+ ^! o4 ^2 G" F( u
See description under TESTS; G6 ?0 j2 I5 b
Cadmium Not more than 1 mg/kg7 a4 y" G! }2 C; v m' h$ P! c
See description under TESTS
1 T5 g% a V6 }% o+ e* O( l: PLead9 |- [0 N' b( v1 g2 f/ Y& c, M
Not more than 10 mg/kg9 Y5 u7 w8 J& J- i) s8 d& q7 E
See description under TESTS
" w" b4 F; \- `0 x- ~" WMercury (Vol. 4) Not more than 1 mg/kg9 z+ C4 k5 k& X- u$ p: X
Determine using the cold vapour atomic absorption technique. Select a. t/ k( M3 |1 J- U7 L4 l4 R
sample size appropriate to the specified level; t% ^$ [7 @0 j
TESTS5 |7 G3 W A3 \: v q
PURITY TESTS- B6 V" G3 j, l- _ \, ~7 w
Impurities soluble in 0.5 N( p- J4 X0 H8 _7 D& n. S+ C
hydrochloric acid
! X5 l( ^' a! n- o( L" QAntimony, arsenic,* }2 x3 Y& c' ?2 R
cadmium and lead
( i, a T/ o, E ^" b: n- D3 m' [(Vol.4)0 N' v# f/ }- P$ z9 M( `) n
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
& B& G" }% a6 _7 M; Q- `) G- W& l0 nhydrochloric acid, cover with a watch glass, and heat to boiling on a
' F0 m& K0 }& V/ [hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml7 m$ [# |* \1 b' l; w, u
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
/ L: P& f% a6 Y0 C- F7 }0 lmaterial settles. Decant the supernatant extract through a Whatman
5 m: x) Q( U1 ONo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml
1 q" V$ n7 z# e( C+ x) Bvolumetric flask and retaining as much as possible of the undissolved
' w& h! s6 v! m- [) {material in the centrifuge bottle. Add 10 ml of hot water to the original& H- `. u# C. x# Y8 Z1 M1 \
beaker, washing off the watch glass with the water, and pour the% O& K; h p, S! H: K
contents into the centrifuge bottle. Form a slurry, using a glass stirring% C. V0 a0 J# s
rod, and centrifuge. Decant through the same filter paper, and collect
+ [9 ^, D+ Q' V8 L' sthe washings in the volumetric flask containing the initial extract.% p' A5 E0 d' y; w& P6 v" h
Repeat the entire washing process two more times. Finally, wash the
$ k' n" K: B- i# F$ `! }" f) @5 mfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask: \0 @+ ~" H7 |( E4 U
to room temperature, dilute to volume with water, and mix.2 I7 O- ]3 D- U3 T; p
Determine antimony, cadmium, and lead using an AAS/ICP-AES
$ P0 n; v% V9 s5 F1 ]technique appropriate to the specified level. Determine arsenic using the
" h$ Q$ L; X( R. tICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
6 I; C. H9 E- E9 F; jMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
' u6 E+ X/ d6 |. G& Q" b; Z6 J1 g. The selection of sample size and method of sample preparation6 e4 G: y0 n7 Z% ?% V+ r1 m O
may be based on the principles of the methods described in Volume 4.2 C% ^- M7 @$ ~' ]! p
Aluminium oxide Reagents and sample solutions; c4 B, E7 ~# `8 D2 f- f
0.01 N Zinc Sulfate
$ m" Z* d$ q: o" GDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to0 J7 r/ u* v L! g6 ?8 [" ]
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
$ M2 V4 g* q0 a% W y! Nof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of3 D% g1 i" M+ A9 R6 v7 K
concentrated hydrochloric acid, heating gently to effect solution, then3 S7 E8 j% B* w5 [! x- g
transfer the solution into a 1000-ml volumetric flask, dilute to volume9 G5 F7 t$ ?$ N) Y+ N, Z$ @
with water, and mix. Transfer a 10 ml aliquot of this solution into a 500+ Y7 Q% X: d9 L' g; j3 E9 Y% n) Q
ml Erlenmeyer flask containing 90 ml of water and 3 ml of/ I* _, c5 H4 m% B. |% N y! h5 G! ]
concentrated hydrochloric acid, add 1 drop of methyl orange TS and
& h7 O5 e7 ^$ X# e- m/ k25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. u( P: ?) v* {( l- p. G3 Xdropwise, ammonia solution (1 in 5) until the colour is just completely
2 [! N3 e4 _4 q* Jchanged from red to orange-yellow. Then, add:
% M5 C! R j9 o* ]3 q(a): 10 ml of ammonium acetate buffer solution (77 g of
0 l* r4 t9 O9 A0 @8 [8 Fammonium acetate plus 10 ml of glacial acetic acid, dilute to
6 R$ D q. I7 I% }9 Q1000 ml with water) and, B Z H; ]& `; [7 k
(b): 10 ml of diammonium hydrogen phosphate solution (150 g6 i; Q6 {4 k4 A3 }
of diammonium hydrogen phosphate in 700 ml of water," d1 f* R0 l3 _# W3 x- h! f$ z
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
% b0 u% Z' @0 |: Bthen dilute to 1000 ml with water).
- `2 ?: F" d8 V$ v4 o o8 o/ rBoil the solution for 5 min, cool it quickly to room temperature in a/ q' f/ m8 U6 ?2 I O
stream of running water, add 3 drops of xylenol orange TS, and mix." P9 H7 q5 q& U- y* j. K
Using the zinc sulfate solution as titrant, titrate the solution to the first4 c3 c2 ~& ~4 N5 Y
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:
% }7 _4 N& m8 ]9 HThis titration should be performed quickly near the end-point by
* m' Y( @$ r* C3 x" Vadding rapidly 0.2 ml increments of the titrant until the first colour; t& |- w. ~4 e* o' G T! \; E
change occurs; although the colour will fade in 5-10 sec, it is the true/ n, U( P; ?5 q5 g) Z4 K
end-point. Failure to observe the first colour change will result in an
1 [) G# H1 e3 _ r1 Lincorrect titration. The fading end-point does not occur at the second
2 g% t1 y+ P+ K- b; @end-point.)4 s+ q: E, h: r
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a* m2 F% c' u% s! c) x9 r- v
stream of running water. Titrate this solution, using the zinc sulfate# Z9 ^+ O& N7 Z3 T1 L3 x( N! q
solution as titrant, to the same fugitive yellow-brown or pink end-point
7 e: }; D" j4 Z3 \* k# Vas described above.
9 w# d6 s/ B3 I% C* zCalculate the titre T of zinc sulfate solution by the formula:/ ?5 o: {4 Q5 Q: V; K0 k
T = 18.896 W / V4 ` \+ [$ }% Y+ S, G1 L
where- W/ {8 n% F% A- `# A5 b6 }0 f! B
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
5 N# h& F4 O" D C% D9 N3 c6 DW is the mass (g) of aluminium wire
6 s% c! ?6 w2 U6 W$ \; gV is the ml of the zinc sulfate solution consumed in the
. D7 T% @7 [, D. W8 U' asecond titration
! H# n" o0 K( J! i18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and- p1 E4 T" B0 ~+ j
R is the ratio of the formula weight of aluminium oxide to3 K1 L/ D/ B. \% R) G
that of elemental aluminium., W2 M+ }* J2 i! ~* |4 D; Q
Sample Solution A
0 |2 W6 F/ p, ^9 n# Q4 h7 DAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
% c5 I, ~' F' N+ J! {' Kglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O)., n) i& D4 I3 k0 s0 n% R
(Note: Do not use more sodium bisulfate than specified, as an excess( a( h6 Y8 l; t W* @3 F
concentration of salt will interfere with the EDTA titration later on in the$ m1 \/ G+ S' ?5 ~
procedure.) Begin heating the flask at low heat on a hot plate, and% U" G3 e+ @: E. g( f
then gradually raise the temperature until full heat is reached.
" S' y% o" ~: c: z* u8 V(Caution: perform this procedure in a well ventilated area. ) When8 p! m5 k$ t; K- Y! d. ~3 x" `
spattering has stopped and light fumes of SO3 appear, heat in the full
$ T* c+ _4 h! i2 Z0 W1 _3 D( Mflame of a Meeker burner, with the flask tilted so that the fusion of the ~9 i( c0 u$ a# R) k
sample and sodium bisulfate is concentrated at one end of the flask.
9 X* F/ {4 i2 c" {5 C0 x# e& XSwirl constantly until the melt is clear (except for silica content), but
! x9 p" N& ?/ |% h3 hguard against prolonged heating to avoid precipitation of titanium2 R& O% [8 C' ]! P
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until$ q- g2 y# ?/ A( a/ o0 F$ Z
the mass has dissolved and a clear solution results. Cool, and dilute to
; X1 Y& s/ D5 ~6 G a120 ml with water. Introduce a magnetic stir bar into the flask.
/ h- A |6 G( ZSample Solution B
( I+ N: n! ]' e) {7 z7 hPrepare 200 ml of an approximately 6.25 M solution of sodium
$ N! u' k: G8 C0 a" o1 _hydroxide. Add 65 ml of this solution to Sample Solution A, while! L) x9 b3 O0 f. J% z6 y! r2 e$ x
stirring with the magnetic stirrer; pour the remaining 135 ml of the/ c4 Q! ~ ?. n7 O6 q5 H& q5 G
alkali solution into a 500-ml volumetric flask.
6 P u( K; h5 N! c( sSlowly, with constant stirring, add the sample mixture to the alkali
& |2 y, F4 o& `: r( u/ msolution in the 500-ml volumetric flask; dilute to volume with water,! `/ |8 ~" @; @6 e) K5 T
and mix. (Note: If the procedure is delayed at this point for more than
3 r v3 X+ ^! U* o' R+ T7 e `' |8 S2 hours, store the contents of the volumetric flask in a polyethylene
) M( e5 g+ @; R4 |0 E9 ebottle.) Allow most of the precipitate to settle (or centrifuge for 5 min), I; s. A. b& D9 S3 z
then filter the supernatant liquid through a very fine filter paper. Label" Y$ ]4 U, O9 Y
the filtrate Sample Solution B.0 x9 e: p4 U0 n- s( o: q
Sample Solution C" e- K* t7 B/ ]: K3 W
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
" u$ |2 w' z$ E+ }. a% Lflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
7 {, `% G$ |/ U- ~solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.028 |% x2 y& J$ Y8 v. h" b
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
+ E: F$ @' a$ |# e- z! Lknown, calculate the optimum volume of EDTA solution to be added
1 E' l5 m D- ` k9 Z/ A& Vby the formula: (4 x % Al2O3) + 5.]
) x- J5 [7 `$ T# w. pAdd, dropwise, ammonia solution (1 in 5) until the colour is just& ^! w+ ` r7 k5 b! x; _
completely changed from red to orange-yellow. Then add10 ml each0 @. g. W# s" M' `' b( H
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to- X0 j3 A4 A+ M3 O0 X) F
room temperature in a stream of running water, add 3 drops of xylenol" g0 `: S: H# P! j3 j8 k
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
9 X7 Z* F/ q; y* ^bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired3 n. Z v7 G/ g& S* n' I
pH, a pink colour indicates that not enough of the EDTA solution has/ b8 M0 J" n& @* {& |" B
been added, in which case, discard the solution and repeat this6 O3 g! F* P j1 b# }4 d0 h" W
procedure with another 100 ml of Sample Solution B, using 50 ml,
: M. J B; A3 m8 C3 m5 Mrather than 25 ml, of 0.02 M disodium EDTA.
3 N% T' g n+ K7 U+ gProcedure }5 w% a8 w# n \ ~: B
Using the standardized zinc sulfate solution as titrant, titrate Sample) V4 o2 ^" e2 J2 h* }+ r% C3 T
Solution C to the first yellow-brown or pink end-point that persists for
; b7 J" X" h+ a8 X7 t1 Y% E- q5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
& t8 b2 p. B3 b/ P: ?. K. ^/ mtitration should require more than 8 ml of titrant, but for more accurate
. o1 U! i& E4 |0 bwork a titration of 10-15 ml is desirable.+ v |) A0 _3 R% c4 W
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-51 b- c$ E! q$ r5 S0 J5 z
min, and cool in a stream of running water. Titrate this solution, using
" u- n1 _0 t& u9 y5 jthe standardized zinc sulfate solution as titrant, to the same fugitive
, T& A0 R* a/ z. ?) dyellow-brown or pink end-point as described above.
; q1 u$ o* P7 N+ `6 pCalculation:
5 G" E, z; G+ R9 ]Calculate the percentage of aluminium oxide (Al2O3) in the sample) v; f$ g6 \: ^5 G
taken by the formula:" E4 H) Y' C3 X/ N7 P- Z+ z7 z/ ]
% Al2O3 = 100 × (0.005VT)/S j) b2 C: g+ z2 g& Q5 L# ~
where
. f4 \0 h [; N# `1 F4 ]: E& dV is the number of ml of 0.01 N zinc sulfate consumed in
, d3 Q6 v1 e4 X* s" L# U# W+ z) Sthe second titration,
* D2 w) J7 x; ~; I3 N E, MT is the titre of the zinc sulfate solution,: b, |( ]$ ?; N' |! r% e
S is the mass (g) of the sample taken, and
2 G6 [+ C% k2 j5 c2 w% e8 w0.005 = 500 ml / (1000mg/g × 100 ml).& |8 M3 ^% o. D" A1 s7 T4 }( S
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
; @, ^) P% V7 Lglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
. w6 o* _) R, O. P4 y$ u7 DHeat gently over a Meeker burner, while swirling the flask, until* J2 d+ X B, M7 c
decomposition and fusion are complete and the melt is clear, except! d+ j# I: P2 C7 g
for the silica content, and then cool. (Caution: Do not overheat the. y) C. G4 ]8 I. v; K3 M
contents of the flask at the beginning, and heat cautiously during9 \) T2 q6 L# W) ^, m
fusion to avoid spattering.)
+ Q* m2 q$ m: {8 U" [9 B( t& BTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
. \! \/ `7 n- j* N; rcarefully and slowly until the melt is dissolved. Cool, and carefully add! M, y& e4 s' P" e5 H
150 ml of water by pouring very small portions down the sides of the
% v1 L. @2 O) Kflask, with frequent swirling to avoid over-heating and spattering. Allow
% A1 J6 \7 d' }/ \! l/ \the contents of the flask to cool, and filter through fine ashless filter
V1 ^3 _0 a4 M; t; ~/ N, |0 Upaper, using a 60 degree gravity funnel. Rinse out all the silica from+ i2 Y0 C ]( h, B! [$ e0 B
the flask onto the filter paper with sulfuric acid solution (1 in 10).
' T9 W; M B# K6 N, ~/ W4 c2 `3 xTransfer the filter paper and its contents into a platinum crucible, dry in
+ ~, q' c" ^2 I3 ]- U' r) Ran oven at 1200, and heat the partly covered crucible over a Bunsen, x" X# C; O$ J
burner. To prevent flaming of the filter paper, first heat the cover from
0 v! V3 x1 O, `' d I/ jabove, and then the crucible from below.- ?$ j/ T9 i7 O1 t
When the filter paper is consumed, transfer the crucible to a muffle
. `5 b# f1 z Q" T/ A7 `7 Vfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and9 f- h# ?7 }: N, e4 m
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated. W' |! u4 C8 P
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first7 z4 ?; f% w: W% ]2 }7 ]
on a low-heat hot plate (to remove the HF) and then over a Bunsen
0 D+ g4 U [3 P& d$ h8 dburner (to remove the H2SO4). Take precautions to avoid spattering,2 S' _% q# `* L- C. T3 \- s
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
?) R+ F2 Q5 E, S6 D( C; X2 Cdesiccator, and weigh again. Record the difference between the two% \& }9 V& }- O
weights as the content of SiO2 in the sample.
5 M6 p N0 I; e) e+ @METHOD OF ASSAY+ P/ s5 p2 o* k2 X) e
Accurately weigh about 150 mg of the sample, previously dried at 105o
( m" k1 O3 t4 S1 tfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water; L4 t$ o; V8 ]) l0 I' } s, ~
and shake until a homogeneous, milky suspension is obtained. Add 307 r) b- c3 i* c: O) @3 Q9 s' W
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
' p4 _* {4 }1 v( oheat gently, then heat strongly until a clear solution is obtained. Cool,! V, ^8 V( @# n. A, S8 E- v
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
% K- n8 L, N. z/ Racid, and stir. Add 3 g of aluminium metal, and immediately insert a1 r" P9 V9 x7 }
rubber stopper fitted with a U-shaped glass tube while immersing the
8 S: |5 ^/ L8 G6 K! X6 pother end of the U-tube into a saturated solution of sodium. E, S j+ F v' T$ `. k
bicarbonate contained in a 500-ml wide-mouth bottle, and generate! s3 o3 I; w' F
hydrogen. Allow to stand for a few minutes after the aluminium metal
( V5 S8 D: G4 ~6 g" v& ]- Ahas dissolved completely to produce a transparent purple solution.
% L2 y2 _# }7 r; DCool to below 50o in running water, and remove the rubber stopper) \" ^( g4 [ l5 B" C+ ]7 T
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
0 |; @) n( D' K9 \% Wsolution as an indicator, and immediately titrate with 0.2 N ferric; `" Z+ x1 o' b
ammonium sulfate until a faint brown colour that persists for 30; X5 y: I% \; D( ~. V4 n
seconds is obtained. Perform a blank determination and make any, _5 Q* m: ?- s, S8 N
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is5 i; n9 F6 n* [) L7 g$ k: c- E: E% h
equivalent to 7.990 mg of TiO2.3 j* G j/ F& R* i8 t
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