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二氧化钛(钛白粉)
二氧化钛(钛白粉)+ j* b4 V0 s& }; X+ b4 {
7 ]& t/ F9 H" l* Y3 R0 Q
JECFA关于二氧化钛(钛白粉)的结论. P+ Y3 t' v+ i5 K
0 w" l3 R* U/ l+ D# S摘要: 2006年JECFA关于二氧化钛的结论 [1 s# P6 h; Q0 Y
ADI值:不作限制。! Z* q2 M) h, {: f
功能:着色剂
5 g8 Q: s' {0 ]9 v' y* r& L) ]& n& T2 g7 c8 g
TITANIUM DIOXIDE' l- y/ I( S9 T) k
Prepared at the 67th JECFA (2006) and published in FAO JECFA+ S" L( x/ I) H9 M8 C5 ^5 Z4 c0 z2 X
Monographs 3 (2006), superseding specifications prepared at the 63rd0 g ]- N0 C d. h- d
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the* I7 x+ M0 r1 M$ ?
Combined Compendium of Food Additive Specifications, FAO JECFA
- e. d, P6 O9 u2 c; r- AMonographs 1 (2005). An ADI “not limited” was established at the 13th
+ ^! q0 x/ k( mJECFA (1969).( l8 A" f( d0 L. j* ~ `
SYNONYMS
' t$ ~/ q# |2 s, @- |Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171& O' u& A- `5 n
DEFINITION% T3 E0 D% I; r% s& V
Titanium dioxide is produced by either the sulfate or the chloride
# q1 V E. ~2 d7 o) j% Pprocess. Processing conditions determine the form (anatase or rutile
9 p5 N5 l$ q; l, wstructure) of the final product.
0 o! ]! ^8 F3 _& C3 \In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
6 a0 v% K8 x0 H% S) ^or ilmenite and titanium slag. After a series of purification steps, the! u0 O+ l1 c% v# t
isolated titanium dioxide is finally washed with water, calcined, and0 o6 }- @) W, c. ]) U$ c9 r
micronized.
A* h: o7 D# q* R( v# R KIn the chloride process, chlorine gas is reacted with a titaniumcontaining( {( m/ U# B, H$ @! o! ?5 W
mineral under reducing conditions to form anhydrous
- T- H7 K, i5 }0 ftitanium tetrachloride, which is subsequently purified and converted to% @3 o8 J i U% ?, u* c
titanium dioxide either by direct thermal oxidation or by reaction with
1 I/ |% x) h; _- _9 Dsteam in the vapour phase. Alternatively, concentrated hydrochloric7 o* d+ ^& u' ^5 m# z2 V
acid can be reacted with the titanium-containing mineral to form a" ?" ?# b% P5 h' G
solution of titanium tetrachloride, which is then further purified and; ?4 y1 F s6 s5 G, v6 y
converted to titanium dioxide by hydrolysis. The titanium dioxide is$ w/ O& t' }# `" s; s
filtered, washed, and calcined.
& x+ N5 _1 h# }) B4 O, f' xCommercial titanium dioxide may be coated with small amounts of7 [' R5 a1 S- ? y7 |" r0 e
alumina and/or silica to improve the technological properties of the, ]+ c% ~. E0 H7 t' C
product.
8 q% U" k/ A$ ^/ I6 QC.A.S. number 13463-67-77 `5 F' E2 b" n
Chemical formula TiO2
( x# J1 ~/ t5 F, \: jFormula weight( O( f! z4 g- f [3 _2 R7 o
79.88
9 W7 ~( S# x, L, G6 WAssay
; _1 w+ C# D) W0 J' D, ONot less than 99.0% on the dried basis (on an aluminium oxide and1 u* k3 [* H. A) l4 y
silicon dioxide-free basis)
+ o! Q. s( \1 _9 x5 U* m" zDESCRIPTION; H. o. ]* H3 ^% }% e/ w9 {
White to slightly coloured powder
$ o2 D. N+ \3 S/ I5 L4 e) VFUNCTIONAL USES
0 ^: }+ H1 P) H+ k) S# [1 ~Colour4 F8 m1 i+ i- L% D( u8 T9 c; j' T
CHARACTERISTICS
# d6 R. W j$ x5 ^7 A/ ZIDENTIFICATION) ?# L" u D/ U
Solubility (Vol. 4)0 f2 c7 ?3 y) E8 w$ f8 J1 @$ J
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
7 L( q* R4 u' a0 Nsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated. ]6 h% G+ M; |/ s
sulfuric acid.
' E" H' a8 ^1 M( gColour reaction* V* ]7 y% c5 A+ j \' t/ {
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
7 g3 ^) u% `& \4 d# V; Msulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
; U9 I- I# c! _, o( R- y8 X9 ^3 v* Fwater and filter. To 5 ml of this clear filtrate, add a few drops of7 E) A) d- s& O4 V6 t4 W8 G3 S1 j
hydrogen peroxide; an orange-red colour appears immediately.
1 x' {* C$ N, cPURITY
8 E: n2 j& B, O" v) @Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h). G9 u* S$ D9 \
Loss on ignition (Vol. 4)9 A' b. {( L4 [- J& \( I0 f
Not more than 1.0% (800o) on the dried basis3 Q' L; n, W1 p8 Y
Aluminium oxide and/or) }' V2 S1 ?% g, L) b4 ~9 j$ U
silicon dioxide5 m5 I! \+ F+ L9 K' ?1 `
Not more than 2%, either singly or combined7 Z% u# i# f# ^+ b; V5 j' {
See descriptions under TESTS
# q1 E; X3 P0 |Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
c" R" x; X; K1 o0 ~alumina or silica.6 e& h$ @' a; e3 R* }
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and. H* [4 G% z$ R. j! N' R# g$ s
place on a steam bath for 30 min with occasional stirring. Filter
8 b1 [ _1 N: M+ E! I mthrough a Gooch crucible fitted with a glass fibre filter paper. Wash
6 l# ]% w4 V9 L* g+ Qwith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the
! k2 J' `% H* r3 T7 Gcombined filtrate and washings to dryness, and ignite at a dull red
! v; [+ Z |" j+ m* u# V' n/ |+ ^heat to constant weight.5 J! t3 w- W" r, G$ _( x
Water-soluble matter V) k- \1 X7 H* a
(Vol. 4)
5 X/ r, K u0 _Not more than 0.5%
, M/ K) E' U5 P3 p3 B9 E# Q2 nProceed as directed under acid-soluble substances (above), using
* k! v* L& b C0 A8 y% Rwater in place of 0.5 N hydrochloric acid.
: _) m/ T2 ?5 }, E: nImpurities soluble in 0.5 N4 A( W: u& T5 _5 _3 z, q) f4 S5 S
hydrochloric acid
, w; {' n9 [, S. b5 i5 L4 \, KAntimony Not more than 2 mg/kg
: f0 Q4 L( j8 X1 cSee description under TESTS
$ d. m+ J0 G+ a1 K8 s. C2 z# }# gArsenic Not more than 1 mg/kg) h! a( c4 U( x4 w& W/ \4 C8 t& q
See description under TESTS
1 F& G. |- y- L7 g uCadmium Not more than 1 mg/kg c/ {9 G5 b7 |6 Q4 z- ?
See description under TESTS
$ B; J. Q5 T/ |0 F' G5 {* c/ bLead
! }/ W2 z; l; ~7 }$ B3 KNot more than 10 mg/kg- A5 s' y- E* | R$ R \
See description under TESTS
4 u2 ]3 L0 n* e0 pMercury (Vol. 4) Not more than 1 mg/kg) }6 U8 G8 \9 w1 W ?3 J' n' j
Determine using the cold vapour atomic absorption technique. Select a
* }; n$ O& {! X9 D5 m0 L. Msample size appropriate to the specified level
4 A9 @2 v3 v7 u) L( z6 OTESTS
! C$ G% a. Z+ `% V) O/ BPURITY TESTS
# V0 b1 V% l* T B4 pImpurities soluble in 0.5 N9 l7 x4 K% Q; L: ?4 ~/ A; a6 u
hydrochloric acid5 X# M7 z! b1 N+ e' b4 i
Antimony, arsenic,
5 }( G) O4 D5 ]+ C8 pcadmium and lead7 p2 e: E8 c$ |0 L( ?: A9 J
(Vol.4)2 _: H S( @3 {' J$ b0 i1 \) o
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N/ P2 l0 `8 E4 O6 I" v* [. D0 @1 K
hydrochloric acid, cover with a watch glass, and heat to boiling on a2 R3 I, l, R0 q0 `/ i7 ]
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml0 E1 Z. m q+ F+ x3 b
centrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved7 k7 J3 M9 L. Q4 z0 k5 p
material settles. Decant the supernatant extract through a Whatman( c4 X9 t! c, a! Z4 z
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml) F9 _7 W- x6 O
volumetric flask and retaining as much as possible of the undissolved
% d v( [$ Z S# Omaterial in the centrifuge bottle. Add 10 ml of hot water to the original
+ a* z \0 n+ D2 ~) L$ ?8 S/ Q; ybeaker, washing off the watch glass with the water, and pour the
6 ~; j6 s5 Z$ p8 n! Lcontents into the centrifuge bottle. Form a slurry, using a glass stirring
- p( D9 u4 s7 \/ d9 F1 J& ~rod, and centrifuge. Decant through the same filter paper, and collect7 k5 j: p& J7 B' \
the washings in the volumetric flask containing the initial extract.
: `" x! q* l/ H8 M% F' Q7 bRepeat the entire washing process two more times. Finally, wash the
' r% T1 c' w' G( P; ~( Sfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask4 s' o3 ~# T7 p, x/ W2 R% q
to room temperature, dilute to volume with water, and mix.
! g5 }: {, c& j" x( a0 S& k& PDetermine antimony, cadmium, and lead using an AAS/ICP-AES' x' y# Q3 d9 ?6 D! ]
technique appropriate to the specified level. Determine arsenic using the
+ N: C$ Z5 c% x" TICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
- @& y1 m' F5 @- Q5 I- p1 W- U7 A2 q/ dMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than D; f7 k5 `) h
1 g. The selection of sample size and method of sample preparation
0 u% Q0 C; \8 G' Zmay be based on the principles of the methods described in Volume 4.
; T7 ^0 k" p: \& ?" H$ \/ y/ e1 rAluminium oxide Reagents and sample solutions- I+ b/ L5 A$ ], O. _# W% U
0.01 N Zinc Sulfate
2 L! M. K# Y7 G( a1 c% ~9 zDissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
$ v _- p1 G; r: a: [& X$ ~ xmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg
e/ m3 X$ |* m/ u% @$ xof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of% n, S9 s$ z9 Y; p% _
concentrated hydrochloric acid, heating gently to effect solution, then
- d( N' b1 r# ~, q4 b( g4 ytransfer the solution into a 1000-ml volumetric flask, dilute to volume
2 z) C) F- T9 y# Y' |1 q/ Swith water, and mix. Transfer a 10 ml aliquot of this solution into a 5002 {# j8 c8 `8 F1 e5 _6 y+ ]
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
( {/ a, d4 u$ Bconcentrated hydrochloric acid, add 1 drop of methyl orange TS and3 c% o+ r2 z6 H; R0 T" G/ |
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
! J1 r& h. h+ I. D3 ^5 Bdropwise, ammonia solution (1 in 5) until the colour is just completely
/ E% @: W/ }! A9 M9 j u0 `changed from red to orange-yellow. Then, add:8 }' M. y) ?; N t( C/ A
(a): 10 ml of ammonium acetate buffer solution (77 g of
3 A2 G$ L) m% l. Qammonium acetate plus 10 ml of glacial acetic acid, dilute to: o# Q- O4 x* }; x
1000 ml with water) and
' y: Y5 @& t- h(b): 10 ml of diammonium hydrogen phosphate solution (150 g
+ R& Y) y+ ~. K9 p/ O& q: xof diammonium hydrogen phosphate in 700 ml of water,
. R6 V- A. K* Q8 Fadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,
) z* B9 X7 x7 x" |& l, t1 z7 Uthen dilute to 1000 ml with water).0 d4 `) T3 f* c: v- u
Boil the solution for 5 min, cool it quickly to room temperature in a
, l3 {: j$ U$ p8 P8 O ^* h4 astream of running water, add 3 drops of xylenol orange TS, and mix.) ?4 H) }' M3 p- H' z
Using the zinc sulfate solution as titrant, titrate the solution to the first. }- }: U8 L+ u; `0 t& \ B
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:! T5 e( F$ z- k$ d; G
This titration should be performed quickly near the end-point by
. s0 f3 U8 t2 ~! fadding rapidly 0.2 ml increments of the titrant until the first colour2 a8 W9 [8 T! k$ c; J8 q O$ Q& N
change occurs; although the colour will fade in 5-10 sec, it is the true
8 f7 E5 v# w) d D: [end-point. Failure to observe the first colour change will result in an
3 ]; x! o" z9 f! m, N1 Z8 N2 H1 Pincorrect titration. The fading end-point does not occur at the second
7 a/ H5 l/ C1 W# qend-point.)& Q3 W0 k8 a$ Y0 r3 e$ ?* d: w
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
: W9 j$ R2 `; Q$ `$ s" Cstream of running water. Titrate this solution, using the zinc sulfate, K9 J3 o$ y a7 ?5 C7 r [
solution as titrant, to the same fugitive yellow-brown or pink end-point
' G0 o* p- H3 E1 Zas described above.
4 d5 M( l4 ]7 ]& SCalculate the titre T of zinc sulfate solution by the formula:, u, H: }7 @& [+ z# p7 N6 R, }
T = 18.896 W / V
6 r! @4 |: i6 u2 Kwhere
6 g& J# ~: o: n0 F& L% w! V; x* T% MT is the mass (mg) of Al2O3 per ml of zinc sulfate solution
; @9 c8 u$ q1 _W is the mass (g) of aluminium wire$ n, m. B3 o, W8 I# E, C
V is the ml of the zinc sulfate solution consumed in the! J- D# i- P6 K
second titration
+ E7 Y" ^7 L" T18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
" W! @ c8 Q& l: r2 ^R is the ratio of the formula weight of aluminium oxide to
0 h m- k! G# l2 Q/ _6 p4 fthat of elemental aluminium.
& d4 \# o/ o2 k# {Sample Solution A& _2 w: m8 k0 P& v
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica- n; w, D1 H# n. F- I
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
d( g5 k6 w, o3 |& l6 i- a1 U(Note: Do not use more sodium bisulfate than specified, as an excess
# u& y$ p! ` S6 [/ U8 F' Kconcentration of salt will interfere with the EDTA titration later on in the( c5 G. J( F8 Z" H/ i$ X
procedure.) Begin heating the flask at low heat on a hot plate, and5 \; d* Q( f/ [ {0 ]; w/ U
then gradually raise the temperature until full heat is reached.
7 g! `% w! ^; K* I0 F/ e( F5 l2 ^1 {(Caution: perform this procedure in a well ventilated area. ) When8 ?5 s: ] n" r8 }9 T. Q6 z
spattering has stopped and light fumes of SO3 appear, heat in the full
+ a: L: J" u7 N7 _: M$ P9 ]flame of a Meeker burner, with the flask tilted so that the fusion of the
: J: Y0 X* h6 ^% o$ [0 h2 asample and sodium bisulfate is concentrated at one end of the flask.2 d: p& N3 d9 i/ I0 B
Swirl constantly until the melt is clear (except for silica content), but
8 C0 c, }' n+ l% _) bguard against prolonged heating to avoid precipitation of titanium9 K' ^/ [ I& K" K
dioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until! U0 J3 S9 j, G! n5 N2 k; \. J
the mass has dissolved and a clear solution results. Cool, and dilute to. V8 K( c+ m6 ~( k: u3 s
120 ml with water. Introduce a magnetic stir bar into the flask.
. j/ [' a' R4 P6 c" I6 cSample Solution B6 \& n( N1 d; [% [3 `
Prepare 200 ml of an approximately 6.25 M solution of sodium# W0 [+ a( \& ]8 v
hydroxide. Add 65 ml of this solution to Sample Solution A, while
) a* v a- B; f+ ustirring with the magnetic stirrer; pour the remaining 135 ml of the
0 G# n8 M3 g4 b# e7 }4 a) |4 E( walkali solution into a 500-ml volumetric flask.3 b! ?' _( I6 H- o: [1 p4 V
Slowly, with constant stirring, add the sample mixture to the alkali4 T$ O" t5 w1 u7 s- {' F
solution in the 500-ml volumetric flask; dilute to volume with water,' I- G1 V$ |5 K; S/ n' _
and mix. (Note: If the procedure is delayed at this point for more than
" R8 ~( B' q$ [& a* v1 u2 Q) ~2 hours, store the contents of the volumetric flask in a polyethylene. F& i% W0 z z7 F: s- l0 k/ w7 c
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
' u1 ~% o( w. d0 w. Sthen filter the supernatant liquid through a very fine filter paper. Label
5 a) @0 U9 ^* l5 L- {+ athe filtrate Sample Solution B.
0 n8 A/ h7 k/ l2 sSample Solution C* t; }1 W2 Q7 G
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer3 g0 s% h2 G& i, c \( r; j
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid$ o8 y& h% u, J$ n/ Y
solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.024 }& J! a6 S# x9 n
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
3 e7 ]- _/ E% T U6 Eknown, calculate the optimum volume of EDTA solution to be added
7 y, Z+ M' A3 iby the formula: (4 x % Al2O3) + 5.]
5 G, O! S( D4 i y3 _Add, dropwise, ammonia solution (1 in 5) until the colour is just% P$ L# ]' Z+ Q, @0 D; C
completely changed from red to orange-yellow. Then add10 ml each/ X P* @1 C3 q7 }- k
of Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to; P X- W8 |5 \# K; q% p# C
room temperature in a stream of running water, add 3 drops of xylenol% G& H8 ]' H* Y2 K( b# `
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
' `6 V' @$ @9 u4 W i' Lbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
2 l5 n1 q9 k0 N+ e% J0 E5 D2 S" WpH, a pink colour indicates that not enough of the EDTA solution has
9 |. S2 Y6 E- G2 y3 B G. {been added, in which case, discard the solution and repeat this
: o6 c( j+ q' A* Q8 E+ }procedure with another 100 ml of Sample Solution B, using 50 ml,
3 ]( L* _: w" A, Z6 z* _5 frather than 25 ml, of 0.02 M disodium EDTA.
1 {9 S# p5 v& }* l. b0 yProcedure! C0 j# w, k, D" z
Using the standardized zinc sulfate solution as titrant, titrate Sample
3 X" E$ r0 G# K+ l0 V7 D# {Solution C to the first yellow-brown or pink end-point that persists for: d! ?6 V: j! r9 f9 D; T$ p# `
5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first5 e& d [+ w8 G; ^4 ~' n; V
titration should require more than 8 ml of titrant, but for more accurate
0 g( V# @6 b/ L# f9 q8 y- m; Y; Xwork a titration of 10-15 ml is desirable.
; T: n% J1 V, \3 o* [Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5( }$ E" z. [4 M; B/ t
min, and cool in a stream of running water. Titrate this solution, using( t: L6 w+ N: d& n$ K" q
the standardized zinc sulfate solution as titrant, to the same fugitive
3 ?/ W2 p' ~8 N: a, ~" oyellow-brown or pink end-point as described above.
' W7 y6 H) ?/ D: s9 ECalculation: Y8 d- B# {8 A) U+ f/ w; r% D
Calculate the percentage of aluminium oxide (Al2O3) in the sample
6 I5 y* T9 F! V# t- d1 x0 Y5 utaken by the formula:: m9 [, J f. ~; {: f# X; F! X6 k
% Al2O3 = 100 × (0.005VT)/S
, F7 J5 r+ o1 zwhere! n+ B1 O; G% F
V is the number of ml of 0.01 N zinc sulfate consumed in( b$ o* i) a5 R4 z, x' G' i- l
the second titration,
8 u* U$ [- G0 \% C; K8 pT is the titre of the zinc sulfate solution,
4 W$ t9 t( T: T/ ?: R+ DS is the mass (g) of the sample taken, and5 C. n' c" e; k% c
0.005 = 500 ml / (1000mg/g × 100 ml).: K- t' p* [7 R- D& ~( k9 c4 H
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
: Y# Z# d' F5 |glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
6 @) G R$ }/ \Heat gently over a Meeker burner, while swirling the flask, until
e0 l9 Y8 t# \9 k' Y9 @decomposition and fusion are complete and the melt is clear, except
0 E( t2 Z! _+ K. t6 mfor the silica content, and then cool. (Caution: Do not overheat the7 Z7 G* H/ @ o) l
contents of the flask at the beginning, and heat cautiously during
' W, |, Z0 y! P1 A: v. ^fusion to avoid spattering.)/ W) \! o) ~: C6 F( e3 f& S
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
( i. Q3 ^6 x! d- ~6 T' F( v+ \carefully and slowly until the melt is dissolved. Cool, and carefully add
/ e8 d& F, c# m3 ]' e* I) P150 ml of water by pouring very small portions down the sides of the
# d6 b4 _/ Y$ D, pflask, with frequent swirling to avoid over-heating and spattering. Allow, \6 z) U5 d/ X/ Z1 x
the contents of the flask to cool, and filter through fine ashless filter
$ w: z6 x. x4 K# |2 @! rpaper, using a 60 degree gravity funnel. Rinse out all the silica from: C; l, i, X p. r$ P: s% c1 k1 Q
the flask onto the filter paper with sulfuric acid solution (1 in 10).
2 ]* E4 @1 @. ~/ YTransfer the filter paper and its contents into a platinum crucible, dry in+ \5 s" j0 Z8 [$ A3 q3 X
an oven at 1200, and heat the partly covered crucible over a Bunsen
. B% R9 M/ V9 a fburner. To prevent flaming of the filter paper, first heat the cover from
' o1 [% m9 Y' Y# v1 D) babove, and then the crucible from below.8 x3 \/ N$ |- B7 c
When the filter paper is consumed, transfer the crucible to a muffle
$ s6 B3 e# X* ^& kfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and0 X1 V8 Q7 }3 o8 D8 n, P
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated- y ~( |0 B! w' r4 N( {. W
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first# S9 X: K# h# i! H" @' g4 S
on a low-heat hot plate (to remove the HF) and then over a Bunsen
% H1 s: Y0 i. f4 q2 }burner (to remove the H2SO4). Take precautions to avoid spattering,9 R( C& H' M9 O
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a
! ^, f) r0 S# @( G; w1 Q% Ldesiccator, and weigh again. Record the difference between the two
. y' Q: `2 p2 Dweights as the content of SiO2 in the sample.
' a7 `$ \- B4 wMETHOD OF ASSAY' G8 i' T# a- n' ~4 Z
Accurately weigh about 150 mg of the sample, previously dried at 105o8 s! s4 p* t# r5 x$ _( @: X& o
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water% V+ p; o, \) }/ Z$ F$ x6 a
and shake until a homogeneous, milky suspension is obtained. Add 30) x1 t) s# e4 x$ I# H& W
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
) f* n& m. I2 [; t8 vheat gently, then heat strongly until a clear solution is obtained. Cool,9 E! f( g$ a+ V$ ]
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric
; }1 I4 L- U8 Y6 [3 ]acid, and stir. Add 3 g of aluminium metal, and immediately insert a
& ^9 C' N* y0 V6 m+ Rrubber stopper fitted with a U-shaped glass tube while immersing the
4 g: \0 B* V% b+ Oother end of the U-tube into a saturated solution of sodium1 N) c6 Y! S" i7 @' |
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
7 i6 t) i* V" I4 g/ [hydrogen. Allow to stand for a few minutes after the aluminium metal. l) R# Z- B" c: A& a6 |$ W2 X: m- v
has dissolved completely to produce a transparent purple solution.
0 ~) x/ T l Z4 ^+ _- \Cool to below 50o in running water, and remove the rubber stopper
1 d0 Q3 d& P) vcarrying the U-tube. Add 3 ml of a saturated potassium thiocyanate9 n( O( Z, d" Y
solution as an indicator, and immediately titrate with 0.2 N ferric
: \1 m7 F8 Y: _1 W: Hammonium sulfate until a faint brown colour that persists for 30
1 o+ V+ [, z/ T5 Aseconds is obtained. Perform a blank determination and make any3 J+ a/ V) H0 Z S
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
& n7 l0 S; A# sequivalent to 7.990 mg of TiO2.6 M( [1 c4 m% e9 Q8 A M
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