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二氧化钛(钛白粉)
二氧化钛(钛白粉)) E X. [6 U7 f% u4 |% G0 q3 F9 G
! X" G( @! `- K
JECFA关于二氧化钛(钛白粉)的结论
- V2 z5 ~7 P( Y' U8 V/ U
7 ` S! a" M8 d" v. m$ X2 `( X摘要: 2006年JECFA关于二氧化钛的结论) L) g) p' h; ~3 M# `- b N9 v
ADI值:不作限制。
: o0 G1 \4 h) Q# a1 j" i- Z功能:着色剂
" l8 W( t7 ?2 I* `- M- ?- ^9 S
. {, C' `7 Y3 ZTITANIUM DIOXIDE2 U9 w0 R# e j
Prepared at the 67th JECFA (2006) and published in FAO JECFA
! s5 ~! a9 f3 m3 L( ~Monographs 3 (2006), superseding specifications prepared at the 63rd+ q& H* l" ^ V9 q$ e
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
4 n( a; ^3 _2 k- hCombined Compendium of Food Additive Specifications, FAO JECFA
7 f" l' J* B! v# DMonographs 1 (2005). An ADI “not limited” was established at the 13th2 y7 A2 [8 G9 n1 n2 Y4 F8 P- w
JECFA (1969).
. ^1 L: A2 {9 m. gSYNONYMS8 K% e4 c2 s, i* `, Q5 H- r% q
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
% t9 h2 I& O- b) b0 ~' R3 \DEFINITION
) i: K5 _: V1 z6 H; K$ D3 r; s6 `Titanium dioxide is produced by either the sulfate or the chloride/ o( Q( V2 ]$ L/ Y
process. Processing conditions determine the form (anatase or rutile. q7 H9 ^+ W& P$ E
structure) of the final product.
, h) ?. V) B4 }# O8 LIn the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)
; G/ t, Q0 m) f1 uor ilmenite and titanium slag. After a series of purification steps, the
; o$ V# L3 S: Q: B+ _1 s2 i7 A) iisolated titanium dioxide is finally washed with water, calcined, and, e( g3 |! p; f: @/ h
micronized.
* C# ?' c1 |0 O3 K, VIn the chloride process, chlorine gas is reacted with a titaniumcontaining# B8 z4 F$ y( G: C
mineral under reducing conditions to form anhydrous% l: S0 s% a+ ?6 @( D
titanium tetrachloride, which is subsequently purified and converted to
h- @+ I) f* D' Mtitanium dioxide either by direct thermal oxidation or by reaction with
; w6 z' {. }0 @2 y5 h: qsteam in the vapour phase. Alternatively, concentrated hydrochloric" c6 q* `7 `2 l0 u
acid can be reacted with the titanium-containing mineral to form a V, \% ~/ H `8 | U, b6 X
solution of titanium tetrachloride, which is then further purified and
3 ^1 B# O! j- d! b0 Jconverted to titanium dioxide by hydrolysis. The titanium dioxide is
5 v8 ~ U$ }# {$ c# {filtered, washed, and calcined.
* A& Y! u9 y( |, D0 yCommercial titanium dioxide may be coated with small amounts of
, H9 @7 g/ V+ \7 Oalumina and/or silica to improve the technological properties of the
# t: b# s# Q% ^ {product.
. V$ U( `; D) V AC.A.S. number 13463-67-7: J {! k* O0 ~* n
Chemical formula TiO2
" q* ^0 K$ ~* ?) e3 YFormula weight
' y1 ^6 }' F( ^" i79.88) F3 u7 g9 o3 w$ W. W2 Y$ x4 G
Assay( y' [0 T. L9 e' W2 O2 D C6 z
Not less than 99.0% on the dried basis (on an aluminium oxide and- p, [% f! ~/ l) t6 f# D
silicon dioxide-free basis)
( A; `0 h+ y# p S4 b3 p! |* zDESCRIPTION0 I2 k3 ?* l) w/ _8 C4 V
White to slightly coloured powder! Q k" O) P& w+ u% ^
FUNCTIONAL USES$ E- [" T. a$ x2 _3 Q6 ~; Y# R! ^( p
Colour
: [5 Q- i- Z- {/ i9 `: S5 F& qCHARACTERISTICS% n8 M% ~7 g) w- m. L) Z
IDENTIFICATION' s9 X6 y% U8 A; E/ M# C
Solubility (Vol. 4): M Z2 ], ~3 i2 O( w3 i$ b' H
Insoluble in water, hydrochloric acid, dilute sulfuric acid, and organic
' f% f& d# y; M! V' ]$ |& D9 Rsolvents. Dissolves slowly in hydrofluoric acid and hot concentrated5 X! B" f7 N4 t' s4 P8 \6 n. L
sulfuric acid.3 j6 \5 H, B2 q( e8 X
Colour reaction5 a9 J. f0 U2 m: s- E
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of
& b. {8 `; |% ?5 A! e7 Ysulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
$ I' X, s' x; I3 N1 ^water and filter. To 5 ml of this clear filtrate, add a few drops of
$ x3 }' a5 p% V' dhydrogen peroxide; an orange-red colour appears immediately.
F/ Q$ T4 x9 L2 @* _0 qPURITY- z) E( B5 i/ U4 p
Loss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)# r# ^- E y5 w. l% y
Loss on ignition (Vol. 4)
- D0 B) [3 }' ]; t3 L0 HNot more than 1.0% (800o) on the dried basis* G2 T- B7 y( r7 P" }& ~9 Q9 y
Aluminium oxide and/or1 f0 l$ J: M3 G$ X: E
silicon dioxide
2 ?/ ~) H+ H$ U- y3 cNot more than 2%, either singly or combined2 C" p5 S$ ]" C z* y$ U. G( s3 w
See descriptions under TESTS
! F! i, _5 u9 \. nAcid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
" e' l) O" k$ ?# k7 Calumina or silica.) R. m8 s0 k0 N& I+ b$ j
Suspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and% ~+ u$ Q8 @% E2 Q+ ]: P- v/ M( b
place on a steam bath for 30 min with occasional stirring. Filter
" h* H* v. O/ m8 o5 tthrough a Gooch crucible fitted with a glass fibre filter paper. Wash% u% X4 c5 V8 e+ h* ]( u
with three 10-ml portions of 0.5 N hydrochloric acid, evaporate the7 N" `1 @' i G1 m% X
combined filtrate and washings to dryness, and ignite at a dull red/ a7 {& g" K% R3 T9 B2 b; t+ `) [
heat to constant weight.
& z! w& G2 } k' D! HWater-soluble matter
( ]- h0 `$ V* a(Vol. 4)
% c4 P+ \! A/ M7 b( q2 `3 {/ uNot more than 0.5%
% o- W I5 t+ ^+ {Proceed as directed under acid-soluble substances (above), using
' k+ I+ j/ Q$ O% o! cwater in place of 0.5 N hydrochloric acid.
( O. L F- y0 h: aImpurities soluble in 0.5 N6 |* M, Q4 R5 S8 q1 E
hydrochloric acid% p: ~6 j1 F. \: A( [
Antimony Not more than 2 mg/kg/ B6 c' x# w2 H) @
See description under TESTS
( d; K- a/ c( T$ Z' I3 c( V: ^Arsenic Not more than 1 mg/kg) v7 E. _& p [- L( W
See description under TESTS
& x% u0 [ F9 ?/ p8 u# E- N2 wCadmium Not more than 1 mg/kg
2 V& z0 j1 d: @4 X8 E' t4 J# zSee description under TESTS
# ]& x7 @9 O( o2 w8 R) JLead: L2 P9 n( {2 t N* _6 H2 J9 o
Not more than 10 mg/kg1 s! ?0 x0 s( a* o* c9 J7 H
See description under TESTS
6 \' G0 y" ]+ s) |( s( WMercury (Vol. 4) Not more than 1 mg/kg
) W/ \* G9 {& J' J$ g: gDetermine using the cold vapour atomic absorption technique. Select a
, j; V5 A- n/ @0 e6 N4 N# n$ _5 `# h' wsample size appropriate to the specified level
) g5 o5 p) w% K5 G$ q; o: v+ iTESTS
/ z0 f Z0 c5 nPURITY TESTS
$ U8 i" [% Y# N' JImpurities soluble in 0.5 N, ~ L* p% o" v4 b4 y& J# ?
hydrochloric acid! N1 y- \/ o; v. p4 D
Antimony, arsenic,+ D9 z* Z& ^* n
cadmium and lead
I. L" D- ]. g(Vol.4)
4 e2 ~" z9 k! O) _& c' Y5 eTransfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N
1 M5 G4 q+ v) rhydrochloric acid, cover with a watch glass, and heat to boiling on a% N+ e0 k* ?1 p* v
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
- F8 W4 Z X8 R1 `8 w) g# Ucentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved
3 H3 I! T9 \( o$ r, o( g. Mmaterial settles. Decant the supernatant extract through a Whatman0 I1 F# B7 V O/ q
No. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml1 e- x' W# C0 A$ A* n' S8 p
volumetric flask and retaining as much as possible of the undissolved
: q( H+ m N' n4 }) M) d. N# ymaterial in the centrifuge bottle. Add 10 ml of hot water to the original4 R* V+ N+ q6 O% S
beaker, washing off the watch glass with the water, and pour the) Z; n b4 _' G n
contents into the centrifuge bottle. Form a slurry, using a glass stirring
: n6 d4 X/ U, U2 Orod, and centrifuge. Decant through the same filter paper, and collect" q7 n' m- i% b/ R( h' P5 @: J
the washings in the volumetric flask containing the initial extract.) l7 w1 X& c$ q( \6 P
Repeat the entire washing process two more times. Finally, wash the
: u. }, g; L% d2 _& pfilter paper with 10 to 15 ml of hot water. Cool the contents of the flask9 `0 U+ }( K0 f5 R: c
to room temperature, dilute to volume with water, and mix.# @9 \2 U4 I6 A% c
Determine antimony, cadmium, and lead using an AAS/ICP-AES
! ?5 S0 J/ L6 ~4 Mtechnique appropriate to the specified level. Determine arsenic using the0 J7 ~; \* q2 o
ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using% u/ Y) w5 Q8 @# l. {5 [9 x
Method II of the Arsenic Limit Test, taking 3 g of the sample rather than
8 |) Y. ]) e$ U0 B5 M- Z* R6 x, }1 g. The selection of sample size and method of sample preparation
+ I8 h( R0 c- L/ c8 r1 T7 \4 Emay be based on the principles of the methods described in Volume 4.
( F" Q u' `9 W! F) LAluminium oxide Reagents and sample solutions
5 q& e p( e0 X+ w# k+ y9 [; Z0.01 N Zinc Sulfate- v- [0 Q. `' r
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to
9 `3 P( d% p3 u8 U7 Hmake 1000 ml. Standardize the solution as follows: Dissolve 500 mg. ~9 A7 x' x. B! b( N# b. K" R
of high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
9 h: I% P, ~2 S- Z8 @% k0 `0 dconcentrated hydrochloric acid, heating gently to effect solution, then' A& X$ O0 W _0 Z
transfer the solution into a 1000-ml volumetric flask, dilute to volume
7 p1 f: Q! \# n4 d$ q/ s, x% jwith water, and mix. Transfer a 10 ml aliquot of this solution into a 5000 m1 P5 M4 A) }+ ~- C
ml Erlenmeyer flask containing 90 ml of water and 3 ml of
( O z- h" J' G# f8 E9 gconcentrated hydrochloric acid, add 1 drop of methyl orange TS and
' C5 I$ r6 [+ U' `25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
. z7 G+ i. `7 H' I6 H- F/ e0 Bdropwise, ammonia solution (1 in 5) until the colour is just completely
: p$ ]% h" G2 x' K8 xchanged from red to orange-yellow. Then, add:- m& i8 a% c# {
(a): 10 ml of ammonium acetate buffer solution (77 g of
: O1 Q3 W$ a2 V9 h6 T1 a# t( ]) gammonium acetate plus 10 ml of glacial acetic acid, dilute to7 H) i c9 s! s9 \$ q; e9 H, A# u
1000 ml with water) and
+ K, F8 z5 n4 t; R+ @(b): 10 ml of diammonium hydrogen phosphate solution (150 g
6 a/ T* V) B: m" V# w. j+ nof diammonium hydrogen phosphate in 700 ml of water,
( a9 h9 t% {; v! x% ^- k, ~" gadjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,( W" V* ~' f6 X, S8 j
then dilute to 1000 ml with water).
, u9 }9 W+ U5 }: L! KBoil the solution for 5 min, cool it quickly to room temperature in a
5 Y( e. c6 h! l' Ostream of running water, add 3 drops of xylenol orange TS, and mix.; _3 @. u% C% k' Y% U" R8 _' ~. `+ G( B
Using the zinc sulfate solution as titrant, titrate the solution to the first
( u8 G7 q/ B5 w6 E4 s2 Iyellow-brown or pink end-point colour that persists for 5-10 sec. (Note:3 o7 R! W4 ^# s7 W, x( |) g
This titration should be performed quickly near the end-point by- c4 b* w' g) X( c4 j7 b6 N
adding rapidly 0.2 ml increments of the titrant until the first colour& M- c- r) k) r9 d
change occurs; although the colour will fade in 5-10 sec, it is the true
) y. v* p/ ]$ U. t9 h6 Mend-point. Failure to observe the first colour change will result in an6 W) M' x( z, x p
incorrect titration. The fading end-point does not occur at the second
% s( \1 e1 Z% `, aend-point.)
4 |/ a; F: S6 C4 C$ J: l' A' ^- fAdd 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
( G/ S- q0 Y0 S) Dstream of running water. Titrate this solution, using the zinc sulfate l. W' H$ p; v! ^* c# Y! \; \0 U
solution as titrant, to the same fugitive yellow-brown or pink end-point9 u% J; E4 F: G# F7 E Y+ l
as described above.
1 K) o/ I* |0 X4 X8 C: Z0 `7 NCalculate the titre T of zinc sulfate solution by the formula:
+ v! H8 R5 X" Y! y, _T = 18.896 W / V
1 T) u% R c8 b& y R( U( ewhere# A% E* I5 Q8 ?# ?! X
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution& d% R% ?1 W o
W is the mass (g) of aluminium wire
+ K* f- c8 _( R$ KV is the ml of the zinc sulfate solution consumed in the
- e, x- U/ |5 A9 h n% y- D% R$ Bsecond titration) U5 x" }/ i) e' G' o- z. \
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and5 R9 j' s8 T1 V: r: ~9 F
R is the ratio of the formula weight of aluminium oxide to, b1 F+ t9 f/ \, w1 C
that of elemental aluminium.9 q/ Q# U5 d7 V0 b
Sample Solution A% ^0 Q" w/ M7 s
Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica
5 ` j( Z' N# c& G4 d# Bglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
- n$ ~; n- I4 }- y8 m' z* J(Note: Do not use more sodium bisulfate than specified, as an excess) b1 O4 W6 S: k% A7 c, M
concentration of salt will interfere with the EDTA titration later on in the
: [/ ]% ?# s+ V: z3 C% D- kprocedure.) Begin heating the flask at low heat on a hot plate, and
, Z# }2 y1 k+ ]then gradually raise the temperature until full heat is reached.
; n4 S- q. D2 m- A(Caution: perform this procedure in a well ventilated area. ) When: t" ~2 x% q- [% r$ ]3 c0 Q: o
spattering has stopped and light fumes of SO3 appear, heat in the full3 i" p5 u7 ^: a1 [1 T
flame of a Meeker burner, with the flask tilted so that the fusion of the
2 u L/ u9 t4 j% ]$ ^; r( csample and sodium bisulfate is concentrated at one end of the flask.4 c4 p3 M5 L. S% n' I/ ]
Swirl constantly until the melt is clear (except for silica content), but
! }, N# e ^. h; ^: ~4 {guard against prolonged heating to avoid precipitation of titanium
7 ^, H, x5 D; ~1 u4 `* S9 pdioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until
0 b5 b. q$ b: V' tthe mass has dissolved and a clear solution results. Cool, and dilute to
# M9 g" `2 u D% p/ }1 w/ V120 ml with water. Introduce a magnetic stir bar into the flask.
) g) _; h( ^" QSample Solution B
" o6 V$ V2 X# I: P) G- NPrepare 200 ml of an approximately 6.25 M solution of sodium
" B; N+ U' t+ N- o7 yhydroxide. Add 65 ml of this solution to Sample Solution A, while1 o* C2 ?$ g a: E( Z3 }
stirring with the magnetic stirrer; pour the remaining 135 ml of the
! x) ?8 L3 e9 I5 N# w3 Malkali solution into a 500-ml volumetric flask.
8 [4 Q8 s/ M( n. B1 S+ pSlowly, with constant stirring, add the sample mixture to the alkali
& P, `6 l9 }) m xsolution in the 500-ml volumetric flask; dilute to volume with water,9 x7 M: T# w2 e1 G4 K6 n
and mix. (Note: If the procedure is delayed at this point for more than* \4 I; Z# F' }) v6 d' b
2 hours, store the contents of the volumetric flask in a polyethylene
! ~+ q8 u2 s k, \bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),
( E4 C$ c, p0 `. N5 J" Y& fthen filter the supernatant liquid through a very fine filter paper. Label
4 x8 ~* p( N ~& jthe filtrate Sample Solution B.) T* w, i9 Y8 s: {) v/ m! ^
Sample Solution C4 O+ a. W2 A4 t, Q$ a" J
Transfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer1 o$ k7 ]6 I0 B; B9 y1 N$ W
flask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
2 o5 Q# N' h( e& }2 K3 _1 {solution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.02
* \0 I2 g$ S. ~1 T+ K1 m1 EM disodium EDTA, and mix. [Note: If the approximate Al2O3 content is# K: Z/ @9 B. W. i* T) d, ]
known, calculate the optimum volume of EDTA solution to be added9 o$ h6 Z$ C7 d9 G
by the formula: (4 x % Al2O3) + 5.]
/ t7 R0 K# E' K1 \7 o6 sAdd, dropwise, ammonia solution (1 in 5) until the colour is just" g2 j. z/ s+ s$ D! h
completely changed from red to orange-yellow. Then add10 ml each
3 k( _: z# k% cof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to
2 {% E4 \" ^" X$ Jroom temperature in a stream of running water, add 3 drops of xylenol% v8 S" z: @% w o! p. L3 Y! e
orange TS, and mix. If the solution is purple, yellow-brown, or pink,
- I, K3 Q1 Y, }2 y! m" h/ t; T4 Cbring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired* D8 o- m% h5 b& n$ h! m* V
pH, a pink colour indicates that not enough of the EDTA solution has
/ \% e S8 F: `: Qbeen added, in which case, discard the solution and repeat this
+ N4 J- ]: |- v1 n- c6 v d% o- j2 Wprocedure with another 100 ml of Sample Solution B, using 50 ml,
+ g( Z0 _# Y4 `3 O6 t3 U" P4 F- U5 ^rather than 25 ml, of 0.02 M disodium EDTA.8 O" ^: w1 n2 O7 q8 g. Z' B
Procedure
6 A+ l6 {8 X& y8 e+ `Using the standardized zinc sulfate solution as titrant, titrate Sample8 o) ^0 z$ K5 Y
Solution C to the first yellow-brown or pink end-point that persists for
. g6 R$ s h8 q% G) }7 ~5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
. t$ U" o+ O1 Y- w0 t3 S/ c9 Ntitration should require more than 8 ml of titrant, but for more accurate& j0 W4 p7 ~+ h9 {
work a titration of 10-15 ml is desirable.
5 ^, a7 Y6 I( D% c7 _Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5" }; d6 k5 z( J% _0 B; G2 L* E) i1 x
min, and cool in a stream of running water. Titrate this solution, using2 z/ T \8 y2 M* k7 `- t, H$ H4 K3 Z
the standardized zinc sulfate solution as titrant, to the same fugitive
Y9 E$ ?7 h; P, Y7 a' H9 r: S, Syellow-brown or pink end-point as described above.
3 ^% ~+ d% J8 F4 [Calculation:4 r) | H" ]0 {( J
Calculate the percentage of aluminium oxide (Al2O3) in the sample
2 o2 f& R9 j! f6 r: {' Jtaken by the formula:
+ T0 s! B7 _1 l* e% Al2O3 = 100 × (0.005VT)/S1 b8 w; _( u& ~8 L% o
where
8 z. ~( {0 J4 u8 x8 n+ |V is the number of ml of 0.01 N zinc sulfate consumed in
- F, [/ Y* Y0 g. B$ D; E9 |3 ythe second titration,
+ o" ^9 f3 _& s9 g5 C2 |, A; UT is the titre of the zinc sulfate solution,6 s5 j0 W( ? ^, f6 t/ A
S is the mass (g) of the sample taken, and
* P" b4 V, K# A" S( i( H9 c" h0.005 = 500 ml / (1000mg/g × 100 ml).3 [+ A; s" { {/ o
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica. A' J1 D% F# L. |/ y, n& J4 c
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).
0 p+ |0 i) @& O& i2 E2 ^6 w2 s9 I8 ?Heat gently over a Meeker burner, while swirling the flask, until
0 N4 g1 ~7 H- Qdecomposition and fusion are complete and the melt is clear, except3 o) a0 Z5 y0 L* g# R. |- B0 {
for the silica content, and then cool. (Caution: Do not overheat the
) H- Z8 y! x1 W' }" Wcontents of the flask at the beginning, and heat cautiously during
* Y# j2 a/ j, Gfusion to avoid spattering.)
! f+ V8 W2 b" [. xTo the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
4 J; ?, |/ a" Q0 S5 p E( N1 Zcarefully and slowly until the melt is dissolved. Cool, and carefully add
0 A- A1 e: V' p& M9 c150 ml of water by pouring very small portions down the sides of the6 M) @+ ~+ Y' |. i; T
flask, with frequent swirling to avoid over-heating and spattering. Allow
% f# u& c3 [- X: P. `& K, H3 ?the contents of the flask to cool, and filter through fine ashless filter# F) r( [! B9 E$ K
paper, using a 60 degree gravity funnel. Rinse out all the silica from
# Y; S: B E: r# \2 L0 H, J! \- mthe flask onto the filter paper with sulfuric acid solution (1 in 10).
; V' `" ?6 f. o `7 H: `Transfer the filter paper and its contents into a platinum crucible, dry in) S. Y! ^$ {5 C' ?2 Q( p3 O
an oven at 1200, and heat the partly covered crucible over a Bunsen% s: w( t. p, d7 s
burner. To prevent flaming of the filter paper, first heat the cover from: I1 F$ G0 ]7 Y. r
above, and then the crucible from below.
% I/ L" x1 I. h% F2 [* u& cWhen the filter paper is consumed, transfer the crucible to a muffle) J2 C4 a2 p2 C% c3 ~
furnace and ignite at 1000o for 30 min. Cool in a desiccator, and2 c9 I0 [9 J+ p
weigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated! P) H# v* s8 `3 R
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
2 U- i7 o( T# Pon a low-heat hot plate (to remove the HF) and then over a Bunsen
7 `4 J% ~- V6 }/ l, @; Tburner (to remove the H2SO4). Take precautions to avoid spattering,
: s& l) r' I6 _% }5 p4 n4 k1 [especially after removal of the HF. Ignite at 1000o for 10 min, cool in a$ t! d$ G; A) g& d
desiccator, and weigh again. Record the difference between the two# B d/ \3 A- Z8 M6 M, ?2 X! P
weights as the content of SiO2 in the sample.
3 s& N& r, q8 }/ E& R/ C8 [METHOD OF ASSAY
$ a' u: k& a/ W- BAccurately weigh about 150 mg of the sample, previously dried at 105o6 F; j1 [9 K. C/ O9 M7 Z" V, c
for 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
( X& o1 e# m+ k$ gand shake until a homogeneous, milky suspension is obtained. Add 30
* i: Q# f6 ]8 y8 e+ Z8 ~8 Yml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
; D" j9 U' ]4 \2 x, m2 Pheat gently, then heat strongly until a clear solution is obtained. Cool,% U: a/ v8 a; G: \8 E8 B
then cautiously dilute with 120 ml of water and 40 ml of hydrochloric* _- U7 v+ ~; R
acid, and stir. Add 3 g of aluminium metal, and immediately insert a
$ Y* o; p( w/ R' l$ arubber stopper fitted with a U-shaped glass tube while immersing the' C1 a1 ~: v, @6 j
other end of the U-tube into a saturated solution of sodium0 o1 s- }( Y( `; F; e) Z+ w4 M1 i1 f
bicarbonate contained in a 500-ml wide-mouth bottle, and generate
5 F% l4 W5 J9 x0 [# ghydrogen. Allow to stand for a few minutes after the aluminium metal
7 r& Z4 {$ d- X, r, zhas dissolved completely to produce a transparent purple solution.
+ r! E. \) _5 N! j8 M/ ?Cool to below 50o in running water, and remove the rubber stopper3 @2 y+ c% K) v; ^) z5 I
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate4 W9 n. n5 F! ^0 L, V
solution as an indicator, and immediately titrate with 0.2 N ferric: S' Y- a$ g1 H1 v$ `7 P+ }, S
ammonium sulfate until a faint brown colour that persists for 30# _. k! d& B( B w9 [
seconds is obtained. Perform a blank determination and make any' u- z$ q* P( }/ Q! {( P
necessary correction. Each ml of 0.2 N ferric ammonium sulfate is
. {6 G/ z' Z& P, ^2 Y) ^equivalent to 7.990 mg of TiO2.
, P* x1 w6 h3 T+ r |
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