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二氧化钛(钛白粉)
二氧化钛(钛白粉) l, F; T3 W( F5 X
0 S/ p% x) j4 o1 S0 {' J$ i8 N
JECFA关于二氧化钛(钛白粉)的结论
# G! u; Z/ d5 Q! {* K8 I$ c! `
9 z# t% A0 i6 E摘要: 2006年JECFA关于二氧化钛的结论
6 ]- ? D) _1 Z3 DADI值:不作限制。
6 z" r$ C) ]- r5 q8 V! H功能:着色剂
, Y O5 ?- F" z7 @+ c0 J2 R3 h, ]# M
TITANIUM DIOXIDE
8 E; s* Q5 U7 j: B8 }$ hPrepared at the 67th JECFA (2006) and published in FAO JECFA8 k# q' j! x: r% o
Monographs 3 (2006), superseding specifications prepared at the 63rd8 w7 }3 u+ Y" [3 `5 b- Q4 w# w
JECFA (2004) and published in FNP 52 Add 12 (2004) and in the
3 P6 J5 R/ C( |Combined Compendium of Food Additive Specifications, FAO JECFA& m! q8 \3 V" o5 y0 S! L
Monographs 1 (2005). An ADI “not limited” was established at the 13th
( j/ E7 d. J+ _8 \" bJECFA (1969).. o, Y) S) u$ r+ b# q1 Y5 ^
SYNONYMS: W J& ~8 K7 p7 b. R5 n* w& w0 c, A
Titania, CI Pigment white 6, CI (1975) No. 77891, INS No. 171
' W% c, Q4 M; }& TDEFINITION
6 H \& X. S& Z( d8 e; XTitanium dioxide is produced by either the sulfate or the chloride
; f* F8 I" L X! G$ t' ~8 Eprocess. Processing conditions determine the form (anatase or rutile
% j9 h% F( ?- f; Qstructure) of the final product.$ V E& D4 J g
In the sulfate process, sulfuric acid is used to digest ilmenite (FeTiO3)+ n8 y3 l* M/ Q3 O0 G
or ilmenite and titanium slag. After a series of purification steps, the* L: T9 A* K) v# v/ X: A z5 H
isolated titanium dioxide is finally washed with water, calcined, and
( i1 U, d& N$ x+ m* F: Lmicronized.
, I/ d8 H2 S2 x( XIn the chloride process, chlorine gas is reacted with a titaniumcontaining
. U5 J# x4 c2 ^$ @8 dmineral under reducing conditions to form anhydrous% z _, V+ Y9 ^2 ~+ l1 w
titanium tetrachloride, which is subsequently purified and converted to5 Q8 Z2 I# v5 b6 O+ v- w' d
titanium dioxide either by direct thermal oxidation or by reaction with" l ?8 x! Z; }- y/ e5 i* A0 }4 G
steam in the vapour phase. Alternatively, concentrated hydrochloric
) G W9 {! e" |, a1 `acid can be reacted with the titanium-containing mineral to form a: B9 W3 {0 s6 i; P; S
solution of titanium tetrachloride, which is then further purified and
& i, Z! L* T: T$ Z' v! {converted to titanium dioxide by hydrolysis. The titanium dioxide is
8 t5 u/ a5 {. z0 Qfiltered, washed, and calcined.6 w3 q i" p% c
Commercial titanium dioxide may be coated with small amounts of+ f3 h8 Z }, a$ H
alumina and/or silica to improve the technological properties of the
, Z$ P: V4 O: ^0 s! c' ~2 dproduct.
0 @, l: j3 C) v' FC.A.S. number 13463-67-7
( R& t6 p" Q" f; |8 g: u/ Q4 aChemical formula TiO2
; X o8 }6 a" H' VFormula weight- b+ \7 M5 _& t( a5 I, N
79.88
/ u% j+ W/ v' b% Q% }Assay5 ~. k( m" k0 s @
Not less than 99.0% on the dried basis (on an aluminium oxide and
3 A. A$ t2 _/ q9 `! G( Ssilicon dioxide-free basis)4 d g; t X$ J8 C- K3 K
DESCRIPTION- Y( b2 l( n% m1 g+ `) D n
White to slightly coloured powder
5 w/ _3 _2 n0 C7 z8 _; t( v+ CFUNCTIONAL USES
/ a& _9 R* `, [/ VColour
' c0 E8 |( j5 H* T: hCHARACTERISTICS
! j4 v, h$ n3 v: Z; vIDENTIFICATION u( y1 Q2 |6 I( }0 W$ c
Solubility (Vol. 4)
% B2 M ?: O4 S# y$ j! Z. DInsoluble in water, hydrochloric acid, dilute sulfuric acid, and organic4 G4 b) v6 d C( _) I% g/ N
solvents. Dissolves slowly in hydrofluoric acid and hot concentrated6 C, r. L' _3 y2 t- [& `
sulfuric acid.
+ ]" i* q0 ^/ X+ W5 C. J/ |Colour reaction, M! [/ l& U8 W6 a$ h
Add 5 ml sulfuric acid to 0.5 g of the sample, heat gently until fumes of) v! W/ E7 X" o' _
sulfuric acid appear, then cool. Cautiously dilute to about 100 ml with
! e. k/ E+ D4 i# z# wwater and filter. To 5 ml of this clear filtrate, add a few drops of% F Z5 X" u1 h( s: p
hydrogen peroxide; an orange-red colour appears immediately.+ f0 ]( h) f4 l
PURITY
$ n6 K# [- Q' X; w$ O; P) a4 H( BLoss on drying (Vol. 4) Not more than 0.5% (105°, 3 h)
6 h* V- K/ M1 Z% ]; W& K0 ~! B1 ELoss on ignition (Vol. 4), N; ~. p8 | K# Q1 ?
Not more than 1.0% (800o) on the dried basis
2 }: h, W8 g, qAluminium oxide and/or! P4 _4 Y4 Z @. y' {# P0 w
silicon dioxide- j$ S9 q% a7 l4 j
Not more than 2%, either singly or combined
- G7 C; q/ c" W# l- [See descriptions under TESTS8 z/ ?7 E" w E. R" K
Acid-soluble substances Not more than 0.5%; Not more than 1.5% for products containing
/ F. u5 w2 J' {, Ealumina or silica.
% d9 H# ?, {5 K: Q* J% O1 u& ASuspend 5 g of the sample in 100 ml 0.5 N hydrochloric acid and
) j5 d6 e; F0 }& Fplace on a steam bath for 30 min with occasional stirring. Filter6 V$ h# l* j7 X6 S+ w
through a Gooch crucible fitted with a glass fibre filter paper. Wash
+ z. W; X& {2 a2 _: A4 g( v7 N! awith three 10-ml portions of 0.5 N hydrochloric acid, evaporate the* t' N0 Z# e3 P7 s1 m, X
combined filtrate and washings to dryness, and ignite at a dull red
* K9 @% Q o) o% oheat to constant weight.
y4 X+ a/ x7 Q% C' _9 E2 tWater-soluble matter y! P' a- G( G( Y+ G6 D8 M4 v
(Vol. 4). o2 Y$ w8 V) d6 [
Not more than 0.5%
5 k" Q$ D- M) o4 F, o* YProceed as directed under acid-soluble substances (above), using
9 K% G/ C4 j. i( R4 s. F7 |4 Fwater in place of 0.5 N hydrochloric acid.! ^; n8 d3 n0 O& }9 i( T
Impurities soluble in 0.5 N
4 ?+ C* `. Z Q' i3 Ahydrochloric acid
8 B9 K6 c9 q5 q: w* J( ~Antimony Not more than 2 mg/kg
8 w5 |9 T$ A; c) j6 `4 _' r ISee description under TESTS8 p3 O+ n, ^7 g% N. J! i# O
Arsenic Not more than 1 mg/kg
% z/ }9 W! J3 p& dSee description under TESTS( @( Y7 ^( m( F B4 F- [; o
Cadmium Not more than 1 mg/kg0 @* a5 |6 q' Y7 U4 n
See description under TESTS. l% z+ i9 s3 o( J% L$ B
Lead( s% q" C; b* j( o* e
Not more than 10 mg/kg
5 p3 A$ J Z6 ], F2 uSee description under TESTS" Q0 p D9 T' u; W) r
Mercury (Vol. 4) Not more than 1 mg/kg& `- E V8 M* Y4 g) \
Determine using the cold vapour atomic absorption technique. Select a( }) Q+ j) L* l1 p7 V0 |
sample size appropriate to the specified level: P9 J6 C! P; O0 \3 l+ _6 e
TESTS
" V" M8 V, o& }3 u6 { g$ @* c0 xPURITY TESTS
$ s% L$ ` y' [% x# Z/ W( e" i% SImpurities soluble in 0.5 N
! z. N0 I# ?/ ?2 W! ] khydrochloric acid
9 y1 j" L2 L" K8 f! WAntimony, arsenic,, ]# C7 B F" @$ s& u
cadmium and lead
2 W/ p' _5 s' c0 Z+ t. Q(Vol.4)8 c; \# }$ y* n
Transfer 10.0 g of sample into a 250-ml beaker, add 50 ml of 0.5 N( H4 Y/ D" ~* [4 ^& l
hydrochloric acid, cover with a watch glass, and heat to boiling on a- o# e! w: f5 H7 ?% }
hot plate. Boil gently for 15 min, pour the slurry into a 100- to 150-ml
. d& [3 a! k/ l; d- t0 p, ucentrifuge bottle, and centrifuge for 10 to 15 min, or until undissolved0 A" X, ^4 d4 h
material settles. Decant the supernatant extract through a Whatman
* ?& c4 R" m, K9 e* @2 E9 LNo. 4 filter paper, or equivalent, collecting the filtrate in a 100-ml% k" X5 c* Y6 C' X5 ?" Z, V0 M' f
volumetric flask and retaining as much as possible of the undissolved
& @9 C" l0 ]; j' f Tmaterial in the centrifuge bottle. Add 10 ml of hot water to the original
. m# {4 m9 ] F" cbeaker, washing off the watch glass with the water, and pour the
* z5 y7 a/ [6 P* w1 j. \1 Y3 Q Jcontents into the centrifuge bottle. Form a slurry, using a glass stirring* `$ B, }1 l7 @3 `, o8 f4 {
rod, and centrifuge. Decant through the same filter paper, and collect
, O- g6 H7 a0 R( Q r) w( Zthe washings in the volumetric flask containing the initial extract.
4 N, ]( U& O( `8 x5 }Repeat the entire washing process two more times. Finally, wash the
1 ^1 f. a0 g; @7 ?filter paper with 10 to 15 ml of hot water. Cool the contents of the flask( x, ?$ N8 }" o
to room temperature, dilute to volume with water, and mix.
& s& c0 k/ \" z2 q' c x8 ADetermine antimony, cadmium, and lead using an AAS/ICP-AES
% R/ K T2 X r2 |technique appropriate to the specified level. Determine arsenic using the
. Y1 `) ~4 q, [ICP-AES/AAS-hydride technique. Alternatively, determine arsenic using
( y- N: P$ V% \4 PMethod II of the Arsenic Limit Test, taking 3 g of the sample rather than
- f" k8 t1 X, f8 a/ o$ P m7 }) i# w1 g. The selection of sample size and method of sample preparation. C% `6 [6 l5 M8 ^8 P) _0 h7 H
may be based on the principles of the methods described in Volume 4.
# t7 T. a* ^; p! h, VAluminium oxide Reagents and sample solutions
/ W/ V) ^, D$ ] L0.01 N Zinc Sulfate# i; }# E' Z7 N' g- E
Dissolve 2.9 g of zinc sulfate (ZnSO4 ? 7H2O) in sufficient water to6 z; |$ }- c7 v9 y- }
make 1000 ml. Standardize the solution as follows: Dissolve 500 mg
, |/ n5 m- R& a; O$ Rof high-purity (99.9%) aluminium wire, accurately weighed, in 20 ml of
8 N" C; e6 a& N% u# U: M: [concentrated hydrochloric acid, heating gently to effect solution, then
- k9 v# p v' Ltransfer the solution into a 1000-ml volumetric flask, dilute to volume
7 \ b- G; I( _0 m/ wwith water, and mix. Transfer a 10 ml aliquot of this solution into a 5009 G) f1 N# Y- g1 n) N2 l
ml Erlenmeyer flask containing 90 ml of water and 3 ml of5 g/ T5 h5 f# V* c- g% V1 M( [
concentrated hydrochloric acid, add 1 drop of methyl orange TS and D1 J( ]# }. V, z) k8 d1 S6 l& j3 X
25 ml of 0.02 M disodium ethylenediaminetetraacetate (EDTA) Add,
; f/ B" j( c. E! b5 qdropwise, ammonia solution (1 in 5) until the colour is just completely: T. a& i% m# N2 Y) q
changed from red to orange-yellow. Then, add:4 i7 i* D8 x. M ]9 h4 c) {
(a): 10 ml of ammonium acetate buffer solution (77 g of' ~: y! o7 m; r0 M
ammonium acetate plus 10 ml of glacial acetic acid, dilute to& {) c$ M7 Z: D* O# R- k
1000 ml with water) and
) C2 ~1 D+ x' p2 K, Z- `(b): 10 ml of diammonium hydrogen phosphate solution (150 g& x' ^9 F% V$ _3 \0 [
of diammonium hydrogen phosphate in 700 ml of water,6 y) A3 w9 ^" \$ M
adjusted to pH 5.5 with a 1 in 2 solution of hydrochloric acid,6 |% [! q; d+ g- _& U
then dilute to 1000 ml with water).
- z( i9 k* R* o6 f3 ?Boil the solution for 5 min, cool it quickly to room temperature in a* `' j. _6 T& M% O: f
stream of running water, add 3 drops of xylenol orange TS, and mix.
8 ~4 Q; ?7 O" eUsing the zinc sulfate solution as titrant, titrate the solution to the first _4 ]! M' I) N* ]3 w
yellow-brown or pink end-point colour that persists for 5-10 sec. (Note:0 j" R0 e) [2 ], d( y6 l
This titration should be performed quickly near the end-point by* A' Y I G- l: T
adding rapidly 0.2 ml increments of the titrant until the first colour
0 y8 V3 E5 c+ R. g% Q4 @( }5 @change occurs; although the colour will fade in 5-10 sec, it is the true
' M9 T( v0 R) U: f0 T7 I& cend-point. Failure to observe the first colour change will result in an- h E! i5 o4 F, f# y2 @ d; S
incorrect titration. The fading end-point does not occur at the second
* l) t, p$ h4 k; {end-point.)3 Y# V4 Y, B9 v$ c) ~: T2 r
Add 2 g of sodium fluoride, boil the mixture for 2-5 min, and cool in a
8 P4 x9 a) G* r! |2 K, sstream of running water. Titrate this solution, using the zinc sulfate8 T' ~. T) i% b- N! i+ H
solution as titrant, to the same fugitive yellow-brown or pink end-point
J0 t4 A! {) Q7 \$ A% i: J1 kas described above.
$ [1 o6 V& E e" {: U$ mCalculate the titre T of zinc sulfate solution by the formula:, U$ ~! r# q7 s$ _0 U0 U1 j; D5 z
T = 18.896 W / V9 Z) T' t! m6 m% J2 R. D3 W
where# B0 X" R9 I9 u% H. A1 l+ t3 p+ O
T is the mass (mg) of Al2O3 per ml of zinc sulfate solution
. V6 P- H2 P4 S. @, K4 kW is the mass (g) of aluminium wire" K/ q2 _4 g( |6 d) }" x
V is the ml of the zinc sulfate solution consumed in the2 F% W# I' u/ K# w+ ]! F
second titration0 g/ M- r6 m k/ r( k; f: C4 |( c
18.896 = (R × 1000 mg/g × 10 ml/2)/1000 ml and
( A* b% K/ M" U0 P. wR is the ratio of the formula weight of aluminium oxide to
& j7 `/ s: y$ r8 Q6 A: j& f! o$ othat of elemental aluminium.+ N' v: J/ l! x3 Q
Sample Solution A
0 D% f2 @8 v nAccurately weigh 1 g of the sample and transfer to a 250-ml high-silica
1 Y0 f% g4 o$ Pglass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).% O& [+ M: z6 j( g2 l
(Note: Do not use more sodium bisulfate than specified, as an excess
& g* r7 n- X. yconcentration of salt will interfere with the EDTA titration later on in the! n O4 G0 ~8 e/ b, X
procedure.) Begin heating the flask at low heat on a hot plate, and7 A l: l7 c8 i }: v
then gradually raise the temperature until full heat is reached.! L, m7 Y- K# F5 b
(Caution: perform this procedure in a well ventilated area. ) When
2 l% t* ? ~9 w$ mspattering has stopped and light fumes of SO3 appear, heat in the full
: ~8 j' `7 [8 Pflame of a Meeker burner, with the flask tilted so that the fusion of the$ z6 m; l s& X, `: s* c! ^& _1 `
sample and sodium bisulfate is concentrated at one end of the flask.; j! k1 q- [$ a, m( p; B
Swirl constantly until the melt is clear (except for silica content), but
" B3 J" F5 X% r; G$ d gguard against prolonged heating to avoid precipitation of titanium
D$ T1 q7 a8 O3 ~) a' y0 P2 r# Ldioxide. Cool, add 25 ml sulfuric acid solution (1 in 2), and heat until3 ?: W' |3 i) @9 y
the mass has dissolved and a clear solution results. Cool, and dilute to+ _- q- W7 X L6 O$ \+ ?
120 ml with water. Introduce a magnetic stir bar into the flask.
$ O* B5 U3 `9 a6 e4 n- i. `Sample Solution B; T4 a T, F! D0 I( a
Prepare 200 ml of an approximately 6.25 M solution of sodium
u$ `, M" K" r9 {# uhydroxide. Add 65 ml of this solution to Sample Solution A, while+ @8 i4 s& d9 p# _* j' ^8 I9 J9 ^
stirring with the magnetic stirrer; pour the remaining 135 ml of the* p* o. |6 d* q. [+ o) r! _
alkali solution into a 500-ml volumetric flask.: R9 |1 s9 k- H0 c: U. t
Slowly, with constant stirring, add the sample mixture to the alkali
' Y& b6 E! R9 H' b, G" T$ `9 J' Ysolution in the 500-ml volumetric flask; dilute to volume with water,9 W2 D2 R$ s1 X# o1 C% \
and mix. (Note: If the procedure is delayed at this point for more than
. m% l* h7 Y9 i- G, ~2 `+ ^2 Z1 i" l2 hours, store the contents of the volumetric flask in a polyethylene# w2 d6 x* h$ q* I W+ L2 v$ W0 ]
bottle.) Allow most of the precipitate to settle (or centrifuge for 5 min),/ D* P* p* @4 [" l
then filter the supernatant liquid through a very fine filter paper. Label
* i* N7 h2 l8 I9 H" gthe filtrate Sample Solution B.
4 E S I- r* GSample Solution C
& C3 l. S2 N" e6 Y' k: C4 QTransfer 100 ml of the Sample Solution B into a 500-ml Erlenmeyer
" j, T, a* m, s. ` G' Iflask, add 1 drop of methyl orange TS, acidify with hydrochloric acid
( L2 ?) P3 I: Hsolution (1 in 2), and then add about 3 ml in excess. Add 25 ml of 0.020 f1 O' [8 m! V0 L, [, t
M disodium EDTA, and mix. [Note: If the approximate Al2O3 content is
3 {, Y( h" O N7 f) M( m+ @known, calculate the optimum volume of EDTA solution to be added3 X1 O/ E( g- q6 k
by the formula: (4 x % Al2O3) + 5.]
5 s2 p' _) ?! G4 k) s$ @* h s3 RAdd, dropwise, ammonia solution (1 in 5) until the colour is just
& N8 n; W& `3 i& E5 I: o$ b. J; Rcompletely changed from red to orange-yellow. Then add10 ml each
# h6 \0 e- k& A" B* W7 Aof Solutions 1 and 2 (see above) and boil for 5 min. Cool quickly to. z, v1 i. c$ D) G+ D( t
room temperature in a stream of running water, add 3 drops of xylenol, Z! C* U% Z/ B0 i7 C! [
orange TS, and mix. If the solution is purple, yellow-brown, or pink,: a2 l" m& c6 W; b4 {( j* e8 Q
bring the pH to 5.3 - 5.7 by the addition of acetic acid. At the desired
2 W0 @8 g1 q w/ T" t9 DpH, a pink colour indicates that not enough of the EDTA solution has
+ r2 Q4 ~; C+ k! t' b& K s' h, _been added, in which case, discard the solution and repeat this# g3 ?% H: T# c5 b+ O
procedure with another 100 ml of Sample Solution B, using 50 ml,7 G" a! h( q! L2 O, r3 C8 e5 ]
rather than 25 ml, of 0.02 M disodium EDTA.7 K4 e {" |: q; j& I2 a* T
Procedure$ u0 c/ n2 s5 i y" R
Using the standardized zinc sulfate solution as titrant, titrate Sample
: l& X7 m- G; P3 Z/ v0 iSolution C to the first yellow-brown or pink end-point that persists for
: }+ A7 o5 f. \* t5-10 sec. (Important: See Note under “0.01 Zinc sulfate”.) This first
/ e+ r1 i9 [% i" O7 e" }( {: etitration should require more than 8 ml of titrant, but for more accurate" g# k! p5 D( v. E! C
work a titration of 10-15 ml is desirable.+ a9 n; U. s' m0 w
Add 2 g of sodium fluoride to the titration flask, boil the mixture for 2-5
- j3 w! J. p. t. M& smin, and cool in a stream of running water. Titrate this solution, using
. e) `( F3 m% r* b) n2 o, fthe standardized zinc sulfate solution as titrant, to the same fugitive" Z. A7 X- E( `+ N
yellow-brown or pink end-point as described above." P( n0 V# e, ^3 ] E; t3 x; l
Calculation:
0 v9 l& C) v+ w; S' y w# I# RCalculate the percentage of aluminium oxide (Al2O3) in the sample& r( A I$ _, |* g0 T: n6 t6 F6 _7 p: Q" n
taken by the formula:2 ? y) [3 V2 @7 F$ r; A8 {8 o
% Al2O3 = 100 × (0.005VT)/S
, t, j! w2 _5 g, K4 G- y8 t8 { fwhere
0 y6 Y8 @: R" u0 s/ @V is the number of ml of 0.01 N zinc sulfate consumed in
' z7 J8 Y) c4 ?4 Dthe second titration,
% K" b6 ^6 s. e& g) [% D4 \T is the titre of the zinc sulfate solution,
t! v; W0 W3 i8 WS is the mass (g) of the sample taken, and/ e$ e2 U% Q& y; r" ]4 X
0.005 = 500 ml / (1000mg/g × 100 ml)./ c$ M. s2 M8 E8 _ T4 A! a
Silicon dioxide Accurately weigh 1 g of the sample and transfer to a 250-ml high-silica6 ~( @* D5 \& I9 c( O
glass Erlenmeyer flask. Add 10 g of sodium bisulfate (NaHSO4 ? H2O).. p% z9 ]8 t9 p" `% d# t
Heat gently over a Meeker burner, while swirling the flask, until {8 Q% z, R- Q! a: r
decomposition and fusion are complete and the melt is clear, except% B0 ^& O; L$ w+ h% Y: L* j
for the silica content, and then cool. (Caution: Do not overheat the6 \( f6 U1 z( n: U
contents of the flask at the beginning, and heat cautiously during5 f7 Q; k7 P- ?2 G+ Y4 ^6 v
fusion to avoid spattering.)3 k" e+ f2 M! w- Q- h2 k
To the cooled melt add 25 ml of sulfuric acid solution (1 in 2) and heat
5 |& }! U9 D! ^6 {% J& y, r0 S; Kcarefully and slowly until the melt is dissolved. Cool, and carefully add
9 Z4 `: h8 J# c. A5 K7 P150 ml of water by pouring very small portions down the sides of the
/ J6 ]# h$ [' z6 w" I( k7 gflask, with frequent swirling to avoid over-heating and spattering. Allow5 h4 O' K2 n1 m7 {, B
the contents of the flask to cool, and filter through fine ashless filter. H _3 `9 f$ e4 a9 x G! w
paper, using a 60 degree gravity funnel. Rinse out all the silica from6 x# T/ m4 Q( V0 h' M- o6 m4 G6 ~4 a
the flask onto the filter paper with sulfuric acid solution (1 in 10).
0 t0 U( H/ B3 c3 `Transfer the filter paper and its contents into a platinum crucible, dry in
6 {3 D7 q& s9 |2 A1 O b* Pan oven at 1200, and heat the partly covered crucible over a Bunsen! U# S+ r8 ?" `/ s6 U. b8 E
burner. To prevent flaming of the filter paper, first heat the cover from
^1 F" W: ~0 k; A& wabove, and then the crucible from below./ O3 [. L" ?: A5 h5 O y" J) [
When the filter paper is consumed, transfer the crucible to a muffle
9 t) d! o5 a: ?+ Y6 G3 g& zfurnace and ignite at 1000o for 30 min. Cool in a desiccator, and
( a0 | A6 ]3 P" o, \ {; W8 mweigh. Add 2 drops of sulfuric acid (1 in 2) and 5 ml of concentrated4 T2 g4 u" t& ?. S6 v2 c
hydrofluoric acid (sp.gr. 1.15), and carefully evaporate to dryness, first
1 _$ N7 H, C% ion a low-heat hot plate (to remove the HF) and then over a Bunsen
& r6 |- P" I$ l- ~$ }burner (to remove the H2SO4). Take precautions to avoid spattering,# y# v, i% A+ B( r; L
especially after removal of the HF. Ignite at 1000o for 10 min, cool in a6 p( h& d0 C' [+ Q3 P
desiccator, and weigh again. Record the difference between the two
8 {; _) k: ^' U4 O- Cweights as the content of SiO2 in the sample.
& ~- `$ R! y! N- }2 |1 B8 M1 rMETHOD OF ASSAY
: H: g6 T$ u, N5 y- \8 EAccurately weigh about 150 mg of the sample, previously dried at 105o
- `+ ?6 M+ w" Jfor 3 hours, and transfer into a 500-ml conical flask. Add 5 ml of water
8 _1 u" U; W3 N# ]and shake until a homogeneous, milky suspension is obtained. Add 30( ]1 G2 L7 _: s4 q# h1 x6 Z
ml of sulfuric acid and 12 g of ammonium sulfate, and mix. Initially
) E9 r& E* R5 v/ O0 Oheat gently, then heat strongly until a clear solution is obtained. Cool,
. ~* z) c6 G& N* [; \: sthen cautiously dilute with 120 ml of water and 40 ml of hydrochloric
6 x/ L6 R; T. l8 A. g0 }acid, and stir. Add 3 g of aluminium metal, and immediately insert a
: J: `% E' A& s, t( e, Rrubber stopper fitted with a U-shaped glass tube while immersing the; _! o; a: s, n( y$ v
other end of the U-tube into a saturated solution of sodium5 f- u2 \8 f& d) B& ~
bicarbonate contained in a 500-ml wide-mouth bottle, and generate8 n0 q7 y. ?/ ?& Q9 ?# T3 y
hydrogen. Allow to stand for a few minutes after the aluminium metal7 T3 H" r. w, Z
has dissolved completely to produce a transparent purple solution.
7 x: |, {' {/ ZCool to below 50o in running water, and remove the rubber stopper7 Q' ]9 i* n1 Q; _$ [3 }. d
carrying the U-tube. Add 3 ml of a saturated potassium thiocyanate
* j4 H$ L( B$ W; V4 Tsolution as an indicator, and immediately titrate with 0.2 N ferric
& V$ }: `* t9 jammonium sulfate until a faint brown colour that persists for 30
" k- B# B. {, Hseconds is obtained. Perform a blank determination and make any
! O: E! g1 v/ b+ i* mnecessary correction. Each ml of 0.2 N ferric ammonium sulfate is
8 B( T) O1 g/ k/ m. R9 n/ Aequivalent to 7.990 mg of TiO2.
3 f+ @: K# X d3 y- }7 X |
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